CN104480754B - A kind of goth black fabric and preparation method thereof - Google Patents
A kind of goth black fabric and preparation method thereof Download PDFInfo
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- CN104480754B CN104480754B CN201410852244.2A CN201410852244A CN104480754B CN 104480754 B CN104480754 B CN 104480754B CN 201410852244 A CN201410852244 A CN 201410852244A CN 104480754 B CN104480754 B CN 104480754B
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- 239000004744 fabric Substances 0.000 title claims abstract description 130
- 238000002360 preparation method Methods 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 229920000728 polyester Polymers 0.000 claims abstract description 137
- -1 amino ethylene glycol fatty acid Chemical class 0.000 claims abstract description 109
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 74
- 239000000194 fatty acid Substances 0.000 claims abstract description 74
- 229930195729 fatty acid Natural products 0.000 claims abstract description 74
- 239000000835 fiber Substances 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 38
- 230000008569 process Effects 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 17
- 229920013822 aminosilicone Polymers 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 230000009471 action Effects 0.000 claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 119
- 238000005886 esterification reaction Methods 0.000 claims description 115
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 114
- 230000032050 esterification Effects 0.000 claims description 105
- 238000006068 polycondensation reaction Methods 0.000 claims description 90
- 239000000047 product Substances 0.000 claims description 71
- 239000001117 sulphuric acid Substances 0.000 claims description 59
- 235000011149 sulphuric acid Nutrition 0.000 claims description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 53
- 238000006243 chemical reaction Methods 0.000 claims description 52
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 45
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 31
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 31
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 30
- 238000004821 distillation Methods 0.000 claims description 30
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 27
- 238000004043 dyeing Methods 0.000 claims description 23
- 229910021529 ammonia Inorganic materials 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims description 20
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 20
- 238000004804 winding Methods 0.000 claims description 20
- 230000004044 response Effects 0.000 claims description 19
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000009835 boiling Methods 0.000 claims description 11
- 229940006460 bromide ion Drugs 0.000 claims description 11
- 238000001125 extrusion Methods 0.000 claims description 11
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 10
- PNZVFASWDSMJER-UHFFFAOYSA-N acetic acid;lead Chemical compound [Pb].CC(O)=O PNZVFASWDSMJER-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 238000006555 catalytic reaction Methods 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 230000001717 pathogenic effect Effects 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000004513 sizing Methods 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 10
- 229910052787 antimony Inorganic materials 0.000 claims description 9
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 9
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 9
- 230000008859 change Effects 0.000 claims description 9
- 150000002148 esters Chemical class 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- 239000006227 byproduct Substances 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 150000004665 fatty acids Chemical class 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 5
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 125000001246 bromo group Chemical group Br* 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- PTVDYMGQGCNETM-UHFFFAOYSA-N trityl 2-methylprop-2-enoate Chemical compound C=1C=CC=CC=1C(C=1C=CC=CC=1)(OC(=O)C(=C)C)C1=CC=CC=C1 PTVDYMGQGCNETM-UHFFFAOYSA-N 0.000 claims 1
- 239000000975 dye Substances 0.000 description 38
- 229920002521 macromolecule Polymers 0.000 description 14
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 12
- 239000005020 polyethylene terephthalate Substances 0.000 description 10
- 238000001291 vacuum drying Methods 0.000 description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 8
- 239000000986 disperse dye Substances 0.000 description 7
- 229920000139 polyethylene terephthalate Polymers 0.000 description 7
- NLAGNNORBYGNAV-UHFFFAOYSA-N isotriacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCC(C)C NLAGNNORBYGNAV-UHFFFAOYSA-N 0.000 description 6
- KUPLEGDPSCCPJI-UHFFFAOYSA-N n-Tetracontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC KUPLEGDPSCCPJI-UHFFFAOYSA-N 0.000 description 6
- CBFCDTFDPHXCNY-UHFFFAOYSA-N octyldodecane Natural products CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 5
- VHQQPFLOGSTQPC-UHFFFAOYSA-N n-Pentatriacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC VHQQPFLOGSTQPC-UHFFFAOYSA-N 0.000 description 5
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical group C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- XRRQZKOZJFDXON-UHFFFAOYSA-N nitric acid;silver Chemical compound [Ag].O[N+]([O-])=O XRRQZKOZJFDXON-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- NHWDPCHMQMJMRM-UHFFFAOYSA-N 2-aminoicosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCC(N)C(O)=O NHWDPCHMQMJMRM-UHFFFAOYSA-N 0.000 description 3
- XEDDSVXNGSVIKY-UHFFFAOYSA-N 2-aminopentadecanoic acid Chemical compound CCCCCCCCCCCCCC(N)C(O)=O XEDDSVXNGSVIKY-UHFFFAOYSA-N 0.000 description 3
- RTBNAMFQHXHWPI-UHFFFAOYSA-N 2-tetracosylpropanedioic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCC(C(O)=O)C(O)=O RTBNAMFQHXHWPI-UHFFFAOYSA-N 0.000 description 3
- WMRCTEPOPAZMMN-UHFFFAOYSA-N 2-undecylpropanedioic acid Chemical compound CCCCCCCCCCCC(C(O)=O)C(O)=O WMRCTEPOPAZMMN-UHFFFAOYSA-N 0.000 description 3
- 229920004933 Terylene® Polymers 0.000 description 3
- 238000004040 coloring Methods 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 150000001991 dicarboxylic acids Chemical class 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- GAWDONPIRRGKHC-UHFFFAOYSA-N 2-aminopentatetracontanoic acid Chemical compound NC(CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC)C(=O)O GAWDONPIRRGKHC-UHFFFAOYSA-N 0.000 description 2
- HRWROHLOIUTEJF-UHFFFAOYSA-N 2-aminopentatriacontanoic acid Chemical compound NC(CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC)C(=O)O HRWROHLOIUTEJF-UHFFFAOYSA-N 0.000 description 2
- GHGIEIMFIMJTLX-UHFFFAOYSA-N 2-aminotetracontanoic acid Chemical compound NC(CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC)C(=O)O GHGIEIMFIMJTLX-UHFFFAOYSA-N 0.000 description 2
- CCDWXBORKKHUCD-UHFFFAOYSA-N 2-aminotriacontanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCC(N)C(O)=O CCDWXBORKKHUCD-UHFFFAOYSA-N 0.000 description 2
- HXKXBCBZXXQPPD-UHFFFAOYSA-N 2-bromododecanoic acid Chemical compound CCCCCCCCCCC(Br)C(O)=O HXKXBCBZXXQPPD-UHFFFAOYSA-N 0.000 description 2
- MSJPZIZRTHHRLP-UHFFFAOYSA-N 2-bromoicosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCC(Br)C(O)=O MSJPZIZRTHHRLP-UHFFFAOYSA-N 0.000 description 2
- MUXQOFXMCVOPPW-UHFFFAOYSA-N 2-bromopentadecanoic acid Chemical compound CCCCCCCCCCCCCC(Br)C(O)=O MUXQOFXMCVOPPW-UHFFFAOYSA-N 0.000 description 2
- BZDUBIFGRWSLRE-UHFFFAOYSA-N 2-bromotetracontanoic acid Chemical compound BrC(CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC)C(=O)O BZDUBIFGRWSLRE-UHFFFAOYSA-N 0.000 description 2
- CGTWXNZDWKWRSL-UHFFFAOYSA-N 2-bromotriacontanoic acid Chemical compound BrC(CCCCCCCCCCCCCCCCCCCCCCCCCCCC)C(=O)O CGTWXNZDWKWRSL-UHFFFAOYSA-N 0.000 description 2
- SNNLICYRIGNYGV-UHFFFAOYSA-N 2-tetratetracontylpropanedioic acid Chemical class C(CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC)(C(=O)O)C(=O)O SNNLICYRIGNYGV-UHFFFAOYSA-N 0.000 description 2
- CNRCURLHTYFOII-UHFFFAOYSA-N 2-tetratriacontylpropanedioic acid Chemical class C(CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC)(C(=O)O)C(=O)O CNRCURLHTYFOII-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- DURCXLFMRCZCFV-UHFFFAOYSA-N 2-bromopentatetracontanoic acid Chemical compound BrC(CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC)C(=O)O DURCXLFMRCZCFV-UHFFFAOYSA-N 0.000 description 1
- XADSXJODDPASFF-UHFFFAOYSA-N 2-bromopentatriacontanoic acid Chemical compound BrC(CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC)C(=O)O XADSXJODDPASFF-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- JZGJHXPGBQFATA-UHFFFAOYSA-M [Br-].[N+](=O)([O-])[O-].[Ag+2] Chemical compound [Br-].[N+](=O)([O-])[O-].[Ag+2] JZGJHXPGBQFATA-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- QETVFNWBXURDPO-UHFFFAOYSA-N nonacosan-1-amine Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCN QETVFNWBXURDPO-UHFFFAOYSA-N 0.000 description 1
- AYYUCYJPSQMEDD-UHFFFAOYSA-N nonatriacontan-1-amine Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCN AYYUCYJPSQMEDD-UHFFFAOYSA-N 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- VYRMHDHLFQRAAY-UHFFFAOYSA-N pentatetracontane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC VYRMHDHLFQRAAY-UHFFFAOYSA-N 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- XYTULFXJTGBOBM-UHFFFAOYSA-N tetratetracontan-1-amine Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCN XYTULFXJTGBOBM-UHFFFAOYSA-N 0.000 description 1
- NDMKRVHBPCRHBA-UHFFFAOYSA-N tetratriacontan-1-amine Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCN NDMKRVHBPCRHBA-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Landscapes
- Artificial Filaments (AREA)
Abstract
The present invention relates to a kind of goth black fabric and preparation method thereof, the fabric that described goth black fabric is prepared by modified polyester fiber, then dye through dispersed black dye and carry out increasing deep and active amino silicone oil process and obtain；The material of described modified polyester fiber fabric is modified poly ester, and the ratio K/S of absorptance K and the scattering coefficient S of opaque body that described goth black fabric increases the opaque body of the fabric after deeply arranging between 400～700nm wavelength is greatly improved than common fabric；Described modified poly ester is made up of with amino ethylene glycol fatty acid polyester, described amino ethylene glycol fatty acid is dispersed in the molecule interchain of described polyester, and the molecule interchain of described amino ethylene glycol fatty acid and described polyester has hydrogen bond action, described amino ethylene glycol fatty acid is made to fix with the relative position of the strand of described polyester.The goth black fabric of described one may be used in various garment material and adornment.
Description
Technical field
The invention belongs to modified fibre technical field, relate to a kind of goth black fabric and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) fiber, since coming out, has obtained rapidly because of the performance of its excellence
Development, its yield has become as the hat of world's synthetic fibers.Polyester fiber has fracture strength and elastic modelling quantity is high, and resilience is fitted
In, thermal finalization is excellent, and heat-resisting light resistance is good and a series of premium properties such as acid-fast alkali-proof corrosion resistance, and fabric has anti-
The advantages such as wrinkle, stiffness are good, so, polyester fiber is widely used in the field such as clothing, home textile.
PET belongs to symmetric straight chain macromolecular, and strand does not contains side-chain radical, and regularity is the best, its main chain
Phenyl ring containing rigidity and flexible alkyl, and the ester group being directly connected with phenyl ring and phenyl ring constitute the conjugated body of rigidity
System, thus constrain rotating freely of its soft segment.This structure is it will be evident that increase on the impact of glass transition temperature
The wall ridge of molecule segment motion, the glass transition temperature of PET is higher, need to dye at very high temperatures, promotes dyestuff
Molecule is to the diffusion of fibrous inside.It addition, the strand of PET is regular, good crystallinity, strand arrangement is tight, and strand
The upper polar group not having an effect with dye molecule, the colouring making polyester fiber is more difficult.
For the problem of solution PET dyeing difficulty, techniques or methods are now used mainly to be connect by introducing dye molecule
By base or the method for increase polyester amorphous regions amount, although the dyeability of polyester can be improved, destroy the segment rule of PET
Whole property, to reduce the performance of polyester fiber to obtain the raising of dyeability.Do not destroying polyester fiber crystallinity and permutation degree
In the case of, the method used at present has three kinds of colouring methods such as support methods, high temperature and high pressure method and high temperature thermosoling.
When textile dyeing, people are generally referred to as unit's color black the deepest for color.Along with sending out rapidly of dyeing and finishing auxiliaries
Exhibition, makes the blackness of black fabric significantly increase deeply by adjusting dyeing and postfinishing process, a kind of by goth black deep-dyeing agent pair
Black fabric carries out Final finishing to the method increasing fabric blackness.Produce special black fiber mainly to have Alkali reduction, dye, climb the tree
Fat, upper deep-dyeing agent, wherein it is crucial that Final finishing deep-dyeing agent technique to be used.Deep-dyeing agent reduces reflection light quantity, improves terylene
Pile-on properties.The purpose of upper resin is to improve the degree of depth and prevent slippage, and owing to upper amount of resin is relatively big, it is unfavorable to produce fabric property
Impact.
Summary of the invention
It is an object of the invention to provide a kind of goth black fabric and preparation method thereof, the present invention utilizes amino fatty acid ethylene glycol
Ester is when uniform temperature condition, and the increasing degree of free volume is far longer than the characteristic of polyester macromolecule chain, improves dispersion dye
Material molecule enters the degree within polyester, improves the dyeability of polyester；Resin, the amount of upper deep-dyeing agent in minimizing, protect
Hold the good characteristic of fabric.
Simultaneously because in the existence of the first amino in amino ethylene glycol fatty acid molecule, increase itself and polyester macromolecule chain
Between hydrogen bond action, add its compatibility with polyester and dispersion in the polyester, decrease migration to greatest extent.
Polyester construction regularity, crystallinity are not destroyed simultaneously, maintain the premium properties of polyester.
The goth black fabric of one of the present invention, modified polyester fiber the fabric prepared, then dye also through dispersed black dye
Carry out increasing and deeply process obtain with active amino silicone oil；The material of described modified polyester fiber fabric is modified poly ester, described goth black
Fabric is under the conditions of temperature is 90～130 DEG C, and the free volume space of fibrous inside molecule interchain increases 20～30v/v%；Institute
State goth black fabric between 400～700nm wavelength, increase the absorptance K of opaque body and the opaque body of the fabric after deep arrangement
The ratio K/S of scattering coefficient S be greatly improved than common fabric；Described modified poly ester is by polyester and amino fatty acid ethylene glycol
Ester is constituted, and described amino ethylene glycol fatty acid is dispersed in the molecule interchain of described polyester, and described amino fatty acid ethylene glycol
Ester has hydrogen bond action with the molecule interchain of described polyester, makes the described amino ethylene glycol fatty acid strand with described polyester
Position relatively is fixed；
The molecular structure of described amino ethylene glycol fatty acid is:
H2N(CH2)nCOOCH2CH2OOC(CH2)nNH2；
Wherein, n=10-50.
As preferred technical scheme:
The goth black fabric of described one, line density deviation ratio≤0.5% of described modified polyester fiber, fracture strength >=
3.8cN/dtex, fracture strength CV value≤5.0%, elongation at break is 33.0 ± 3.0%, extension at break CV value≤10.0%,
Yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ± 0.20%.
The goth black fabric of described one, described amino ethylene glycol fatty acid accounts for the weight percent of described modified polyester fiber
Ratio is 0.5～2.5%.
Present invention also offers the preparation method of a kind of goth black fabric, by modified poly ester through measuring, extrude, cool down, oiling,
Stretching, thermal finalization and winding, prepare modified polyester fiber；Modified polyester fiber carries out dispersed black dye dye after being woven into fabric again
Color carrying out increases deep and active amino silicone oil process and obtains goth black fabric；Spinning technique is:
The temperature of described extrusion is 280～290 DEG C；
The pathogenic wind-warm of described cooling is 20～25 DEG C；
The speed of described winding is 4000～4600m/min；
Filament number is 0.3～1.0dtex；
The preparation process of described modified poly ester includes:
(1) preparation of amino ethylene glycol fatty acid:
1) binary of fatty acids is added in reactor with the amount of 1:1.5 mol ratio with methanol, under the catalysis of concentrated sulphuric acid, add
Heat is to 80～110 DEG C, and refuxing esterification, cooling, separating-purifying obtains binary of fatty acids mono-methyl；Esterification time is usually 2～3h；
Described binary of fatty acids is dodecanedicarboxylic acid to the one in dopentacontane dicarboxylic acids；Reaction equation is:
HOOC(CH2)nCOOH+CH3OH→CH3OOC(CH2)nCOOH
Wherein n=10～50.
2) by described binary of fatty acids mono-methyl, lead tetraacetate and lithium bromide during 1:1:1 is dissolved in benzene in molar ratio, wherein two
The concentration of unit's fatty acid mono-methyl is 0.05～0.1mol/L, and under nitrogen atmosphere, 80～90 DEG C of reactions, backflow, when no longer
When having gas to produce, add a certain amount of dilute sulfuric acid and react 2～3 hours, be washed out, purify and be dried, obtain product bromo
Fatty acid；Reaction equation is:
3), by the ammonia of bromo fatty acid and 15～25wt% during 1:2 joins reactor in molar ratio, stirring, in room temperature
Lower reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is less than 70 DEG C, until nothing
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, by product
Vacuum drying obtains product amino fatty acid；Vacuum drying temperature can use 60～70 DEG C；Reaction equation is:
HOOC(CH2)nBr+NH3→HOOC(CH2)nNH2+NH4Br；
4) ethylene glycol and amino fatty acid are stirred for 1.1:2 in molar ratio, and press amino fatty acid wt 1～
3% add concentration be 40～50wt% sulphuric acid be catalyst, carry out esterification, esterification reaction temperature is 160～220 DEG C,
It is esterification terminal that esterification water quantity of distillate reaches more than the 90% of theoretical value；The separated purification of product obtains amino fat
Acid glycol ester；Reaction equation is:
HOOC(CH2)nNH2+HOCH2CH2OH→
H2N(CH2)nCOOCH2CH2OOC(CH2)nNH2；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
Use p-phthalic acid and ethylene glycol as raw material, after being made into uniform sizing material, carry out esterification, obtain esterification and produce
Thing；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at normal pressure～0.3MPa, and temperature is at 250～260 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction coarse vacuum stage, esterification products adds catalyst and stabilizer, under conditions of negative pressure
Starting polycondensation reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature controls at 260～270 DEG C,
Response time is 30～50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino ethylene glycol fatty acid, and stir, generally stir
15～20 minutes；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275～280 DEG C, response time 50～90 minutes；
Prepare modified poly ester；
The preparation method of a kind of goth black fabric as above, described ethylene glycol with the mol ratio of described p-phthalic acid is
1.2～2.0:1.
The preparation method of a kind of goth black fabric as above, described catalyst selected from antimony oxide, antimony glycol and
One in antimony acetate, catalyst amount is the 0.01%～0.05% of described p-phthalic acid weight.
The preparation method of a kind of goth black fabric as above, described stabilizer is selected from triphenyl phosphate, trimethyl phosphate
With the one in NSC 6513, stabilizing agent dosage is the 0.01%～0.05% of described p-phthalic acid weight.
The preparation method of a kind of goth black fabric as above, is washed with deionized water to without using silver nitrate bromide ion
Solution detects.
The preparation method of a kind of goth black fabric as above, described concentrated sulphuric acid refers to the sulfur that mass concentration is 70～80%
Acid, concentrated sulphuric acid addition is the 1～3wt% of binary of fatty acids；Described a certain amount of dilute sulfuric acid refer to mass concentration be 40～
The sulphuric acid of 50%, dilute sulfuric acid addition is the 1～3wt% of binary of fatty acids mono-methyl.
Fabric is when dyeing, and the upper dye process of fabric can be divided into the next stage by disperse dyes:
1) disperse dyes flowing with dye liquor in dye liquor moves closer to fiber interface；2) disperse dyes are near fiber interface
Adsorbed by fiber surface rapidly；3), after disperse dyes are adsorbed to fiber surface, in fiber, a concentration difference or inside and outside is produced
Dyestuff chemistry potential difference, dyestuff will spread to fibrous inside；4) disperse dyes diffusion velocity and fiber unformed area content, hole or
Free volume content is relevant, and therefore the dyeing speed of disperse dyes is in addition to dyestuff dissolubility in the solution, further depends on
When the structure of fiber is outer and dyes, the degree of swelling of fiber is relevant.
Polyster fibre is hydrophobic synthetic fibers, lacks as cellulose or protein fibre in terylene molecular structure
Energy and dyestuff occur combine active group, terylene molecules align must compare closely, only exist less space in fiber,
When dyeing under the conditions of humidity, polyester fiber will not can be by the most swelling and make space increase as cotton fiber, dyestuff divides
Son is difficult to see through fibrous inside.Therefore, raising will assist in the carrying out of dyeing to the free volume between fiber molecule.
The molecular chain structure of polyester is the linear macromolecule containing benzene ring structure, the functional group's marshalling on strand,
Unbranched, macromole chain flexibility is poor.The regularity of polyester is good and rigidity is the biggest simultaneously, and intermolecular active force is bigger.
Compared with other macromolecular materials, the strand generation sliding of polyester, rotation the most more difficulty, these characteristics hinder dyestuff and enter
Enter inside polyester, thus dyeability is poor.
It is main that amino ethylene glycol fatty acid is mainly with C-C, C-O key, has certain molecular weight simultaneously, i.e. has certain
The strand of length, strand flexibility is relatively big, linear big compared with benzene ring structure of the amount of crimp of amino ethylene glycol fatty acid
Molecule is bigger, simultaneously strong compared with the linear macromolecule containing benzene ring structure to the sensitivity of temperature.When the temperature is changed, amino fatty acid
Glycol ester moves prior to the linear macromolecule containing benzene ring structure, and the produced free volume of motion is far longer than containing phenyl ring
Produced by the linear macromolecule of structure.
Added the free volume diffusion with increase dyestuff of polyester fiber by fatty acid ester, improve polyester fiber
Dyeability, make fiber obtain high dye-uptake.
Oxygen in fatty acid ester can form hydrogen bond, but oxygen is when centre position, due to space steric effect and fat
The factors such as the curling of fat acid ester molecules reduce the quantity of itself and the hydrogen evolution hydrogen bond in polyester macromolecule chain；If amino is in α position
On, i.e. amino acids, owing to amino and carbonyl interact, also it is unfavorable for amino and the hydrogen evolution hydrogen in polyester macromolecule chain
Key；When end position at macromole of the amino of amino fatty acid ester, the curling of macromole is little on its impact, adds aminolipid
Amino in fat acid esters and the formation of the hydrogen evolution hydrogen bond in polyester macromolecule chain, improve amino fatty acid ester and polyester simultaneously
Active force between macromolecular chain, decreases sliding and the migration of amino fatty acid ester.
Add amino fatty acid ester and the compatibility of polyester and dispersion in the polyester, decrease to greatest extent and move
Move.Polyester construction regularity, crystallinity are not destroyed simultaneously, maintain the premium properties of polyester.
Beneficial effect:
The modified polyester fiber of gained the most of the present invention, owing to amino ethylene glycol fatty acid is based on C-C, has simultaneously
Certain molecular weight, i.e. has the strand of certain length, and strand flexibility is relatively big, and amino adds the compatibility with polyester.
The fiber of gained is good with the compatibility of amino ethylene glycol fatty acid.
2. due in amino ethylene glycol fatty acid molecule in the existence of the first amino, increase and it and polyester macromolecule chain
Between hydrogen bond action, add its compatibility with polyester and dispersion in the polyester, decrease migration to greatest extent.
The modified poly ester of gained the most of the present invention, owing to the content of amino ethylene glycol fatty acid is less, advises polyester construction
Whole property, crystallinity are not destroyed, and maintain the premium properties of polyester.
4. the amount of crimp of amino ethylene glycol fatty acid is bigger, simultaneously to temperature compared with the linear macromolecule of benzene ring structure
Sensitive strong compared with the linear macromolecule containing benzene ring structure.When the temperature is changed, transport prior to the linear macromolecule containing benzene ring structure
Dynamic, the produced free volume of motion of amino ethylene glycol fatty acid is far longer than the linear macromolecule institute containing benzene ring structure
Produce, increase the diffusion of additive, improve the functional of polyester.
5. fatty acid ester adds the free volume diffusion with increase dyestuff of polyester fiber, improves the dyeing of fabric
Performance.
The most goth black fabric increase between 400～700nm wavelength the absorptance K of the opaque body of the fabric after deep arrangement with
Ratio K/the S of the scattering coefficient S of opaque body is greatly improved than common fabric.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate this
Bright rather than limit the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, art technology
The present invention can be made various changes or modifications by personnel, and these equivalent form of values fall within the application appended claims equally and limited
Fixed scope.
The goth black fabric of one of the present invention, the fabric that described goth black fabric is prepared by modified polyester fiber, then through dispersion
Black dyeing carrying out increases deep and active amino silicone oil process and obtains；The material of described modified polyester fiber fabric is modified poly-
Ester, described goth black fabric under the conditions of temperature is 90～130 DEG C, the free volume space of fibrous inside molecule interchain increase 20～
30v/v%；Described goth black fabric increases the absorptance K of the opaque body of the fabric after deep arrangement between 400～700nm wavelength
It is greatly improved than common fabric with the ratio K/S of the scattering coefficient S of opaque body；Described modified poly ester is by polyester and aminolipid
Fat acid glycol ester is constituted, and described amino ethylene glycol fatty acid is dispersed in the molecule interchain of described polyester, and described aminolipid
Fat acid glycol ester has hydrogen bond action with the molecule interchain of described polyester, makes described amino ethylene glycol fatty acid and described polyester
The relative position of strand fix；
The molecular structure of described amino ethylene glycol fatty acid is:
H2N(CH2)nCOOCH2CH2OOC(CH2)nNH2；
Wherein, n=10-50.
The goth black fabric of described one, line density deviation ratio≤0.5% of described modified polyester fiber, fracture strength >=
3.8cN/dtex, fracture strength CV value≤5.0%, elongation at break is 33.0 ± 3.0%, extension at break CV value≤10.0%,
Yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ± 0.20%.
The goth black fabric of described one, described amino ethylene glycol fatty acid accounts for the weight percent of described modified polyester fiber
Ratio is 0.5～2.5%.
Colouring method: dyeing disperse dyes are the black CN of beautiful element difficult to understand, fabric dyes respectively in High Temperature High Pressure machine.Knit before dye
Thing nonionic surfactant processes 30 minutes at 60 DEG C.Dye dosage is 2.0% (o.w.f)；Dispersant NNO1.2g/L,
PH value is 5, and bath raio is 1:50, and 60 DEG C enter dye, are warming up to 130 DEG C of each constant temperature dyeing 1h.
Fabric after dyeing carries out increasing deep and active amino silicone oil process.
Case depth contrasts:
As the black textile that brightness value is minimum, its case depth can use storehouse Bel card-Munch (Kubelka-
Munk) equation is expressed as:
K/S=(1-R)2/2R
In formula: R is fabric face reflectance；K is the absorptance of opaque body；S is the scattering coefficient of opaque body. surveys
Determine and calculate the K/S value of the fabric after increasing deep arrangement between 400～700nm wavelength.
Embodiment 1
The preparation method of a kind of goth black fabric, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) dodecanedicarboxylic acid is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 80 DEG C, refuxing esterification, cooling, separating-purifying obtains dodecanedicarboxylic acid mono-methyl；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of dodecanedicarboxylic acid；
2) described dodecanedicarboxylic acid mono-methyl, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Dodecanedicarboxylic acid mono-methyl concentration is 0.05mol/L, under nitrogen atmosphere, in 80 DEG C of reactions, backflow, produces when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2 hours, be washed out, purify and be dried, obtain product bromoundecane carboxylic acid；
Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40%, and dilute sulfuric acid addition is dodecanedicarboxylic acid mono-methyl
3wt%；
3), by the ammonia of bromoundecane carboxylic acid Yu 15wt% during 1:2 joins reactor in molar ratio, stirring, in room temperature
Lower reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, uses silver nitrate
Solution detects, and product vacuum drying is obtained product amino-undecanoic carboxylic acid；
4) ethylene glycol and amino-undecanoic carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino-undecanoic carboxylic acid
1% addition concentration of weight is the sulphuric acid of 40wt%, carries out esterification, and esterification reaction temperature is 160 DEG C, esterification water quantity of distillate
Reaching more than the 90% of theoretical value is esterification terminal；The separated purification of product obtains amino-undecanoic carboxylic acid ethylene glycol
Ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.2 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.3MPa, and temperature is 250 DEG C, esterification
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, three oxidations of the 0.01% of addition p-phthalic acid weight in esterification products
Two antimony and the triphenyl phosphate of p-phthalic acid weight 0.01%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Steadily be evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 260 DEG C, and the response time is 50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino-undecanoic carboxylic acid glycol ester, and stir 15 points
Clock；Described amino-undecanoic carboxylic acid glycol ester, addition is the 0.5wt% of modified poly ester；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 90 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 15000.
(3) preparation of goth black fabric
By modified poly ester through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified polyester fiber；Change
Property polyester fiber be woven into fabric after carry out dispersed black dye dyeing carrying out again and increase deep and active amino silicone oil process and obtain spy
Black fabric；Spinning technique is:
The temperature of described extrusion is 280 DEG C；
The pathogenic wind-warm of described cooling is 20 DEG C；
The speed of described winding is 4000m/min；
Filament number is 0.3dtex；
The goth black fabric of gained is under the conditions of temperature is 100 DEG C, and the free volume space of fibrous inside molecule interchain increases
25v/v%, line density deviation ratio 1.5%, fracture strength 4.5cN/dtex, fracture strength CV value 4.9%, elongation at break is
36.0%, extension at break CV value 9.1%, yarn unevenness CV2.00%, boiling water shrinkage 8.0%, oil content 1.1%.
Table 1: different product deeply arrange after K/S value at different wavelengths
| Wavelength | Goth black fabric | Common fabric |
| 400-450 | 51.88 | 45.12 |
| 460-500 | 52.36 | 41.28 |
| 510-550 | 52.31 | 38.95 |
| 560-600 | 53.00 | 46.22 |
| 610-650 | 50.12 | 47.56 |
| 660-700 | 40.36 | 31.87 |
Embodiment 2
The preparation method of a kind of goth black fabric, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) dopentacontane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, in the catalysis of concentrated sulphuric acid
Under, it being heated to 110 DEG C, refuxing esterification, cooling, separating-purifying obtains dopentacontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to
Mass concentration is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of dopentacontane dicarboxylic acids；
2) described dopentacontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), its
Middle dopentacontane mono methyl dicarboxylate's concentration is 0.07mol/L, and under nitrogen atmosphere, 85 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 3 hours, be washed out, purify and be dried, obtain product bromo henpentacontane
Carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40%, and dilute sulfuric acid addition is dopentacontane dicarboxylic acids
The 3wt% of mono-methyl；
3), by the ammonia of bromo henpentacontane carboxylic acid Yu 25wt% during 1:2 joins reactor in molar ratio, stirring, in room
The lower reaction of temperature, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 62 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses nitric acid
Silver solution detection, obtains product amino henpentacontane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino henpentacontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino henpentacontane
2% addition concentration of carboxylic acid weight is the sulphuric acid of 45wt%, carries out esterification, and esterification reaction temperature is 220 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；The separated purification of product obtains amino henpentacontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:2.0 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.2MPa, and temperature, at 260 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, three oxidations of the 0.05% of addition p-phthalic acid weight in esterification products
Two antimony and the triphenyl phosphate of p-phthalic acid weight 0.05%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Steadily be evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 270 DEG C, and the response time is 30 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino henpentacontane carboxylic acid glycol ester, and stir 20 points
Clock；Described amino henpentacontane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 2.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 280 DEG C, 50 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 30000.
(3) preparation of goth black fabric
By modified poly ester through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified polyester fiber；Change
Property polyester fiber be woven into fabric after carry out dispersed black dye dyeing carrying out again and increase deep and active amino silicone oil process and obtain spy
Black fabric；Spinning technique is:
The temperature of described extrusion is 290 DEG C；
The pathogenic wind-warm of described cooling is 25 DEG C；
The speed of described winding is 4600m/min；
Filament number is 1.0dtex；
The goth black fabric of gained is under the conditions of temperature is 90 DEG C, and the free volume space of fibrous inside molecule interchain increases 20v/
V%, line density deviation ratio 1.4%, fracture strength 3.9cN/dtex, fracture strength CV value 4.8%, elongation at break is
30.0%, extension at break CV value 9.8%, yarn unevenness CV1.90%, boiling water shrinkage 7.0%, oil content 0.70%.
Table 1: different product deeply arrange after K/S value at different wavelengths
| Wavelength | Goth black fabric | Common fabric |
| 400-450 | 51.80 | 45.12 |
| 460-500 | 52.39 | 41.28 |
| 510-550 | 52.34 | 38.95 |
| 560-600 | 53.13 | 46.22 |
| 610-650 | 50.15 | 47.56 |
| 660-700 | 40.45 | 31.87 |
Embodiment 3
The preparation method of a kind of goth black fabric, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) pentacosane dicarboxylic acid is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 85 DEG C, refuxing esterification, cooling, separating-purifying obtains pentacosane dicarboxylic acid mono-methyl；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of pentacosane dicarboxylic acid；
2) described pentacosane dicarboxylic acid mono-methyl, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Pentacosane dicarboxylic acid mono-methyl concentration is 0.08mol/L, under nitrogen atmosphere, in 90 DEG C of reactions, backflow, produces when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.5 hours, be washed out, purify and be dried, obtain product bromotetradecane carboxylic
Acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 50%, and dilute sulfuric acid addition is pentacosane dicarboxylic acid list first
The 3wt% of ester；
3), by the ammonia of bromotetradecane carboxylic acid Yu 20wt% during 1:2 joins reactor in molar ratio, stirring, in room temperature
Lower reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, uses silver nitrate
Solution detects, and product vacuum drying is obtained product amino tetradecane carboxylic acid；
4) ethylene glycol and amino tetradecane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino tetradecane carboxylic acid
2% addition concentration of weight is the sulphuric acid of 50wt%, carries out esterification, and esterification reaction temperature is 190 DEG C, esterification water quantity of distillate
Reaching more than the 90% of theoretical value is esterification terminal；The separated purification of product obtains amino tetradecane carboxylic acid ethylene glycol
Ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.6 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.3MPa, and temperature, at 255 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, three oxidations of the 0.03% of addition p-phthalic acid weight in esterification products
Two antimony and the triphenyl phosphate of p-phthalic acid weight 0.03%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Steadily be evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 265 DEG C, and the response time is 40 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino tetradecane carboxylic acid glycol ester, and stir 16 points
Clock；Described amino tetradecane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 1.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 276 DEG C, 70 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 22500.
(3) preparation of goth black fabric
By modified poly ester through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified polyester fiber；Change
Property polyester fiber be woven into fabric after carry out dispersed black dye dyeing carrying out again and increase deep and active amino silicone oil process and obtain spy
Black fabric；Spinning technique is:
The temperature of described extrusion is 285 DEG C；
The pathogenic wind-warm of described cooling is 23 DEG C；
The speed of described winding is 4300m/min；
Filament number is 0.6dtex；
The goth black fabric of gained is under the conditions of temperature is 110 DEG C, and the free volume space of fibrous inside molecule interchain increases
30v/v%, line density deviation ratio 1.3%, fracture strength 4.0cN/dtex, fracture strength CV value 4.2%, elongation at break is
33.0%, extension at break CV value 9.9%, yarn unevenness CV1.80%, boiling water shrinkage 7.5%, oil content 0.90%.
Table 1: different product deeply arrange after K/S value at different wavelengths
| Wavelength | Goth black fabric | Common fabric |
| 400-450 | 51.78 | 45.12 |
| 460-500 | 52.32 | 41.28 |
| 510-550 | 52.24 | 38.95 |
| 560-600 | 52.88 | 46.22 |
| 610-650 | 50.01 | 47.56 |
| 660-700 | 40.21 | 31.87 |
Embodiment 4
The preparation method of a kind of goth black fabric, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) eicosane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 85 DEG C, refuxing esterification, cooling, separating-purifying obtains eicosane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of eicosane dicarboxylic acids；
2) described eicosane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Eicosane mono methyl dicarboxylate's concentration is 0.09mol/L, under nitrogen atmosphere, in 80 DEG C of reactions, backflow, produces when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.1 hours, be washed out, purify and be dried, obtain product bromo nonadecane carboxylic
Acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 43%, and dilute sulfuric acid addition is eicosane dicarboxylic acids list first
The 2wt% of ester；
3), by the ammonia of bromo nonadecane carboxylic acid Yu 16wt% during 1:2 joins reactor in molar ratio, stirring, in room temperature
Lower reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 69 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, uses silver nitrate
Solution detects, and product vacuum drying is obtained product amino nonadecane carboxylic acid；
4) ethylene glycol and amino nonadecane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino nonadecane carboxylic acid
2% addition concentration of weight is the sulphuric acid of 42wt%, carries out esterification, and esterification reaction temperature is 160 DEG C, esterification water quantity of distillate
Reaching more than the 90% of theoretical value is esterification terminal；The separated purification of product obtains amino nonadecane carboxylic acid ethylene glycol
Ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.2 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.15MPa, and temperature, at 251 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, three oxidations of the 0.02% of addition p-phthalic acid weight in esterification products
Two antimony and the triphenyl phosphate of p-phthalic acid weight 0.02%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Steadily be evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 262 DEG C, and the response time is 33 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino nonadecane carboxylic acid glycol ester, and stir 17 points
Clock；Described amino nonadecane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 1.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 277 DEG C, 55 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 16000.
(3) preparation of goth black fabric
By modified poly ester through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified polyester fiber；Change
Property polyester fiber be woven into fabric after carry out dispersed black dye dyeing carrying out again and increase deep and active amino silicone oil process and obtain spy
Black fabric；Spinning technique is:
The temperature of described extrusion is 2801 DEG C；
The pathogenic wind-warm of described cooling is 21 DEG C；
The speed of described winding is 4100m/min；
Filament number is 0.4dtex；
The goth black fabric of gained is under the conditions of temperature is 100 DEG C, and the free volume space of fibrous inside molecule interchain increases
20v/v%, line density deviation ratio 1.2%, fracture strength 4.1cN/dtex, fracture strength CV value 4.8%, elongation at break is
35.0%, extension at break CV value 9.3%, yarn unevenness CV1.70%, boiling water shrinkage 7.8%, oil content 1.0%.
Table 1: different product deeply arrange after K/S value at different wavelengths
| Wavelength | Goth black fabric | Common fabric |
| 400-450 | 52.02 | 45.12 |
| 460-500 | 52.45 | 41.28 |
| 510-550 | 52.21 | 38.95 |
| 560-600 | 52.04 | 46.22 |
| 610-650 | 49.88 | 47.56 |
| 660-700 | 40.30 | 31.87 |
Embodiment 5
The preparation method of a kind of goth black fabric, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) melissane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 90 DEG C, refuxing esterification, cooling, separating-purifying obtains melissane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of melissane dicarboxylic acids；
2) described melissane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Melissane mono methyl dicarboxylate's concentration be 0.10mol/L under nitrogen atmosphere, 85 DEG C of reactions, backflow, produce when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.3 hours, be washed out, purify and be dried, obtain product bromo nonacosane carboxylic
Acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40%, and dilute sulfuric acid addition is melissane dicarboxylic acids list first
The 3wt% of ester；
3), by the ammonia of bromo nonacosane carboxylic acid Yu 18wt% during 1:2 joins reactor in molar ratio, stirring, in room
The lower reaction of temperature, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 67 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses nitric acid
Silver solution detection, obtains product amino nonacosane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino nonacosane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino nonacosane
2% addition concentration of carboxylic acid weight is the sulphuric acid of 48wt%, carries out esterification, and esterification reaction temperature is 170 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；The separated purification of product obtains amino nonacosane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.5 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.3MPa, and temperature, at 254 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, the ethylene glycol of the 0.01% of addition p-phthalic acid weight in esterification products
Antimony and the trimethyl phosphate of p-phthalic acid weight 0.03%, under conditions of negative pressure start polycondensation reaction, this staged pressure by
Normal pressure is steadily evacuated to below absolute pressure 500Pa, and temperature controls at 266 DEG C, and the response time is 39 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino nonacosane carboxylic acid glycol ester, and stir 18 points
Clock；Described amino nonacosane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 2.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power drops
To absolute pressure less than 100Pa, reaction temperature controls at 278 DEG C, 60 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 22000.
(3) preparation of goth black fabric
By modified poly ester through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified polyester fiber；Change
Property polyester fiber be woven into fabric after carry out dispersed black dye dyeing carrying out again and increase deep and active amino silicone oil process and obtain spy
Black fabric；Spinning technique is:
The temperature of described extrusion is 289 DEG C；
The pathogenic wind-warm of described cooling is 24 DEG C；
The speed of described winding is 4500m/min；
Filament number is 0.8dtex；
The goth black fabric of gained is under the conditions of temperature is 120 DEG C, and the free volume space of fibrous inside molecule interchain increases
25v/v%, line density deviation ratio 1.0%, fracture strength 4.1cN/dtex, fracture strength CV value 4.5%, elongation at break is
31.0%, extension at break CV value 9.4%, yarn unevenness CV1.50%, boiling water shrinkage 7.2%, oil content 0.8%.
Table 1: different product deeply arrange after K/S value at different wavelengths
| Wavelength | Goth black fabric | Common fabric |
| 400-450 | 51.97 | 45.12 |
| 460-500 | 52.24 | 41.28 |
| 510-550 | 53.01 | 38.95 |
| 560-600 | 53.00 | 46.22 |
| 610-650 | 50.34 | 47.56 |
| 660-700 | 41.27 | 31.87 |
Embodiment 6
The preparation method of a kind of goth black fabric, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) pentatriacontane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, in the catalysis of concentrated sulphuric acid
Under, it being heated to 95 DEG C, refuxing esterification, cooling, separating-purifying obtains pentatriacontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to matter
Amount concentration is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 2wt% of pentatriacontane dicarboxylic acids；
2) described pentatriacontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), its
Middle pentatriacontane mono methyl dicarboxylate's concentration be 0.09mol/L under nitrogen atmosphere, 90 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 2.6 hours, be washed out, purify and be dried, obtain product bromo 34
Alkane carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 45%, and dilute sulfuric acid addition is pentatriacontane dicarboxyl
The 1wt% of acid mono-methyl
3), by the ammonia of bromo tetratriacontane carboxylic acid Yu 20wt% during 1:2 joins reactor in molar ratio, stirring, in room
The lower reaction of temperature, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 69 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses nitric acid
Silver solution detection, obtains product amino tetratriacontane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino tetratriacontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino tetratriacontane
1% addition concentration of carboxylic acid weight is the sulphuric acid of 50wt%, carries out esterification, and esterification reaction temperature is 180 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；The separated purification of product obtains amino tetratriacontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.6 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.4MPa, and temperature, at 256 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, the antimony acetate of the 0.04% of addition p-phthalic acid weight in esterification products
With the NSC 6513 of p-phthalic acid weight 0.02%, under conditions of negative pressure start polycondensation reaction, this staged pressure by
Normal pressure is steadily evacuated to below absolute pressure 500Pa, and temperature controls at 267 DEG C, and the response time is 40 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino tetratriacontane carboxylic acid glycol ester, and stir 18 points
Clock；Described amino tetratriacontane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 2.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 70 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 24000.
(3) preparation of goth black fabric
By modified poly ester through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified polyester fiber；Change
Property polyester fiber be woven into fabric after carry out dispersed black dye dyeing carrying out again and increase deep and active amino silicone oil process and obtain spy
Black fabric；Spinning technique is:
The temperature of described extrusion is 288 DEG C；
The pathogenic wind-warm of described cooling is 21 DEG C；
The speed of described winding is 4200m/min；
Filament number is 0.5dtex；
The goth black fabric of gained is under the conditions of temperature is 130 DEG C, and the free volume space of fibrous inside molecule interchain increases
30v/v%, line density deviation ratio 1.1%, fracture strength 4.0cN/dtex, fracture strength CV value 4.2%, elongation at break is
35.0%, extension at break CV value 9.4%, yarn unevenness CV1.90%, boiling water shrinkage 7.7%, oil content 0.80%.
Table 1: different product deeply arrange after K/S value at different wavelengths
| Wavelength | Goth black fabric | Common fabric |
| 400-450 | 51.68 | 45.12 |
| 460-500 | 52.56 | 41.28 |
| 510-550 | 52.44 | 38.95 |
| 560-600 | 52.89 | 46.22 |
| 610-650 | 50.56 | 47.56 |
| 660-700 | 40.45 | 31.87 |
Embodiment 7
The preparation method of a kind of goth black fabric, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) tetracontane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 100 DEG C, refuxing esterification, cooling, separating-purifying obtains tetracontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of tetracontane dicarboxylic acids；
2) described tetracontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Tetracontane mono methyl dicarboxylate's concentration be 0.06mol/L under nitrogen atmosphere, 80 DEG C of reactions, backflow, produce when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.7 hours, be washed out, purify and be dried, obtain product bromo nonatriacontane carboxylic
Acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 48%, and dilute sulfuric acid addition is tetracontane dicarboxylic acids list first
The 2wt% of ester；
3), by the ammonia of bromo nonatriacontane carboxylic acid Yu 22wt% during 1:2 joins reactor in molar ratio, stirring, in room
The lower reaction of temperature, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses nitric acid
Silver solution detection, obtains product amino nonatriacontane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino nonatriacontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino nonatriacontane
2% addition concentration of carboxylic acid weight is the sulphuric acid of 46wt%, carries out esterification, and esterification reaction temperature is 190 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；The separated purification of product obtains amino nonatriacontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.8 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.2MPa, and temperature, at 258 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, the antimony acetate of the 0.05% of addition p-phthalic acid weight in esterification products
With the trimethyl phosphate of p-phthalic acid weight 0.03%, starting polycondensation reaction under conditions of negative pressure, this staged pressure is by often
Flattening and be surely evacuated to below absolute pressure 500Pa, temperature controls at 268 DEG C, and the response time is 45 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino nonatriacontane carboxylic acid glycol ester, and stir 16 points
Clock；Described amino nonatriacontane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 1.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 75 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 25000.
(3) preparation of goth black fabric
By modified poly ester through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified polyester fiber；Change
Property polyester fiber be woven into fabric after carry out dispersed black dye dyeing carrying out again and increase deep and active amino silicone oil process and obtain spy
Black fabric；Spinning technique is:
The temperature of described extrusion is 287 DEG C；
The pathogenic wind-warm of described cooling is 23 DEG C；
The speed of described winding is 4400m/min；
Filament number is 0.7dtex；
The goth black fabric of gained is under the conditions of temperature is 100 DEG C, and the free volume space of fibrous inside molecule interchain increases
25v/v%, line density deviation ratio 1.3%, fracture strength 4.2cN/dtex, fracture strength CV value 4.2%, elongation at break is
35.5%, extension at break CV value 9.5%, yarn unevenness CV1.75%, boiling water shrinkage 7.3%, oil content 0.85%.
Table 1: different product deeply arrange after K/S value at different wavelengths
| Wavelength | Goth black fabric | Common fabric |
| 400-450 | 51.67 | 45.12 |
| 460-500 | 52.30 | 41.28 |
| 510-550 | 52.45 | 38.95 |
| 560-600 | 53.34 | 46.22 |
| 610-650 | 51.08 | 47.56 |
| 660-700 | 41.23 | 31.87 |
Embodiment 8
The preparation method of a kind of goth black fabric, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) pentatetracontane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, in the catalysis of concentrated sulphuric acid
Under, it being heated to 110 DEG C, refuxing esterification, cooling, separating-purifying obtains pentatetracontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to
Mass concentration is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 2wt% of pentatetracontane dicarboxylic acids；
2) described pentatetracontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), its
Middle pentatetracontane mono methyl dicarboxylate's concentration is 0.07mol/L, and under nitrogen atmosphere, 88 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 2.3 hours, be washed out, purify and be dried, obtain product bromo 44
Alkane carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 45%, and dilute sulfuric acid addition is pentatetracontane dicarboxyl
The 2wt% of acid mono-methyl；
3), by the ammonia of bromo tetratetracontane carboxylic acid Yu 25wt% during 1:2 joins reactor in molar ratio, stirring, in room
The lower reaction of temperature, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is less than 70 DEG C, until
Bubble-free produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses
Silver nitrate solution detects, and product vacuum drying is obtained product amino tetratetracontane carboxylic acid；
4) ethylene glycol and amino tetratetracontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino tetratetracontane
1% addition concentration of carboxylic acid weight is the sulphuric acid of 50wt%, carries out esterification, and esterification reaction temperature is 210 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；The separated purification of product obtains amino tetratetracontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:2.0 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.3MPa, and temperature, at 260 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, the ethylene glycol of the 0.02% of addition p-phthalic acid weight in esterification products
Antimony and the trimethyl phosphate of p-phthalic acid weight 0.05%, under conditions of negative pressure start polycondensation reaction, this staged pressure by
Normal pressure is steadily evacuated to below absolute pressure 500Pa, and temperature controls at 270 DEG C, and the response time is 50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino tetratetracontane carboxylic acid glycol ester, and stir 20 points
Clock；Described amino tetratetracontane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 2.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 280 DEG C, 85 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 30000.
(3) preparation of goth black fabric
By modified poly ester through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified polyester fiber；Change
Property polyester fiber be woven into fabric after carry out dispersed black dye dyeing carrying out again and increase deep and active amino silicone oil process and obtain spy
Black fabric；Spinning technique is:
The temperature of described extrusion is 288 DEG C；
The pathogenic wind-warm of described cooling is 23 DEG C；
The speed of described winding is 4400m/min；
Filament number is 0.7dtex；
The goth black fabric of gained is under the conditions of temperature is 130 DEG C, and the free volume space of fibrous inside molecule interchain increases
30v/v%, line density deviation ratio 1.3%, fracture strength 4.2cN/dtex, fracture strength CV value 4.2%, elongation at break is
35.5%, extension at break CV value 9.5%, yarn unevenness CV1.75%, boiling water shrinkage 7.3%, oil content 0.85%.
Table 1: different product deeply arrange after K/S value at different wavelengths
| Wavelength | Goth black fabric | Common fabric |
| 400-450 | 51.67 | 45.12 |
| 460-500 | 52.36 | 41.28 |
| 510-550 | 52.45 | 38.95 |
| 560-600 | 53.32 | 46.22 |
| 610-650 | 51.08 | 47.56 |
| 660-700 | 41.25 | 31.87 |
Claims (10)
1. a goth black fabric, is characterized in that: the fabric that described goth black fabric is prepared by modified polyester fiber, more black through dispersion
Dyeing carrying out increases deep and active amino silicone oil process and obtains；The material of described modified polyester fiber fabric is modified poly ester
Fiber；Described goth black fabric is under the conditions of temperature is 90～130 DEG C, and the free volume space of fibrous inside molecule interchain increases 20
～30v/v%；Described goth black fabric increases the absorption system of the opaque body of the fabric after deep arrangement between 400～700nm wavelength
Ratio K/the S of number K and the scattering coefficient S of opaque body is greatly improved than common fabric；Described modified poly ester is by polyester and ammonia
Base ethylene glycol fatty acid is constituted, and described amino ethylene glycol fatty acid is dispersed in the molecule interchain of described polyester, and described ammonia
Base ethylene glycol fatty acid has hydrogen bond action with the molecule interchain of described polyester, makes described amino ethylene glycol fatty acid with described
The relative position of the strand of polyester is fixed；
The molecular structure of described amino ethylene glycol fatty acid is:
H2N(CH2)nCOOCH2CH2OOC(CH2)n NH2；
Wherein, n=10-50.
The goth black fabric of one the most according to claim 1, it is characterised in that the line density deviation of described modified polyester fiber
Rate≤0.5%, fracture strength >=3.8cN/dtex, fracture strength CV value≤5.0%, elongation at break is 33.0 ± 3.0%, disconnected
Split elongation CV value≤10.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ±
0.20%.
The goth black fabric of one the most according to claim 1, it is characterised in that described amino ethylene glycol fatty acid accounts for described
The percentage by weight of modified polyester fiber is 0.5～2.5%.
A kind of goth black fabric preparation method the most as claimed in claim 1, is characterized in that: by modified poly ester through metering, extrusion, cold
But, oil, stretch, thermal finalization and winding, prepare modified polyester fiber；Modified polyester fiber disperses after being woven into fabric again
Black dyeing carrying out increases deep and active amino silicone oil process and obtains goth black fabric；Spinning technique is:
The temperature of described extrusion is 280～290 DEG C；
The pathogenic wind-warm of described cooling is 20～25 DEG C；
The speed of described winding is 4000～4600m/min；
Filament number is 0.3～1.0dtex；
The preparation process of described modified poly ester includes:
(1) preparation of amino ethylene glycol fatty acid:
1) binary of fatty acids is added in reactor with the amount of 1:1.5 mol ratio with methanol, under the catalysis of concentrated sulphuric acid, be heated to
80～110 DEG C, refuxing esterification, cooling, separating-purifying obtains binary of fatty acids mono-methyl；Described binary of fatty acids is dodecane two
Carboxylic acid is to the one in dopentacontane dicarboxylic acids；
2) by described binary of fatty acids mono-methyl, lead tetraacetate and lithium bromide during 1:1:1 is dissolved in benzene in molar ratio, wherein binary fat
The concentration of fat acid mono-methyl is 0.05～0.1mol/L, and under nitrogen atmosphere, 80～90 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 2～3 hours, be washed out, purify and be dried, obtain product bromo fat
Acid；
3) by the ammonia of bromo fatty acid and 15～25wt% during 1:2 joins reactor in molar ratio, stirring, the most instead
Should, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is less than 70 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, by product vacuum
It is dried to obtain product amino fatty acid；
4) ethylene glycol and amino fatty acid are stirred for 1.1:2 in molar ratio, and press the 1～3% of amino fatty acid wt
Adding the sulphuric acid that concentration is 40～50wt%, carry out esterification, esterification reaction temperature is 160～220 DEG C, esterification water quantity of distillate
Reaching more than the 90% of theoretical value is esterification terminal；The separated purification of product obtains amino ethylene glycol fatty acid；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
Use p-phthalic acid and ethylene glycol as raw material, carry out esterification after being made into uniform sizing material, obtain esterification products；Ester
Changing reaction to pressurize in nitrogen atmosphere, Stress control is at normal pressure～0.3MPa, and temperature is at 250～260 DEG C, and esterification water quantity of distillate reaches
It is esterification terminal to more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction coarse vacuum stage, esterification products adds catalyst and stabilizer, starts under conditions of negative pressure
Polycondensation reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature controls at 260～270 DEG C, reaction
Time is 30～50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino ethylene glycol fatty acid, and stir；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 275～280 DEG C, response time 50～90 minutes；
Prepare modified poly ester.
The preparation method of a kind of goth black fabric the most according to claim 4, it is characterised in that described ethylene glycol is right with described
The mol ratio of phthalic acid is 1.2～2.0:1.
The preparation method of a kind of goth black fabric the most according to claim 4, it is characterised in that described catalyst is selected from three oxygen
Change the one in two antimony, antimony glycol and antimony acetate, catalyst amount be described p-phthalic acid weight 0.01%～
0.05%.
The preparation method of a kind of goth black fabric the most according to claim 4, it is characterised in that described stabilizer is selected from phosphoric acid
One in triphenylmethyl methacrylate, trimethyl phosphate and NSC 6513, stabilizing agent dosage is described p-phthalic acid weight
0.01%～0.05%.
The preparation method of a kind of goth black fabric the most according to claim 4, it is characterised in that add amino fatty acid second two
Stirring after alcohol ester, the time is 15～20 minutes.
The preparation method of a kind of goth black fabric the most according to claim 4, it is characterised in that be washed with deionized water to without bromine
Silver nitrate solution detection is used till ion.
The preparation method of a kind of goth black fabric the most according to claim 4, it is characterised in that described concentrated sulphuric acid refers to matter
Amount concentration is the sulphuric acid of 70～80%, and concentrated sulphuric acid addition is the 1～3wt% of binary of fatty acids；Described a certain amount of dilute sulfuric acid
Referring to the sulphuric acid that mass concentration is 40～50%, dilute sulfuric acid addition is the 1～3wt% of binary of fatty acids mono-methyl.
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| CN1377380A (en) * | 1999-08-06 | 2002-10-30 | 伊斯曼化学公司 | Polyesters having a controlled melting point and fibers formed therefrom |
| CN103145957A (en) * | 2013-03-21 | 2013-06-12 | 宁波大发化纤有限公司 | Method for producing low-melting-point renewable polyester for sheath-core polyester through glycol degradation |
| CN104131360A (en) * | 2014-06-17 | 2014-11-05 | 福建百宏聚纤科技实业有限公司 | Micro-nano modified super bright polyester fibers and preparation method thereof |
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| US20040005457A1 (en) * | 2002-07-03 | 2004-01-08 | Kimberly-Clark Worldwide, Inc. | Methods of improving the softness of fibers and nonwoven webs and fibers and nonwoven webs having improved softness |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377380A (en) * | 1999-08-06 | 2002-10-30 | 伊斯曼化学公司 | Polyesters having a controlled melting point and fibers formed therefrom |
| CN103145957A (en) * | 2013-03-21 | 2013-06-12 | 宁波大发化纤有限公司 | Method for producing low-melting-point renewable polyester for sheath-core polyester through glycol degradation |
| CN104131360A (en) * | 2014-06-17 | 2014-11-05 | 福建百宏聚纤科技实业有限公司 | Micro-nano modified super bright polyester fibers and preparation method thereof |
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