CN106432670A - Preparation method of organic silicon-modified polyurethane copolymer fabric softener - Google Patents
Preparation method of organic silicon-modified polyurethane copolymer fabric softener Download PDFInfo
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- CN106432670A CN106432670A CN201610826047.2A CN201610826047A CN106432670A CN 106432670 A CN106432670 A CN 106432670A CN 201610826047 A CN201610826047 A CN 201610826047A CN 106432670 A CN106432670 A CN 106432670A
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- organic silicon
- modified polyurethane
- silicon modified
- preparation
- polyurethane copolymer
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- 239000004814 polyurethane Substances 0.000 title claims abstract description 45
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002979 fabric softener Substances 0.000 title claims abstract description 18
- -1 polysiloxane Polymers 0.000 claims abstract description 29
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 229920000570 polyether Polymers 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004970 Chain extender Substances 0.000 claims abstract description 8
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 7
- 229920005862 polyol Polymers 0.000 claims abstract description 7
- 150000003077 polyols Chemical class 0.000 claims abstract description 7
- 125000005442 diisocyanate group Chemical group 0.000 claims abstract description 6
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 6
- 239000012974 tin catalyst Substances 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 40
- 239000010703 silicon Substances 0.000 claims description 40
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 39
- 229920000642 polymer Polymers 0.000 claims description 13
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 7
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 7
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 4
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 4
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 3
- 150000002009 diols Chemical class 0.000 claims description 3
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical group [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 150000002191 fatty alcohols Chemical class 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 4
- 238000004383 yellowing Methods 0.000 abstract description 2
- 229920001730 Moisture cure polyurethane Polymers 0.000 abstract 2
- 125000003277 amino group Chemical group 0.000 abstract 1
- 239000004902 Softening Agent Substances 0.000 description 19
- 239000003921 oil Substances 0.000 description 10
- 229920002545 silicone oil Polymers 0.000 description 7
- 238000007334 copolymerization reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 210000000481 breast Anatomy 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical group NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- WBYWAXJHAXSJNI-SREVYHEPSA-N Cinnamic acid Chemical compound OC(=O)\C=C/C1=CC=CC=C1 WBYWAXJHAXSJNI-SREVYHEPSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000005233 alkylalcohol group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229930016911 cinnamic acid Natural products 0.000 description 1
- 235000013985 cinnamic acid Nutrition 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 1
- 125000005474 octanoate group Chemical group 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/2805—Compounds having only one group containing active hydrogen
- C08G18/285—Nitrogen containing compounds
- C08G18/2865—Compounds having only one primary or secondary amino group; Ammonia
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
- D06M15/568—Reaction products of isocyanates with polyethers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/08—Polyurethanes from polyethers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/11—Oleophobic properties
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Dispersion Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a preparation method of an organic silicon-modified polyurethane copolymer fabric softener. The method comprises the following steps: (a) carrying out a stirring reaction on polyether polyol, a hydroxyl-terminated polysiloxane linear body and diisocyanate for 2-3h at the temperature of 75-85 DEG C under the action of a tin catalyst, so as to obtain an isocyanate-terminated organic silicone-modified polyurethane prepolymer; (b) adding a small molecular amine chain extender into the organic silicone-modified polyurethane prepolymer, and carrying out a stirring reaction for 1-2h at the temperature of 50-60 DEG C, so as to obtain an organic silicon-modified polyurethane copolymer; (c) evenly mixing the organic silicon-modified polyurethane copolymer obtained in the step (b) with an emulsifying agent at the temperature of 50-70 DEG C, and slowly adding deionized water into the mixture for emulsifying, so as to obtain the organic silicon-modified polyurethane copolymer fabric softener. The softener prepared by the method is good in stability, endows fabric with excellent softnesss, smoothness and hydrophilic property, has excellent yellowing resistance, and can maintain the brightness of the light-colored fabrics and the whiteness of the white fabrics.
Description
Technical field
The invention belongs to the preparing technical field of polyurethane textile auxiliary agent, more particularly to a kind of organic silicon modified polyurethane are altogether
The preparation method of polymers fabric softener.
Background technology
Fabric softener is a kind of textile auxiliary that can give the special feel of fabric, and wherein silicone softening agent is weaving
Extremely important and conventional one kind in product softening agent.Silicone softening agent is mainly polydimethylsiloxane class softening agent, has
Abundant methyl and good molecule flexibility, can effectively reduce the static and dynamic friction coefficient between fiber, reach good softness
Effect.But because polydimethylsiloxane (i.e. silicone oil) does not have hydrophilic group and the group with fiber crosslinking, fabric after arrangement in itself
Hydrophilic and washability are poor, cause snugness of fit to decline, soft not durable.For improving this problem, people have developed in succession
The group modified silicone softening agent of difference in functionality, wherein amino-modified silicone oil are that performance is best, most widely used in the market
General softening agent, it can give the excellent flexibility of fabric, resilience and hydrophilic.But the presence due to amino, amino
Modified silicon oil reduces white fabrics whiteness (fabric xanthochromia) when heating or bake, and affects color and luster and the vividness of light coloured fabrics,
And the softening agent less stable of this kind of silicone oil preparation, easily occur layering, floating oil during storage, transport and use, break
The shortcomings of breast and oil mark stain.
Content of the invention
The present invention is improved for problem above, is provided a kind of excellent organic silicon modified polyurethane copolymer of feel and is knitted
The preparation method of thing softening agent.Softening agent prepared by the present invention not only remain the flexibility of amino-modified silicone oil, resilience and
Hydrophilic, gives " soft glutinous but non-greasy " feel style of fabric uniqueness, and fabric hydrophilic is good, and xanthochromia is little, can keep shallow
The whiteness of the vividness and white fabrics of yarn dyed fabric, and with excellent stability during storage, transport and use.Its skill
Art scheme is：
A kind of preparation method of organic silicon modified polyurethane copolymer fabric softener, its preparation method includes following step
Suddenly：
A) preparation of organic silicon modified polyurethane performed polymer：By by polyether polyol and hydroxy-terminated polysiloxane linear body
Mixture, diisocyanate and tin catalyst, three is with 47.4～62.7：36.3～52.6：0.1～0.2 mass ratio is 75
DEG C～85 DEG C of 2～3h of stirring reaction, obtain isocyanate-terminated organic silicon modified polyurethane performed polymer；
B) chain extension of organic silicon modified polyurethane performed polymer：Small molecule amine is added in organic silicon modified polyurethane performed polymer
Class chain extender, small molecule amine chain extender consumption is the 0.5%～3% of organic silicon modified polyurethane performed polymer quality fraction, 50
DEG C～60 DEG C of 1～2h of stirring reaction；
C) emulsifying of organic silicon modified aqueous polyurethane copolymer：Organic silicon modified polyurethane copolymerization in step b) gained
In thing add emulsifying agent, 50 DEG C～70 DEG C mix homogeneously, emulsifier for organic silicon polyurethane copolymer quality 5%～
30%, adding deionized water carries out emulsifying, and deionized water consumption is uniform in 60～90%, 30 minutes of whole system quality
Completion of dropping, obtains final product organic silicon modified polyurethane copolymer fabric softener.
A kind of preparation method of described organic silicon modified polyurethane copolymer fabric softener, polyethers described in step a)
Polyhydric alcohol is Polyethylene Glycol or Polyoxypropylene diol, and number-average molecular weight is 1000～2000；Diisocyanate is different Fo Er
One or two mixture in ketone diisocyanate or hexamethylene diisocyanate；Hydroxy-terminated polysiloxane linear body is
Number-average molecular weight 1000～3000 ethoxy polysiloxanes or hydroxypropyl based polysiloxane in one or two mixture；
Polyether polyol with the mass fraction of hydroxy-terminated polysiloxane linear body in the mixture of hydroxy-terminated polysiloxane linear body is
25%～40%；Tin catalyst is stannous octoate or dibutyl tin laurate.
A kind of preparation method of described organic silicon modified polyurethane copolymer softening agent, step b) the small molecule amine
Chain extender is the mixture of diethylamine or triethylamine or both.
A kind of preparation method of described organic silicon modified polyurethane copolymer softening agent, the step c) emulsifying agent is different
Structure C12～C13 fatty alcohol-polyoxyethylene ether, isomery C12～C13 fatty alcohol-polyoxyethylene ether or isomery C12～C13 poly alkyl alcohol
The mixture of one or more in oxygen vinyl Ether.
The present invention compared with prior art, has an advantage in that：By polyether polyol, diisocyanate, the poly- silicon of terminal hydroxy group
The copolymerization of oxygen alkane is obtained block copolymer, and not only the carbamate chain link containing certain rigidity and polarity, can give fabric only
Special " soft glutinous but non-greasy " feel style, and the low pole of the polyethers that adds water " soft section ", it is ensured that the hydrophilic of fabric, give
The excellent wearing comfort of fabric.The softening agent for preparing after Over emulsfication not only has excellent storage, transport and using stable
Property good, the problems such as being less prone to layering, floating oil, breakdown of emulsion and oil mark and stain, and fabric whiteness is affected little, maintains white and knit
The high whiteness of thing and the original color and luster of light coloured fabrics and vividness.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail, but the scope of protection of present invention not office
It is limited to the scope that example represents.
Embodiment 1, concretely comprises the following steps：
A) 37.5g Polyoxypropylene diol (molecular weight 1800), 22.5g hydroxypropyl are added in the reactor of dry cleansing
Based polysiloxane (molecular weight 2600), 39.82g hexamethylene diisocyanate (HDI), add catalyst dibutyltin cinnamic acid dibutyl
Stannum 0.18g, obtains isocyanate-terminated organic silicon modified polyurethane performed polymer in 80 DEG C of stirring reactions 2h.
B) 1.5g triethylamine chain extender continuously added, 55 DEG C of stirring reactions 2.0h, obtain organic silicon modified polyurethane copolymerization
Body.
C) by the copolymer for preparing in 70 DEG C and 8g isomery C12～C13 fatty alcohol-polyoxyethylene ether (6EO) and 6g isomery
C12～C13 fatty alcohol-polyoxyethylene ether (8EO) mix homogeneously, then uniform Deca 450g deionized water carries out breast in 30 minutes
Change, obtain organic silicon modified polyurethane copolymer softening agent.
Embodiment 2, concretely comprises the following steps：
A) in the reactor of dry cleansing, 43.35g poly- second dihydroxylic alcohols (molecular weight 1200), 15.5g ethoxy is added to gather
Siloxanes (molecular weight 1500), 41.02g isophorone diisocyanate (IPDI), add octoate catalyst stannous 0.13g,
75 DEG C of stirring reactions 2.5h obtain isocyanate-terminated organic silicon modified polyurethane performed polymer.
B) 0.8g diethyl amine chainextender continuously added, 50 DEG C of stirring reactions 1.5h, obtain organic silicon modified polyurethane copolymerization
Body.
C) copolymer for preparing is mixed all with 4.0g isomery C12～C13 fatty alcohol-polyoxyethylene ether (7EO) at 60 DEG C
Even, then in 30 minutes, uniform Deca 200g deionized water carries out emulsifying, obtains organic silicon modified polyurethane copolymer softening agent.
Softening agent application effect is tested referring to table 1：
The softening agent of the present invention of the table 1 commercially available amino-modified silicone oil softening agent excellent with screenability is arranged to fabric sofetening
Contrast on effect：
| Contrast on effect | Blank sample | Embodiment 1 | Embodiment 2 | Amino-modified silicone oil softening agent |
| Soft rank (1-5 level) | 1 grade | 5 grades | 5 grades | 4-5 level |
| Smooth rank (1-5 level) | 1 grade | 4 grades | 4 grades | 3-4 level |
| Hydrophilic | 6.12s | 7.23s | 8.15s | 135s |
| Whiteness | 145.68 | 146.29 | 147.01 | 144.56 |
| High-temperature stability | / | Boil stable | Boil stable | 82 DEG C of floating oils |
| Shear stability | / | Stable | Stable | Slight floating oil |
Soft rank and smooth rank are all tested using Handle-O-Meter pliability tester；Hydrophilic is tested
According to AATCC79-2010《Textile water absorption》；Whiteness test is according to GB/T 8424.2-2001《Textile color stability is tested
Objective ranking method with respect to whiteness》；The method of testing of high-temperature stability is as follows：The solution of configuration 20g/L sample, is heated to
100 DEG C, after cooling, see whether surface has floating oil phenomenon；The method of testing of shear stability is as follows：Prepare the solution of 40g/L
500mL, adjusts pH value 5 and 10 with acetic acid or sodium hydroxide, with agitator in 1500rpm stirring 30 minutes, maintenance solution temperature
At 50 DEG C, degree sees whether surface has floating oil phenomenon.
Softening agent of the present invention be can be seen that from the data of table 1 soft all than amino-modified silicone oil pliability and smooth degree
Soft dose of protrusion, forms unique " soft glutinous but non-greasy " feel style, and with excellent hydrophilic, has little influence on fabric
Hydrophilic, and the fabric that far superior to amido silicon oil is processed, while anti-yellowing property and stability protrusion, especially high-temperature stable
Property and shear stability so as to more extensive using process conditions.
Claims (8)
1. a kind of preparation method of organic silicon modified polyurethane copolymer fabric softener, its preparation method is comprised the following steps：
A) preparation of organic silicon modified polyurethane performed polymer：By the mixing by polyether polyol and hydroxy-terminated polysiloxane linear body
Thing, diisocyanate and tin catalyst, three is with 47.4～62.7：36.3～52.6：0.1～0.2 mass ratio 75 DEG C～
85 DEG C of 2～3h of stirring reaction, obtain isocyanate-terminated organic silicon modified polyurethane performed polymer；
B) chain extension of organic silicon modified polyurethane performed polymer：In organic silicon modified polyurethane performed polymer, add small molecule amine to expand
Chain agent, small molecule amine chain extender consumption is the 0.5%～3% of organic silicon modified polyurethane performed polymer quality fraction, 50 DEG C～
60 DEG C of 1～2h of stirring reaction；
C) emulsifying of organic silicon modified aqueous polyurethane copolymer：In the organic silicon modified polyurethane copolymer of step b) gained
Emulsifying agent, 50 DEG C～70 DEG C mix homogeneously is added, emulsifier is the 5%～30% of organic silicon polyurethane copolymer quality,
Adding deionized water carries out emulsifying, and deionized water consumption is uniform Deca in 60～90%, 30 minutes of whole system quality
Finish, obtain final product organic silicon modified polyurethane copolymer fabric softener.
2. the preparation method of a kind of organic silicon modified polyurethane copolymer fabric softener according to claim 1, which is special
Levy and be：Polyether polyol described in step a) is Polyethylene Glycol or Polyoxypropylene diol, number-average molecular weight 1000～
2000.
3. the preparation method of a kind of organic silicon modified polyurethane copolymer fabric softener according to claim 1, which is special
Levy and be：Step a) the diisocyanate be the one kind in isophorone diisocyanate or hexamethylene diisocyanate or
Two kinds of mixture.
4. the preparation method of a kind of organic silicon modified polyurethane copolymer fabric softener according to claim 1, which is special
Levy and be：Step a) the hydroxy-terminated polysiloxane linear body be number-average molecular weight 1000～3000 ethoxy polysiloxanes
Or the mixture of one or two in hydroxypropyl based polysiloxane.
5. the preparation method of a kind of organic silicon modified polyurethane copolymer fabric softener according to claim 1, which is special
Levy and be：Step a) the polyether polyol is linear with hydroxy-terminated polysiloxane in the mixture of hydroxy-terminated polysiloxane linear body
The mass fraction of body is 25%～40%.
6. the preparation method of a kind of organic silicon modified polyurethane copolymer fabric softener according to claim 1, which is special
Levy and be：Step a) the tin catalyst is stannous octoate or dibutyl tin laurate.
7. the preparation method of a kind of organic silicon modified polyurethane copolymer fabric softener according to claim 1, which is special
Levy and be：Step b) the small molecule amine chain extender is the mixture of diethylamine or triethylamine or both.
8. the preparation method of a kind of organic silicon modified polyurethane copolymer fabric softener according to claim 1, which is special
Levy and be：Step c) the emulsifying agent is isomery C12～C13 fatty alcohol-polyoxyethylene ether, isomery C12～C13 fatty alcohol polyoxy
The mixture of one or more in vinyl Ether or isomery C12～C13 fatty alcohol-polyoxyethylene ether.
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