CN103668519B - A kind of Multifunctional cellulose fiber and preparation method thereof - Google Patents
A kind of Multifunctional cellulose fiber and preparation method thereof Download PDFInfo
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- CN103668519B CN103668519B CN201310647195.4A CN201310647195A CN103668519B CN 103668519 B CN103668519 B CN 103668519B CN 201310647195 A CN201310647195 A CN 201310647195A CN 103668519 B CN103668519 B CN 103668519B
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- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920000297 Rayon Polymers 0.000 claims abstract description 65
- 238000009987 spinning Methods 0.000 claims abstract description 51
- 229920002678 cellulose Polymers 0.000 claims abstract description 43
- 239000001913 cellulose Substances 0.000 claims abstract description 43
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 41
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 41
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 41
- 239000012452 mother liquor Substances 0.000 claims abstract description 34
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 238000012805 post-processing Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 47
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 24
- 230000001112 coagulating effect Effects 0.000 claims description 16
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 14
- 238000006477 desulfuration reaction Methods 0.000 claims description 13
- 230000023556 desulfurization Effects 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 235000010265 sodium sulphite Nutrition 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- -1 sodium alkyl benzene Chemical class 0.000 claims description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 230000003009 desulfurizing effect Effects 0.000 claims description 6
- 229940077388 benzenesulfonate Drugs 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 4
- 239000003945 anionic surfactant Substances 0.000 claims description 3
- 239000002280 amphoteric surfactant Substances 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 10
- 239000002253 acid Substances 0.000 abstract description 9
- 239000003063 flame retardant Substances 0.000 abstract description 9
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 9
- 229920005591 polysilicon Polymers 0.000 abstract description 9
- 239000004745 nonwoven fabric Substances 0.000 abstract description 2
- 238000009941 weaving Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 7
- 239000003513 alkali Substances 0.000 description 6
- FPVGTPBMTFTMRT-NSKUCRDLSA-L fast yellow Chemical compound [Na+].[Na+].C1=C(S([O-])(=O)=O)C(N)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 FPVGTPBMTFTMRT-NSKUCRDLSA-L 0.000 description 6
- 230000003068 static effect Effects 0.000 description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 230000002421 anti-septic effect Effects 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000000554 physical therapy Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of Multifunctional cellulose fiber and preparation method thereof, containing cellulose, Ag/SiO in described Multifunctional cellulose fiber
2, ZrO
2, Fe
2o
3and polysilicon acid.Preparation method comprises following steps: (1) is by ZrO
2, Ag/SiO
2, Fe
2o
3add in deionized water, add dispersant evenly, be made into multi-functional interpolation mother liquor.(2) sodium metasilicate deionized water is mixed with solution of sodium metasilicate through.(3) solution of sodium metasilicate through is joined yellow terminate after in the viscose solution filtered in arbitrary step, multi-functional interpolation mother liquor is joined in spinning viscose, obtains multi-functional blended viscose solution.(4) by multi-functional blended viscose solution spinning moulding, obtain described Multifunctional cellulose fiber through post processing.Multifunctional cellulose fiber of the present invention has the several functions such as fire-retardant, antibacterial, far infrared generation simultaneously, can be widely used in the weaving such as family expenses, public place and non-woven fabric.
Description
Technical field
The present invention relates to functional cellulose fibre technology field, be specifically related to a kind of Multifunctional cellulose fiber.
Background technology
Fire resistant viscose fiber because having not molten drop, the incomparable premium properties of the synthetic fiber such as biodegradable, moisture absorption is breathed freely, thus there is good development prospect, development in recent years is rapid, market scale constantly expands, Application Areas constantly extends to home-use textiles, toy for children, the vehicles, the drapery of public place, Work Clothes and fireproof-clothes, military and industrial coat, underwear, Heat-preventing clothes lining etc.
Along with more and more stricter to flame-retardancy requirements such as the draperies of household textiles, public place in the world, to the demand of fire resistance fibre and textiles thereof also in continuous expansion, many product anti-flammability indexs are as the enforceable product standard of one, and flame-retardancy requirements is also a basic function of product.
The market demand has expedited the emergence of the production development of fire resistance fibre, and the Fire resistant viscose fiber on market mainly contains several series such as silicon system, phosphorus system, phosphorus nitrogen system, but majority only possesses anti-flaming function, has other functional product favourable to health and then seldom occurs.Along with improving constantly of people's living standard, require also in raising to the functionalization of product, single anti-flaming function is the prerequisite basic function of product, under the prerequisite meeting anti-flaming function, there is other function again, as restraining and sterilizing bacteria, far infrared, anion etc., the favor of consumer will inevitably be subject to, and market exactly lack at present the product of this type of multifunctional fibre especially Multifunctional cellulose fiber.
Summary of the invention
First technical problem to be solved by this invention is: for the problem of the shortage Multifunctional cellulose fiber existed in prior art, provide a kind of Multifunctional cellulose fiber, and this cellulose fibre has fire-retardant, antibacterial and far infrared generation several functions.
Second technical problem to be solved by this invention is: for the problem of the shortage Multifunctional cellulose fiber existed in prior art, there is provided a kind of preparation method of Multifunctional cellulose fiber, cellulose fibre prepared by the method has fire-retardant, antibacterial and far infrared generation several functions.
For solving above-mentioned first technical problem, technical scheme of the present invention is:
A kind of Multifunctional cellulose fiber, containing cellulose, Ag/SiO in described Multifunctional cellulose fiber
2, ZrO
2, Fe
2o
3and polysilicon acid.
Further, in described Multifunctional cellulose fiber by weight percentage, contain: Ag/SiO
20.5 ~ 3.5%(presses SiO
2meter), ZrO
21.2 ~ 6.5%, Fe
2o
30.02 ~ 0.1%, polysilicon acid 13.5 ~ 35%, cellulose 56 ~ 84%.
For solving above-mentioned second technical problem, technical scheme of the present invention is:
A preparation method for Multifunctional cellulose fiber, comprises following steps:
(1) multi-functional interpolation mother liquor is prepared: by ZrO
2, Ag/SiO
2, Fe
2o
3join in deionized water and mix, add dispersant evenly, be made into multi-functional interpolation mother liquor.
(2) solution of sodium metasilicate through is prepared: sodium metasilicate deionized water is mixed with solution of sodium metasilicate through.
(3) preparation of cellulose viscose glue: employing cellulose pulp is raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow step obtain cellulose viscose solution, and then obtain spinning viscose through dissolving, deaeration and filtration step.
(4) prepare multi-functional blended viscose solution: the solution of sodium metasilicate through that step (2) obtains is joined yellow in step (3) terminate after in the viscose solution filtered in arbitrary step, the addition of sodium metasilicate is (by SiO
2meter) be 15 ~ 50% of the fine quality of first in cellulose sulfonate, first fibre 8 ~ 15wt% is contained in cellulose yellow acid fat after adding sodium metasilicate, alkali 5 ~ 10wt%, viscosity 30 ~ 70s(falling ball viscosity), multi-functional interpolation mother liquor is joined in spinning viscose by injection before spinning before spinning, Ag/SiO in described multi-functional interpolation mother liquor
2, ZrO
2, Fe
2o
3addition be respectively 0.5 ~ 5%, 1.2 ~ 10% and 0.02 ~ 1% of the fine quality of first in spinning viscose, obtain described multi-functional blended viscose solution.
(5) co-blended spinning: by the spinning in coagulating bath of described multi-functional blended viscose solution, draw forming, then through comprising washing, desulfurization, the post-processing step that oils obtain described Multifunctional cellulose fiber.
Preferred a kind of technical scheme, by described Ag/SiO
2, ZrO
2, Fe
2o
3join in deionized water by the weight ratio of 0.5 ~ 5:1.2 ~ 10:0.02 ~ 1 and mix, add dispersant evenly, be made into multi-functional interpolation mother liquor.
Preferably, in described multi-functional interpolation mother liquor, the addition of Ag is the particle diameter of 0.1 ~ 1%, described Ag of the fine quality of first in cellulose sulfonate is 0.02 ~ 0.5 μm, described ZrO
2and Fe
2o
3particle diameter be 0.1 ~ 1 μm.
Preferably, the temperature of described coagulating bath is 40 ~ 60 DEG C, containing sulfuric acid 90 ~ 150g/l, zinc sulfate 5 ~ 50g/l, sodium sulphate 270 ~ 350g/l in described coagulating bath.
Preferably, the total stretch ratio of described drawing-off is 10 ~ 300%.
Preferably, described dispersant is anion surfactant or amphoteric surfactant.
As further preferred, described dispersant is at least one in sodium alkyl benzene sulfonate, sodium alkyl sulfate or alkyl ethoxy sulfobetaines.
Improve as one, use sodium sulfite as desulfurizing agent during described desulfurization, the concentration 5 ~ 15g/l of described sodium sulfite, temperature 80 ~ 95 DEG C.
Owing to have employed technique scheme, the invention has the beneficial effects as follows:
Containing cellulose, Ag/SiO in Multifunctional cellulose fiber of the present invention
2, ZrO
2, Fe
2o
3and polysilicon acid, wherein, Ag/SiO
2as a kind of antibiotic bactericide, impart cellulosic fibrous product antibacterial functions, and compared with the anti-bacterial fibre utilizing the silver system anti-bacterial fibre that is prepared from of inorganic antiseptic containing silver and organic antibacterial agent to prepare, overcome the poor heat resistance of organic anti-bacterial finishing agent, easily stripping, shortcoming that Long-Time Service easily produces drug resistance, compare organic antibacterial agent and there is broad-spectrum antiseptic, efficient, lasting and features such as high safety, the every field such as therefore can be widely used in medical treatment, clothes, family are spun, and by ZrO in the present invention
2, SiO
2, Fe
2o
3combinationally use, product is made to have possessed again far infrared generation effect, have and absorb and emitting far-infrared function, the far infrared of certain wavelength in use launched by fiber, the far infrared of the radiation such as sunlight or human body can be absorbed simultaneously, own temperature is raised, there is special health care, physical therapy function, its far infrared mechanism of production: a lot of inorganic compound, as oxide, carbide, borides etc. all have far infrared radiation characteristic, what often select is oxide, as alundum (Al2O3), zinc oxide, zirconia, magnesia, titanium dioxide and silica etc., due to the result that far infrared radiation is lattice vibration, a kind of material can not all have comparatively high radiant rate one section of wave-length coverage, therefore the complementary effect of multiple material can be utilized, therefore select the mixture of multiple above-mentioned substance to do far-infrared functional material, the preferred ZrO of the present invention
2, SiO
2, Fe
2o
3combinationally use, due to ZrO
2, SiO
2, Fe
2o
3all high temperature resistant, three enters in fiber, also helps the fire-retardant and resistance to elevated temperatures improving fiber.
The sodium metasilicate added in the present invention resolves into silicic acid in coagulating bath, and silicic acid aggregates into polysilicon acid further, and the flame retardant constituent playing fire retardation is in the fibre polysilicon acid, the ZrO added at the same time
2, SiO
2, Fe
2o
3synergy under, make fiber have higher resistance to elevated temperatures and further increase flame retardant effect, simultaneously can not produce toxic gas again when fiber burns, only produce a small amount of smog and CO, CO
2gas, therefore, cellulose fibre of the present invention not only possesses the several functions such as fire-retardant, antibacterial, far infrared generation, and it is when same addition, has better high temperature resistant and flame retardant effect than independent silicon-series five-retardant.
Multifunctional cellulose fiber of the present invention has the several functions such as fire-retardant, antibacterial, far infrared generation simultaneously, can be widely used in the weaving such as family expenses, public place and non-woven fabric, to environmental protect condition, promotes that user is healthy, plays good action.
Detailed description of the invention
The present invention is set forth further below in conjunction with specific embodiment.
Embodiment 1
A kind of Multifunctional cellulose fiber, in described over dry Multifunctional cellulose fiber by weight percentage, contains: Ag/SiO
21.0%(presses SiO
2meter), ZrO
21.5%, Fe
2o
30.05%, polysilicon acid 15.5%, cellulose 81.95%.
Embodiment 2
A kind of Multifunctional cellulose fiber, in described over dry Multifunctional cellulose fiber by weight percentage, contains: Ag/SiO
23.0%(presses SiO
2meter), ZrO
23.5%, Fe
2o
30.08%, polysilicon acid 25%, cellulose 68.42%.
Embodiment 3
A kind of Multifunctional cellulose fiber, in described over dry Multifunctional cellulose fiber by weight percentage, contains: Ag/SiO
22.5%(presses SiO
2meter), ZrO
25.5%, Fe
2o
30.1%, polysilicon acid 30%, cellulose 61.9%.
Embodiment 4
A preparation method for Multifunctional cellulose fiber, comprises following steps:
(1) by ZrO
2, Ag/SiO
2, Fe
2o
3join in deionized water and mix, add anion surfactant and be uniformly dispersed, be made into multi-functional interpolation mother liquor.
(2) sodium metasilicate deionized water is mixed with solution of sodium metasilicate through.
(3) adopt cellulose pulp to be raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow step obtain cellulose viscose solution, and then obtain spinning viscose through dissolving, deaeration and filtration step.
(4) solution of sodium metasilicate through that step (2) obtains is joined yellow in step (3) terminate after viscose solution in, the addition of sodium metasilicate is (by SiO
2meter) be 20% of the fine quality of first in cellulose sulfonate, the fine 9.2wt% of first is contained in cellulose yellow acid fat after adding sodium metasilicate, alkali 7.5wt%, the viscosity that viscosity 40s(falling ball method measures), multi-functional interpolation mother liquor is joined in spinning viscose by injection before spinning before spinning, Ag/SiO in described multi-functional interpolation mother liquor
2, ZrO
2, Fe
2o
3addition be respectively 1%, 8% and 1% of the fine quality of first in spinning viscose, in described multi-functional interpolation mother liquor, the addition of Ag is 0.6% of the fine quality of first in cellulose sulfonate, with spinning viscose through static or dynamically mix and obtain described multi-functional blended viscose solution.
(5) by the spinning in coagulating bath of described multi-functional blended viscose solution, draw forming, then after washing, desulfurization, the post processing that oils, described Multifunctional cellulose fiber is obtained.
Embodiment 5
A preparation method for Multifunctional cellulose fiber, comprises following steps:
(1) by ZrO
2, Ag/SiO
2, Fe
2o
3join in deionized water and mix, add dispersant sodium alkyl benzene sulfonate and be uniformly dispersed, be made into multi-functional interpolation mother liquor.
(2) sodium metasilicate deionized water is mixed with solution of sodium metasilicate through.
(3) adopt cellulose pulp to be raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow step obtain cellulose viscose solution, and then obtain spinning viscose through dissolving, deaeration and filtration step.
(4) solution of sodium metasilicate through that step (2) obtains is joined yellow in step (3) to terminate in the viscose solution in rear dissolving step, the addition of sodium metasilicate is (by SiO
2meter) be 30% of the fine quality of first in cellulose sulfonate, the fine 12wt% of first is contained in cellulose yellow acid fat after adding sodium metasilicate, alkali 10wt%, the viscosity that viscosity 65s(falling ball method measures), multi-functional interpolation mother liquor is joined in spinning viscose by injection before spinning before spinning, Ag/SiO in described multi-functional interpolation mother liquor
2, ZrO
2, Fe
2o
3addition be respectively 3%, 6% and 0.5% of the fine quality of first in spinning viscose, in described multi-functional interpolation mother liquor, the addition of Ag is 0.88% of the fine quality of first in cellulose sulfonate, obtains described multi-functional blended viscose solution with spinning viscose through dynamically mixing.
(5) by the spinning in coagulating bath of described multi-functional blended viscose solution, draw forming, then after washing, desulfurization, the post processing that oils, described Multifunctional cellulose fiber is obtained, use sodium sulfite as desulfurizing agent during desulfurization, the concentration 9g/l of described sodium sulfite, temperature 85 DEG C.
Embodiment 6
A preparation method for Multifunctional cellulose fiber, comprises following steps:
(1) by ZrO
2, Ag/SiO
2, Fe
2o
3join in deionized water and mix, the particle diameter of described Ag is 0.02 ~ 0.05 μm, described ZrO
2, and Fe
2o
3particle diameter be 0.1 ~ 0.5 μm, add dispersant sodium alkyl sulfate and be uniformly dispersed, be made into multi-functional interpolation mother liquor.
(2) sodium metasilicate deionized water is mixed with solution of sodium metasilicate through.
(3) adopt cellulose pulp to be raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow step obtain cellulose viscose solution, and then obtain spinning viscose through dissolving, deaeration and filtration step.
(4) solution of sodium metasilicate through that step (2) obtains being joined yellow in step (3) terminates in the viscose solution in rear course of dissolution, and the addition of sodium metasilicate is (by SiO
2meter) be 35% of the fine quality of first in cellulose sulfonate, the fine 10wt% of first is contained in cellulose yellow acid fat after adding sodium metasilicate, alkali 7.5wt%, the viscosity that viscosity 45s(falling ball method measures), multi-functional interpolation mother liquor is joined in spinning viscose by injection before spinning before spinning, Ag/SiO in described multi-functional interpolation mother liquor
2, ZrO
2, Fe
2o
3addition be respectively 2.5%, 4.5% and 0.2% of the fine quality of first in spinning viscose, wherein in multi-functional interpolation mother liquor, the addition of Ag is 0.25% of the fine quality of first in cellulose sulfonate, evenly obtains described multi-functional blended viscose solution with spinning viscose through static mixing.
(5) by the spinning in coagulating bath of described multi-functional blended viscose solution, draw forming, then after washing, desulfurization, the post processing that oils, described Multifunctional cellulose fiber is obtained, use sodium sulfite as desulfurizing agent during desulfurization, the concentration 12g/l of described sodium sulfite, temperature 85 DEG C.
Embodiment 7
A preparation method for Multifunctional cellulose fiber, comprises following steps:
(1) by ZrO
2, Ag/SiO
2, Fe
2o
3join in deionized water and mix, the particle diameter of described Ag is 0.02 ~ 0.1 μm, described ZrO
2, and Fe
2o
3particle diameter be 0.1 ~ 0.58 μm, add dispersant alkyl ethoxy sulfobetaines and be uniformly dispersed, be made into multi-functional interpolation mother liquor.
(2) sodium metasilicate deionized water is mixed with solution of sodium metasilicate through.
(3) adopt cellulose pulp to be raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow step obtain cellulose viscose solution, and then obtain spinning viscose through dissolving, deaeration and filtration step.
(4) solution of sodium metasilicate through that step (2) obtains is joined yellow in step (3) terminate after viscose solution in, the addition of sodium metasilicate is (by SiO
2meter) be 25% of the fine quality of first in cellulose sulfonate, the fine 15wt% of first is contained in cellulose yellow acid fat after adding sodium metasilicate, alkali 6wt%, the viscosity that viscosity 50s(falling ball method measures), multi-functional interpolation mother liquor is joined in spinning viscose by injection before spinning before spinning, Ag/SiO in described multi-functional interpolation mother liquor
2, ZrO
2, Fe
2o
3addition be respectively 4.5%, 5% and 0.06% of the fine quality of first in spinning viscose, wherein in multi-functional interpolation mother liquor, the addition of Ag is 1.0% of the fine quality of first in cellulose sulfonate, with spinning viscose through static or dynamically mix and obtain described multi-functional blended viscose solution.
(5) by the spinning in coagulating bath of described multi-functional blended viscose solution, draw forming, then after washing, desulfurization, the post processing that oils, described Multifunctional cellulose fiber is obtained, the temperature of described coagulating bath is 49 DEG C, containing sulfuric acid 120g/l, zinc sulfate 10g/l, sodium sulphate 290g/l in described coagulating bath; The total stretch ratio of described drawing-off is 30%; Use sodium sulfite as desulfurizing agent during desulfurization, the concentration 10g/l of described sodium sulfite, temperature 85 DEG C.
Embodiment 8
A preparation method for Multifunctional cellulose fiber, comprises following steps:
(1) by ZrO
2, Ag/SiO
2, Fe
2o
3join in deionized water by the weight ratio of 4:3:0.6 and mix, the particle diameter of described Ag is 0.02 ~ 0.5 μm, described ZrO
2, and Fe
2o
3particle diameter be 0.1 ~ 1 μm, add dispersant sodium alkyl benzene sulfonate and sodium alkyl sulfate is uniformly dispersed, be made into multi-functional interpolation mother liquor.
(2) sodium metasilicate deionized water is mixed with solution of sodium metasilicate through.
(3) adopt cellulose pulp to be raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow step obtain cellulose viscose solution, and then obtain spinning viscose through dissolving, deaeration and filtration step.
(4) joined by the solution of sodium metasilicate through that step (2) obtains in the viscose solution after dissolving in step (3), before deaeration, the addition of sodium metasilicate is (by SiO
2meter) be 40% of the fine quality of first in cellulose sulfonate, the fine 11.5wt% of first is contained in cellulose yellow acid fat after adding sodium metasilicate, alkali 8.6wt%, the viscosity that viscosity 55s(falling ball method measures), multi-functional interpolation mother liquor is joined in spinning viscose by injection before spinning before spinning, Ag/SiO in described multi-functional interpolation mother liquor
2, ZrO
2, Fe
2o
3addition be respectively 4%, 3% and 0.6% of the fine quality of first in spinning viscose, wherein in multi-functional interpolation mother liquor, the addition of Ag is 0.9% of the fine quality of first in cellulose sulfonate, with spinning viscose through static or dynamically mix and obtain described multi-functional blended viscose solution.
(5) by the spinning in coagulating bath of described multi-functional blended viscose solution, draw forming, then after washing, desulfurization, the post processing that oils, described Multifunctional cellulose fiber is obtained, the temperature of described coagulating bath is 55 DEG C, containing sulfuric acid 120g/l, zinc sulfate 15g/l, sodium sulphate 320g/l in described coagulating bath; The total stretch ratio of described drawing-off is 55%; Use sodium sulfite as desulfurizing agent during desulfurization, the concentration 12g/l of described sodium sulfite, temperature 90 DEG C.
Comparative example 1
Comparative example 1 is with the difference of embodiment 7: do not have step (1), and only add solution of sodium metasilicate through in step (4), do not add Ag/SiO
2, ZrO
2, Fe
2o
3multi-functional interpolation mother liquor, all the other are all identical.
The performance indications of viscose prepared by embodiment 4-8 and comparative example 1 see the following form.
Claims (6)
1. a preparation method for Multifunctional cellulose fiber, is characterized in that comprising following steps:
(1) multi-functional interpolation mother liquor is prepared: by ZrO
2, Ag/SiO
2, Fe
2o
3join in deionized water and mix, add dispersant evenly, be made into multi-functional interpolation mother liquor; Described dispersant is anion surfactant or amphoteric surfactant;
(2) solution of sodium metasilicate through is prepared: sodium metasilicate deionized water is mixed with solution of sodium metasilicate through;
(3) preparation of cellulose viscose glue: employing cellulose pulp is raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow step obtain cellulose viscose solution, and then obtain spinning viscose through dissolving, deaeration and filtration step;
(4) prepare multi-functional blended viscose solution: the solution of sodium metasilicate through that step (2) obtains is joined yellow in step (3) terminate after in the viscose solution filtered in arbitrary step, the addition of sodium metasilicate presses SiO
2count 15 ~ 50% of the fine quality of first in cellulose sulfonate, multi-functional interpolation mother liquor is joined in spinning viscose by injection before spinning before spinning, Ag/SiO in described multi-functional interpolation mother liquor
2, ZrO
2, Fe
2o
3addition be respectively 0.5 ~ 5%, 1.2 ~ 10% and 0.02 ~ 1% of the fine quality of first in spinning viscose, obtain described multi-functional blended viscose solution;
(5) co-blended spinning: by the spinning in coagulating bath of described multi-functional blended viscose solution, draw forming, then through comprising washing, desulfurization, the post-processing step that oils obtain described Multifunctional cellulose fiber.
2. the preparation method of a kind of Multifunctional cellulose fiber as claimed in claim 1, it is characterized in that: in described multi-functional interpolation mother liquor, the addition of Ag is 0.1 ~ 1% of the fine quality of first in cellulose sulfonate, the particle diameter of described Ag is 0.02 ~ 0.5 μm, described ZrO
2and Fe
2o
3particle diameter be 0.1 ~ 1 μm.
3. the preparation method of a kind of Multifunctional cellulose fiber as claimed in claim 1, is characterized in that: the temperature of described coagulating bath is 40 ~ 60 DEG C, containing sulfuric acid 90 ~ 150g/l, zinc sulfate 5 ~ 50g/l, sodium sulphate 270 ~ 350g/l in described coagulating bath.
4. the preparation method of a kind of Multifunctional cellulose fiber as claimed in claim 1, is characterized in that: the total stretch ratio of described drawing-off is 10 ~ 300%.
5. the preparation method of a kind of Multifunctional cellulose fiber as claimed in claim 1, is characterized in that: described dispersant is at least one in sodium alkyl benzene sulfonate, sodium alkyl sulfate or alkyl ethoxy sulfobetaines.
6. the preparation method of a kind of Multifunctional cellulose fiber as claimed in claim 1, is characterized in that: use sodium sulfite as desulfurizing agent during described desulfurization, the concentration 5 ~ 15g/l of described sodium sulfite, temperature 80 ~ 95 DEG C.
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