CN101649495B - Method for preparing flame resistance anti-thawing fibre spinning dope through solvent method - Google Patents
Method for preparing flame resistance anti-thawing fibre spinning dope through solvent method Download PDFInfo
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- CN101649495B CN101649495B CN2009100151443A CN200910015144A CN101649495B CN 101649495 B CN101649495 B CN 101649495B CN 2009100151443 A CN2009100151443 A CN 2009100151443A CN 200910015144 A CN200910015144 A CN 200910015144A CN 101649495 B CN101649495 B CN 101649495B
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- thawing
- flame resistance
- spinning dope
- resistance anti
- fibre spinning
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- 239000000835 fiber Substances 0.000 title claims abstract description 39
- 238000009987 spinning Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002904 solvent Substances 0.000 title claims abstract description 13
- 238000010257 thawing Methods 0.000 title claims abstract description 12
- 239000002608 ionic liquid Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000005496 tempering Methods 0.000 claims abstract description 3
- 229920002678 cellulose Polymers 0.000 claims description 15
- 239000001913 cellulose Substances 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000013016 damping Methods 0.000 claims description 10
- 239000006166 lysate Substances 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 5
- 150000001768 cations Chemical class 0.000 claims description 5
- 150000002460 imidazoles Chemical class 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 239000004111 Potassium silicate Substances 0.000 claims description 2
- 230000006837 decompression Effects 0.000 claims description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 7
- 239000004627 regenerated cellulose Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003063 flame retardant Substances 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 11
- 235000017491 Bambusa tulda Nutrition 0.000 description 11
- 241001330002 Bambuseae Species 0.000 description 11
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 11
- 229920000297 Rayon Polymers 0.000 description 11
- 239000011425 bamboo Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000003292 glue Substances 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$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229920003043 Cellulose fiber Polymers 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- GAUFKBQSTGCCOC-UHFFFAOYSA-N 2-[(5,5-dimethyl-2-sulfanylidene-1,3,2$l^{5}-dioxaphosphinan-2-yl)oxy]-5,5-dimethyl-2-sulfanylidene-1,3,2$l^{5}-dioxaphosphinane Chemical compound O1CC(C)(C)COP1(=S)OP1(=S)OCC(C)(C)CO1 GAUFKBQSTGCCOC-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000002467 phosphate group Chemical class [H]OP(=O)(O[H])O[*] 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Abstract
The invention discloses a method for preparing flame resistance anti-thawing fibre spinning dope through solvent method which is suitable for industrialized production. The method comprises the following steps: grinding fibre with the degree of polymerization of 300-1000, humidifying, then mixing the obtained material with ionic liquid water solution in a weight ratio of 10:90-20:80 evenly, adding solving liquid with silicate to dissolve and mix, and then defoaming and filtrating to obtain flame resistance anti-thawing fibre spinning dope. When mixing cellulose powder with ionic liquid water solution, the materials are firstly sent to a tempering tank with an agitator for preliminary mixing and then to a double-screw extruder to mix at 70-100 DEG C for 10-60min. The technical solution of the invention is adopted so as to ensure that the production process of the flame resistance anti-thawing fibre spinning dope is easier and more environmentally friendly, improve the wet strength of regenerated cellulose material and reduce the energy consumption, thus being applicable to industrialized production.
Description
Technical field
The present invention relates to the ruling field, relate in particular to a kind of preparation method of fiber spinning dope.
Background technology
A large amount of NaOH, H in traditional viscose generative process
2SO
4And CS
2, emit H
2Toxic gas and zinc-containing waters such as S are made pollution to empty G&W, and ecological environment is destroyed.China is viscose big producing country in the world, and viscose accounts for very big ratio in the world.In recent years, because environmental protection is attached great importance in countries in the world, the production of viscose mainly concentrates on some developing countries at present.Many developed countries strengthen the research to the processing of pollution problem in the adhering process on the one hand, have proposed to reduce use CS
2Technology with solve to produce in three wastes problem, the also new technology of good cellulose fibre promptly adopts the solvent produce cellulose fibers on the other hand.
The solvent spun fibre technology do not need to alkalize, experienced, sulfonation, maturation and complicated postprocessing working procedures; The solvent spun fibre production technology is compared with traditional cellulose viscose manufacturing technique and is had an enormous advantage: adopt closed production basically; Solvent almost completely reclaims; Do not produce the three wastes, therefore can not damage environment; Cellulose viscose manufacturing technique is complicated on the other hand, and energy consumption is big, and it is simple to dissolve spinning process, solvent method, and its preparation process has only dissolving, spinning and solvent recovery, less energy consumption.Fibre property also is superior to viscose in addition, so the title of " green fiber of 21 century " is arranged.
Meanwhile, in vehicle, public building, family and office, fire safety problem more causes people's attention, and in order to reduce the harm of fabric fire, various countries have formulated the flame-retardant standard and use rules of various textiless.Limit non-flame-retardant textile with fabric types and field of employment, therefore, fire resistance fibre and fabric have obtained very fast development.
In recent years, several fire retardant antiflux fibers have preferably appearred on the overseas market.Like the permanent fire retardant antiflux fiber (PFR Rayon) of the U.S., the permanent fire retardant antiflux fiber of company of Avis section; The HFG fiber (additive is a chlorinated phosphate) of Japan Diawabo company; Clock spins the BeLL FLame fiber of company; The Lenzing fire retardant antiflux fiber of Austria Lenzing company; SandofLam 5060 (ExoLit 5060) fire retardant and the fiber of Switzerland former Sandoz company (existing CLariant), the VisiL viscose glue/polysilicate composite fibre of companies such as Finland Kemira etc.
A domestic climax that the development of fire retardant antiflux fiber before and after nineteen ninety, once occurred; There are many enterprises, scientific research institutions and colleges and universities to participate in; What adopt all is SandofLame5060 based flame retardants; But the quality of the fire retardant of domestic production does not reach spinning requirement because the fire retardant import price is too high, does not finally carry out suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of technology is simple, less energy consumption, be fit to the method for the method for preparing flame resistance anti-thawing fibre spinning dope through solvent that industrialization produces.
For solving the problems of the technologies described above; Technical scheme of the present invention is: the method for method for preparing flame resistance anti-thawing fibre spinning dope through solvent is after the degree of polymerization is 300～1000 pulverizing and damping; Mix with the weight ratio of the ion liquid aqueous solution with 10: 90～20: 80; Add the lysate that contains silicate and dissolve mixing, obtain flame resistance anti-thawing fibre spinning dope through deaeration and filtration afterwards.
After the said damping with cellulose pulp powder weight moisture content 2%～5%;
Said ionic liquid anion is Cl
-And Br
-One or both, CATION is the substituting group imidazoles; The said ion liquid aqueous solution with powder mixes before through the decompression inspissation to weight moisture capacity≤10%;
Said silicate is SiO
2Its modulus of predecessor (SiO
2: Na
2O) be 1～3.5 sodium metasilicate, potassium silicate or the mixture of the two, addition is 1～50%, preferred 10～20% of a relative a-cellulose quality.
After in the tempering tank of belt stirrer, just mixing earlier when cellulose powder and ionic liquid aqueous solution mix, feed double screw extruder again, and stir 10～60min down at 70～100 ℃.
Silicate is as SiO
2Predecessor join lysate after, through stirring, fully dissolving generates nano level SiO
2, the SiO of this nanometerization
2, not only have good flame retardancy, and in filtration step, be not easy to cause the obstruction of filter screen, have good strainability, thereby guaranteed carrying out smoothly of production; Simultaneously, in the spinning step, the SiO of nanometerization
2Can be distributed in equably in the regenerated cellulose matrix, can reduce SiO on the one hand
2Addition, reduce influence to cellulose physics mechanical performance, on the other hand, the SiO of the nanometerization that high flame retardant is active
2Can solve the contradiction between anti-flammability and the Material Physics mechanical performance; Nanometer SiO2 particle can be induced the cellulosic molecule crystallization as the heterogeneous nucleation agent simultaneously, and form more microstructure, and improve cellulosic degree of crystallinity, thus the mechanical property of raising regenerated cellulose/SiO2 nano composite material.Higher degree of crystallinity and uniform microstructure also can reduce the hygrometric state swollen effect of regenerated cellulose; Guarantee cellulosic molecularly oriented under the hygrometric state; And can prevent that cellulose from too much rupturing because of moisture absorption makes hydrogen bond, thereby improve the wet strength of material of regenerated cellulose.
Owing to adopted technique scheme, make and produce more simple, the environmental protection of flame resistance anti-thawing fibre spinning dope technology, reduce energy consumption and be fit to industrialization production, improved the wet strength of material of regenerated cellulose.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1:
With the degree of polymerization is that 300～1000 bamboo fibre pulp is ground into bamboo cellulose end, damping, and moisture content reaches 2%, is Cl with anion
-, CATION is the ion liquid aqueous solution inspissation under reduced pressure of substituting group imidazoles, makes its moisture content reach 10%, and the end of the bamboo cellulose after the damping and ionic liquid aqueous solution with weight ratio mixing in 10: 90, are made into the 60L lysate; Afterwards with 20kgSiO
2Content is 21% nine water sodium metasilicate (Na
2SiO
39H
2O); Join in the 60L lysate, stir 60min down at 70 ℃ and form faint yellow pastel, making total stereoplasm amount content is 9.55%; The viscose glue of NaOH mass content 7.24% makes 1.5D anti-flame fusion-resisting bamboo fibre spinning solution through deaeration, dehydration, filtration again.
Afterwards the above-mentioned spinning solution that makes is carried out spinning and can make 1.5D anti-flame fusion-resisting bamboo fibre.
Fiber index: do fracture strength: 2.13cN/dtex; Wet breaking strength: 1.12cN/dtex; Dried elongation at break: 20.4%; Line density deviation ratio :-1.2%; Whiteness: 79%; Oil content: 0.18%; Regain: 12.1%; Limited oxygen index (LOI) 27.5.
Embodiment 2:
With the degree of polymerization is that 300～1000 bamboo fibre pulp is ground into bamboo cellulose end, damping; Moisture content reaches 2%; With anion is that Br-, CATION are the ion liquid aqueous solution inspissation under reduced pressure of substituting group imidazoles; Make its moisture content reach 8%, end of the bamboo cellulose after the damping and ionic liquid aqueous solution are mixed with weight ratio at 20: 90, be made into the 80L lysate; Afterwards with 10Kg SiO
2Content is 49% sodium metasilicate (Na
2SiO
3); Join in the 80L lysate, stir 35min down at 85 ℃ and form faint yellow pastel, making total stereoplasm amount content is 9.35%; The viscose glue of NaOH mass content 6.26% makes 3.0D anti-flame fusion-resisting bamboo fibre spinning solution through deaeration, dehydration, filtration again.
Afterwards the above-mentioned spinning solution that makes is carried out spinning and can make 3.0D anti-flame fusion-resisting bamboo fibre.
Fiber index: do fracture strength: 2.03cN/dtex; Wet breaking strength: 1.01cN/dtex; Dried elongation at break: 21.0%; Line density deviation ratio :-2.8%; Whiteness: 78%; Oil content: 0.19%; Regain: 11.4%; Limited oxygen index (LOI) 28.
Embodiment 3:
With the degree of polymerization is that 300～1000 fiber pulp is ground into bamboo cellulose end, damping; Moisture content reaches 2%; With anion is that Cl-and Br-, CATION are the ion liquid aqueous solution inspissation under reduced pressure of substituting group imidazoles; Make its moisture content reach 9%, end of the cellulose after the damping and ionic liquid aqueous solution are mixed with weight ratio at 20: 80, be made into the 70L lysate; Afterwards with 10KgSiO
2Content is 49% sodium metasilicate (Na
2SiO
3), join in the 70L lysate, stir 10min down at 100 ℃ and form faint yellow pastel, making total stereoplasm amount content is 9.45%, the viscose glue of NaOH mass content 6.76% makes the fire retardant antiflux fiber spinning solution through deaeration, dehydration, filtration again.
Afterwards the above-mentioned spinning solution that makes is carried out spinning and can make fire retardant antiflux fiber.
Fiber index: do fracture strength: 2.10cN/dtex; Wet breaking strength: 1.05cN/dtex; Dried elongation at break: 21.3%; Line density deviation ratio :-2.4%; Whiteness: 79%; Oil content: 0.17%; Regain: 11.8%; Limited oxygen index (LOI) 28.5.
Claims (2)
1. the method for method for preparing flame resistance anti-thawing fibre spinning dope through solvent is characterized in that, said method is:
After in the tempering tank of belt stirrer, just mixing earlier when cellulose powder and ionic liquid aqueous solution mix, feed double screw extruder again, and stir 10～60min down at 70～100 ℃;
Then with the degree of polymerization be 300～1000 pulp pulverize and damping after; Mix with the weight ratio of the ion liquid aqueous solution with 10: 90～20: 80; Add the lysate that contains silicate and dissolve mixing, obtain flame resistance anti-thawing fibre spinning dope through deaeration and filtration afterwards;
After the said damping with cellulose pulp powder weight moisture content 2%～5%;
Said silicate is sodium metasilicate or the potassium silicate or the mixture of the two of modulus 1～3.5, and addition is 1～50% of a relative a-cellulose quality;
Said ionic liquid anion is one or both of Cl-and Br-, and CATION is the substituting group imidazoles;
The said ion liquid aqueous solution with powder mixes before through the decompression inspissation to weight moisture capacity≤10%.
2. the method for method for preparing flame resistance anti-thawing fibre spinning dope through solvent as claimed in claim 1, it is characterized in that: the addition of said silicate is 10～20% of an a-cellulose quality.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100151443A CN101649495B (en) | 2009-05-12 | 2009-05-12 | Method for preparing flame resistance anti-thawing fibre spinning dope through solvent method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100151443A CN101649495B (en) | 2009-05-12 | 2009-05-12 | Method for preparing flame resistance anti-thawing fibre spinning dope through solvent method |
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| Publication Number | Publication Date |
|---|---|
| CN101649495A CN101649495A (en) | 2010-02-17 |
| CN101649495B true CN101649495B (en) | 2012-06-06 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147145A (en) * | 2013-03-20 | 2013-06-12 | 天津工业大学 | Method for preparing modified cellulose fire-retardant fiber through reaction extrusion |
| CN103173932A (en) * | 2013-03-20 | 2013-06-26 | 天津工业大学 | Preparation method of antiflaming cellulose non-woven cloth |
| CN103334173B (en) * | 2013-07-11 | 2015-04-22 | 宜宾丝丽雅股份有限公司 | Antiflaming viscose fiber and preparation method thereof |
| CN103981592B (en) * | 2014-05-28 | 2022-10-25 | 天津工业大学 | Flame-retardant cellulose fiber and preparation method thereof |
| CN105297164B (en) * | 2015-10-20 | 2017-07-28 | 恒天海龙（潍坊）新材料有限责任公司 | High-strength coloring organic fire-resisting regenerated celulose fibre and preparation method thereof |
| CN109208103B (en) * | 2018-08-31 | 2020-12-08 | 龙丝（上海）新材料科技有限公司 | Preparation method of flame-retardant cellulose fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472374A (en) * | 2003-06-26 | 2004-02-04 | 东华大学 | Manufacturing method for bamboo cellulose fibre by solvent method |
| CN1796444A (en) * | 2004-12-28 | 2006-07-05 | 中国科学院化学研究所 | Method for preparing functional material of regenerated cellulose |
| CN1977072A (en) * | 2004-06-26 | 2007-06-06 | 纺织和塑料研究协会图林根研究院 | Method and device for the production of molded cellulose bodies |
| CN101007853A (en) * | 2001-10-03 | 2007-08-01 | 阿拉巴马大学 | Dissolution and processing of cellulose using ionic liquids |
| CN101177792A (en) * | 2007-11-21 | 2008-05-14 | 山东海龙股份有限公司 | Method for preparing cellulose spin dope |
-
2009
- 2009-05-12 CN CN2009100151443A patent/CN101649495B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101007853A (en) * | 2001-10-03 | 2007-08-01 | 阿拉巴马大学 | Dissolution and processing of cellulose using ionic liquids |
| CN1472374A (en) * | 2003-06-26 | 2004-02-04 | 东华大学 | Manufacturing method for bamboo cellulose fibre by solvent method |
| CN1977072A (en) * | 2004-06-26 | 2007-06-06 | 纺织和塑料研究协会图林根研究院 | Method and device for the production of molded cellulose bodies |
| CN1796444A (en) * | 2004-12-28 | 2006-07-05 | 中国科学院化学研究所 | Method for preparing functional material of regenerated cellulose |
| CN101177792A (en) * | 2007-11-21 | 2008-05-14 | 山东海龙股份有限公司 | Method for preparing cellulose spin dope |
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| CN101649495A (en) | 2010-02-17 |
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