CN116288769A - Aluminosilicate flame-retardant regenerated cellulose fiber and preparation method thereof - Google Patents
Aluminosilicate flame-retardant regenerated cellulose fiber and preparation method thereof Download PDFInfo
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- 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 title claims abstract description 124
- 239000003063 flame retardant Substances 0.000 title claims abstract description 124
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 31
- 229910000323 aluminium silicate Inorganic materials 0.000 title claims abstract description 29
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000004627 regenerated cellulose Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000835 fiber Substances 0.000 claims abstract description 62
- 230000001112 coagulating effect Effects 0.000 claims abstract description 49
- 238000004132 cross linking Methods 0.000 claims abstract description 32
- 229920002678 cellulose Polymers 0.000 claims abstract description 24
- 239000001913 cellulose Substances 0.000 claims abstract description 24
- 239000011734 sodium Substances 0.000 claims abstract description 10
- 229920000297 Rayon Polymers 0.000 claims description 42
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 41
- 229910052710 silicon Inorganic materials 0.000 claims description 41
- 239000010703 silicon Substances 0.000 claims description 41
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000009987 spinning Methods 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 17
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 16
- 238000007670 refining Methods 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 239000002243 precursor Substances 0.000 claims description 13
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 claims description 12
- 238000000465 moulding Methods 0.000 claims description 12
- 239000012991 xanthate Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 8
- 230000015271 coagulation Effects 0.000 claims description 7
- 238000005345 coagulation Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 6
- 238000004061 bleaching Methods 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 6
- 230000005070 ripening Effects 0.000 claims description 6
- 238000004383 yellowing Methods 0.000 claims description 6
- 238000006477 desulfuration reaction Methods 0.000 claims description 4
- 230000023556 desulfurization Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims 1
- 238000009740 moulding (composite fabrication) Methods 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 8
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 abstract description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 abstract description 4
- 229960001763 zinc sulfate Drugs 0.000 abstract description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003111 delayed effect Effects 0.000 abstract description 2
- 229910052708 sodium Inorganic materials 0.000 abstract description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 abstract description 2
- 235000011152 sodium sulphate Nutrition 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 230000000149 penetrating effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 40
- 239000004115 Sodium Silicate Substances 0.000 description 8
- 229910052911 sodium silicate Inorganic materials 0.000 description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 8
- 229920000742 Cotton Polymers 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000004480 active ingredient Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 229920001131 Pulp (paper) Polymers 0.000 description 3
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910001388 sodium aluminate Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000003009 desulfurizing effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 239000012615 aggregate Substances 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides an aluminosilicate flame-retardant regenerated cellulose fiber and a preparation method thereof, wherein the cellulose content in the fiber is 60-80 wt%, and SiO is prepared by the following steps of 2 The content is 20 to 35 weight percent, al 2 O 3 The content is 0-5 wt%. According to the invention, the temperature of the coagulating bath is reduced, the contents of sulfuric acid and sodium sulfate in the coagulating bath are reduced, the zinc sulfate content is increased, the forming speed of fibers is delayed, and meanwhile, more cellulose zinc sulfonate with a cross-linking structure can be generated by the action of zinc sulfate and cellulose sodium sulfonate, so that the two-bath cross-linking forming is used as a bedding; the drafting in the coagulating bath is reduced, the breakage of incompletely formed tows is stopped, and the spinnability of the fibers is ensured. Al in two baths 3+ Crosslinking and curing reaction with silicic acid and polysilicic acid in gel state in the incompletely formed tow to generate aluminosilicate penetrating through cellulose macromoleculesThe net structure, the as-spun fiber tows which are not completely formed are solidified and formed through sulfuric acid in the two baths, so that the strength of the fibers can be improved to a certain extent.
Description
Technical Field
The invention belongs to the field of cellulose fibers, and particularly relates to an aluminosilicate flame-retardant regenerated cellulose fiber and a preparation method thereof.
Background
Regenerated cellulose fiber is the second largest fiber variety in chemical fibers, has the nature of cotton, the quality of silk, and is derived from the world but is superior to natural, is an important textile raw material, and is widely applied in the textile industry. However, the flammability of the cellulose fiber brings great hidden trouble to the life and property safety of people, limits the application field to a certain extent, and the flame retardant research of the cellulose fiber is always one of the key points of research and development of people. The prior flame-retardant fiber preparation technology is mainly summarized into three types of blended flame retardance, graft copolymerization flame retardance and after-finishing flame retardance. The existing market industrialized products mainly adopt a method of adding and blending, which can lead the fiber to obtain longer-lasting flame retardant performance, but the flame retardant viscose fiber produced by the blending technology has the problems of large addition amount of the flame retardant, loss of the flame retardant, reduced mechanical performance of the flame retardant fiber, reduced fiber taking performance and the like in the fiber production or use process. The national '863' project of Qingdao university and Shandong sea dragon, namely research on new flame-retardant and anti-melting fiber materials and textiles, realizes the industrialized production of inorganic silicon flame-retardant viscose fibers, is popularized and applied in the field of non-woven, but the problem of loss of flame retardant in dyeing and finishing and washing processes of fiber fabrics always affects the application of the fiber fabrics in the field of textile and clothing.
Patent CN200310117767.4 discloses SiO 2 Sodium silicate or potassium silicate as precursor is added into the viscose solution to produce the silicon dioxide/cellulose composite material; patent CN102605452a discloses a preparation method of flame-retardant silicate fiber for improving SiO 2 SiO in the process of coagulating bath forming by the blending solution of the precursor and the viscose 2 Is increased in SiO by the loss of coagulation bath composition 2 And (5) controlling the index. Patent CN1847476A discloses a process method of inorganic silicon flame-retardant viscose fiber, which aims to improve inorganic silicon flame-retardant viscoseThe flame-retardant finishing-resistant performance of the fiber is improved by adding crosslinking treatment in the refining process, the crosslinking treatment is carried out when the meta-aluminate is adopted to desulfurate the inorganic flame-retardant viscose fiber, and the silicic acid on the fiber is dissolved and Al is carried out under the high-temperature alkaline condition 3+ And the stable aluminosilicate is formed on the surface of the fiber by the reaction, so that the flame-retardant finishing-resistant performance of the fiber is improved. The refining crosslinking treatment improves the adhesion firmness of the flame retardant and the fiber and simultaneously causes a certain amount of flame retardant SiO 2 The problem of uneven cross-linking treatment exists between the upper cotton layer and the lower cotton layer of the refiner, and the treatment technology is not suitable for industrialized continuous production.
Wang Ke in the paper "development and development of high temperature resistant flame retardant silicon-aluminum-cellulose blended viscose fibers" it is proposed to add a certain amount of sodium aluminate to a mixed solution of sodium silicate and viscose in a pre-spinning injection manner, and at the same time, to add an aluminum sulfate component in a coagulation bath during the forming process, and at the same time, it is also mentioned that the addition of sodium aluminate affects the filtration and spinnability of the flame retardant viscose solution. The method can cause the reaction of sodium aluminate and sodium silicate in the viscose mixed solution, and has gel risk and Al in the coagulating bath 3+ Can react with silicic acid, aggregate and precipitate, and has no continuous production feasibility. The invention adjusts the spinning forming process based on the process of the patent CN102605452A, delays the forming speed of the flame-retardant tows in the coagulating bath, increases the two-bath crosslinking forming technology of the flame-retardant tows, and realizes the development and stable production of flame-retardant finishing-resistant aluminosilicate flame-retardant regenerated cellulose fibers.
Disclosure of Invention
In order to solve the problem of loss of flame retardant in inorganic silicon flame-retardant viscose fibers in the prior art, the invention provides an aluminosilicate flame-retardant regenerated cellulose fiber and a preparation method thereof, and the preparation method is characterized in that solidification molding conditions are adjusted, and a two-bath crosslinking molding technology is adopted to prepare finishing-resistant aluminosilicate flame-retardant regenerated cellulose fiber.
In order to solve the technical problems, one of the purposes of the invention is to provide an aluminosilicate flame-retardant regenerated cellulose fiber, wherein the cellulose content in the fiber is 60 to 80 weight percent, and SiO 2 The content is 20 to 35 weight percent, al 2 O 3 The content is 0-5 wt%.
The second object of the invention is to provide a preparation method of aluminosilicate flame-retardant regenerated cellulose fiber, which comprises the following steps:
s1, preparation of flame-retardant viscose spinning solution
Adopting cellulose pulp as a raw material, and preparing cellulose xanthate through steps of dipping, squeezing, crushing, ageing, yellowing and the like; cellulose xanthate is dissolved in 4-8% sodium hydroxide solution, then precursor dissolving solution of silicon flame retardant is added, and the flame-retardant viscose spinning solution is prepared through filtration, ripening and deaeration.
Preferably, the content of alpha cellulose in the flame-retardant viscose spinning solution is 6.2 to 7.8 weight percent, and the silicon flame retardant is the active ingredient SiO 2 The content is 30-50wt% relative to the alpha cellulose; the NaOH content in the flame-retardant viscose spinning solution is 6.0-8.2 wt%.
Preferably, the precursor of the silicon-based flame retardant is sodium silicate.
S2, coagulating bath treatment
And solidifying the flame-retardant viscose spinning solution in a coagulating bath to obtain the nascent fiber tows.
Preferably, the coagulation bath comprises H 2 SO 4 、ZnSO 4 、Na 2 SO 4 And a silicon-based flame retardant.
Preferably, the content of each component in the coagulating bath is as follows: h 2 SO 4 60-80 g/L ZnSO 4 50 to 60g/L of Na 2 SO 4 220-250 g/L, and the effective content of the silicon flame retardant SiO 2 0.1-1.2 g/L.
The temperature of the coagulating bath is controlled at 35-40 ℃, the time is 0.5-2.0S, and the drafting in the coagulating bath is controlled at 10-50%.
S3, two-bath crosslinking forming
The primary fiber tows which are discharged from the coagulating bath are drawn between discs to enter a two-bath for crosslinking and forming, and the two-bath time is 20-50S.
Preferably, the interdisk draft is controlled to be 30-60%.
Preferably, the two baths are H containing aluminum salts 2 SO 4 Solution of Al salt 2 SO 4 Or AlCl 3 Or Al 2 SO 4 With AlCl 3 Is a mixture of (a) and (b); the contents of each component in the two baths are as follows: h 2 SO 4 20 to 60g/L of Al 3+ The concentration is 0.5-5 g/L; the temperature of the two baths is controlled between 55 and 90 ℃.
S4, refining and drying
The fiber after the two-bath crosslinking molding is washed, cut off and enters a refining process, and the aluminosilicate flame-retardant regenerated cellulose fiber finished product is prepared through washing, desulfurization, bleaching, oiling, drying and packing.
By adopting the technical scheme, the invention has the following technical effects:
1. the aluminosilicate flame-retardant regenerated cellulose fiber prepared by the invention has excellent mechanical properties, the dry breaking strength is as high as 2.05-2.5 cN/dtex, and the spinnability is stronger.
2. According to the invention, the temperature of the coagulating bath is reduced, the contents of sulfuric acid and sodium sulfate in the coagulating bath are reduced, the zinc sulfate content is increased, the forming speed of fibers is delayed, and meanwhile, more cellulose zinc sulfonate with a cross-linking structure can be generated by the action of zinc sulfate and cellulose sodium sulfonate, so that the two-bath cross-linking forming is used as a bedding; the drafting in the coagulating bath is reduced, the breakage of incompletely formed tows is stopped, and the spinnability of the fibers is ensured. Al in two baths 3+ And the non-fully formed primary fiber tows are solidified and formed through sulfuric acid in two baths, so that the strength of the fibers can be improved to a certain extent.
3. According to the invention, the aluminosilicate flame-retardant regenerated cellulose fiber is prepared by adopting two-bath crosslinking and curing, so that the loss of the flame retardant in the fiber preparation process is reduced, the flame retardant is more stable and uniform in the fiber, the flame retardance and washing resistance of the fiber are ensured, the operation is simple, the cost is low, and the method is suitable for industrial production.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1
S1, preparation of flame-retardant viscose spinning solution
Adopting wood pulp as a raw material, and preparing cellulose xanthate through steps of dipping, squeezing, crushing, aging, yellowing and the like; cellulose xanthate is dissolved in a 6% sodium hydroxide solution, then precursor dissolution liquid of a silicon flame retardant is added, and the flame-retardant viscose spinning solution is prepared through filtration, ripening and defoaming.
The content of alpha cellulose in the flame-retardant viscose spinning solution is 6.2wt%, and the silicon flame retardant is the active ingredient SiO 2 The content is 30wt% relative to the alpha cellulose; the NaOH content in the flame-retardant viscose spinning solution is 6.0wt%.
The precursor of the silicon flame retardant is sodium silicate.
S2, coagulating bath treatment
And (3) the flame-retardant viscose spinning solution is metered by a metering pump and sprayed into a coagulating bath through a spinneret to be coagulated, so as to obtain a nascent fiber tow.
The coagulating bath comprises H 2 SO 4 、ZnSO 4 、Na 2 SO 4 And a silicon-based flame retardant.
The coagulating bath comprises the following components in percentage by weight: h 2 SO 4 65g/L ZnSO 4 60g/L, na 2 SO 4 230g/L, effective content of SiO of the silicon flame retardant 2 1.2g/L.
The temperature of the coagulating bath is controlled at 38 ℃, the time is 0.8S, and the drafting in the coagulating bath is controlled at 26%.
S3, two-bath crosslinking forming
The primary fiber tows which are discharged from the coagulating bath are drawn between discs to enter a two-bath for crosslinking and forming, and the two-bath time is 45S.
The interdisk draft was controlled at 30%.
The two baths contain Al 2 SO 4 H of (2) 2 SO 4 A solution; the contents of each component in the two baths are as follows: h 2 SO 4 56g/L of Al 3+ Concentration is 2.5g/L; the temperature of the two baths is controlled at 82 ℃.
S4, refining and drying
The fiber after the two-bath crosslinking molding is washed, cut off and enters a refining process, and an aluminosilicate flame-retardant regenerated cellulose fiber finished product is prepared through washing, desulfurization, bleaching, oiling, drying and packing; the fiber obtained had a fineness of 3.33dtex, a dry break strength of 2.5cN/dtex and a burning residue of 31.9% (wherein SiO 2 28.6％、Al 2 O 3 3.3 percent) and the loss rate of the silicon flame retardant after 50 times of water washing is 2.06 percent.
Example 2
S1, preparation of flame-retardant viscose spinning solution
Adopting cotton pulp as a raw material, and preparing cellulose xanthate through steps of dipping, squeezing, crushing, ageing, yellowing and the like; cellulose xanthate is dissolved in 4% sodium hydroxide solution, then precursor dissolving liquid of a silicon flame retardant is added, and the flame-retardant viscose spinning solution is prepared through filtration, ripening and defoaming.
The content of alpha cellulose in the flame-retardant viscose spinning solution is 7.8wt%, and the silicon flame retardant is the active ingredient SiO 2 The content of the alpha cellulose is 42.5wt percent relative to the alpha cellulose; the NaOH content in the flame-retardant viscose spinning solution is 8.2wt%.
The precursor of the silicon flame retardant is sodium silicate.
S2, coagulating bath treatment
And (3) the flame-retardant viscose spinning solution is metered by a metering pump and sprayed into a coagulating bath through a spinneret to be coagulated, so as to obtain a nascent fiber tow.
The coagulating bath comprises H 2 SO 4 、ZnSO 4 、Na 2 SO 4 And a silicon-based flame retardant.
The coagulating bath comprises the following components in percentage by weight: h 2 SO 4 75g/L ZnSO 4 50g/L, na 2 SO 4 Effective content of SiO of the silicon flame retardant is 220g/L 2 0.1g/L.
The temperature of the coagulating bath is controlled at 36 ℃, the time is 0.5S, and the drafting in the coagulating bath is controlled at 35%.
S3, two-bath crosslinking forming
The primary fiber tows which are discharged from the coagulating bath are drawn between discs to enter a two-bath for crosslinking and forming, and the two-bath time is 35S.
The interdisk draft was controlled at 45%.
The two baths contain AlCl 3 H of (2) 2 SO 4 A solution; the contents of each component in the two baths are as follows: h 2 SO 4 45g/L of Al 3+ The concentration is 5g/L; the temperature of the two baths is controlled at 70 ℃.
S4, refining and drying
The fiber after the two-bath crosslinking molding is washed, cut off and enters a refining process, and an aluminosilicate flame-retardant regenerated cellulose fiber finished product is prepared through washing, desulfurization, bleaching, oiling, drying and packing; the fiber obtained had a fineness of 4.89dtex, a dry break strength of 2.34cN/dtex and a burning residue of 33.6% (wherein SiO 2 29.4％、Al 2 O 3 4.2 percent) and the loss rate of the silicon flame retardant after 50 times of water washing is 2.73 percent.
Example 3
S1, preparation of flame-retardant viscose spinning solution
Adopting cotton pulp and wood pulp with mass ratio of 1:1 as raw materials, and preparing cellulose xanthate through steps of dipping, squeezing, crushing, ageing, yellowing and the like; cellulose xanthate is dissolved in 8% sodium hydroxide solution, then precursor dissolving liquid of a silicon flame retardant is added, and the flame-retardant viscose spinning solution is prepared through filtration, ripening and defoaming.
The content of alpha cellulose in the flame-retardant viscose spinning solution is 7.2wt%, and the silicon flame retardant is an active ingredient SiO 2 The content is 50wt% relative to the alpha cellulose; the NaOH content in the flame-retardant viscose spinning solution is 7.8wt%.
The precursor of the silicon flame retardant is sodium silicate.
S2, coagulating bath treatment
And (3) the flame-retardant viscose spinning solution is metered by a metering pump and sprayed into a coagulating bath through a spinneret to be coagulated, so as to obtain a nascent fiber tow.
The coagulating bath comprises H 2 SO 4 、ZnSO 4 、Na 2 SO 4 And a silicon-based flame retardant.
The coagulating bath comprises the following components in percentage by weight: h 2 SO 4 80g/L ZnSO 4 58g/L, na 2 SO 4 Effective content of SiO of the silicon flame retardant is 250g/L 2 0.86g/L.
The temperature of the coagulating bath is controlled at 35 ℃, the time is 2.0S, and the drafting in the coagulating bath is controlled at 10%.
S3, two-bath crosslinking forming
The primary fiber tows which are discharged from the coagulating bath are drawn between discs to enter a two-bath for crosslinking and forming, and the two-bath time is 50S.
The interdisk draft was controlled at 60%.
The two baths contain AlCl 3 H of (2) 2 SO 4 A solution; the contents of each component in the two baths are as follows: h 2 SO 4 60g/L of Al 3+ Concentration is 0.5g/L; the temperature of the two baths is controlled at 55 ℃.
S4, refining and drying
The fiber after two-bath crosslinking molding enters a refining process after washing and cutting, and the finished product of aluminosilicate flame-retardant regenerated cellulose fiber is prepared by washing, desulfurizing, bleaching, oiling, drying and packing, the fineness of the prepared fiber is 4.78dtex, the dry breaking strength is 2.05cN/dtex, and the burning residue is 34.8 percent (wherein SiO 2 33.8％、Al 2 O 3 1.0 percent) and the loss rate of the silicon flame retardant after 50 times of water washing is 2.27 percent.
Example 4
S1, preparation of flame-retardant viscose spinning solution
Adopting cotton pulp and wood pulp with mass ratio of 1:3 as raw materials, and preparing the cellulose xanthate through the steps of dipping, squeezing, crushing, ageing, yellowing and the like; cellulose xanthate is dissolved in a 6% sodium hydroxide solution, then precursor dissolution liquid of a silicon flame retardant is added, and the flame-retardant viscose spinning solution is prepared through filtration, ripening and defoaming.
The content of alpha cellulose in the flame-retardant viscose spinning solution is 7.4wt%, and the silicon flame retardant is an active ingredient SiO 2 The content is 46wt% relative to the alpha cellulose; the NaOH content in the flame-retardant viscose spinning solution is 7.2wt%.
The precursor of the silicon flame retardant is sodium silicate.
S2, coagulating bath treatment
And (3) the flame-retardant viscose spinning solution is metered by a metering pump and sprayed into a coagulating bath through a spinneret to be coagulated, so as to obtain a nascent fiber tow.
The coagulating bath comprises H 2 SO 4 、ZnSO 4 、Na 2 SO 4 And a silicon-based flame retardant.
The coagulating bath comprises the following components in percentage by weight: h 2 SO 4 60g/L ZnSO 4 52g/L, na 2 SO 4 Effective content of SiO of silicon flame retardant of 240g/L 2 0.5g/L.
The temperature of the coagulating bath is controlled at 40 ℃, the time is 1.2S, and the drafting in the coagulating bath is controlled at 50%.
S3, two-bath crosslinking forming
The primary fiber tows which are discharged from the coagulating bath are drawn between discs to enter a two-bath for crosslinking and forming, and the two-bath time is 25S.
The interdisk draft was controlled at 35%.
The two baths contain Al 2 SO 4 H of (2) 2 SO 4 A solution; the contents of each component in the two baths are as follows: h 2 SO 4 20g/L of Al 3+ Concentration is 3g/L; the two-bath temperature was controlled at 65 ℃.
S4, refining and drying
The fiber after two-bath crosslinking molding enters a refining process after washing and cutting, and the finished product of aluminosilicate flame-retardant regenerated cellulose fiber is prepared by washing, desulfurizing, bleaching, oiling, drying and packing, the fineness of the prepared fiber is 5.56dtex, the dry breaking strength is 2.18cN/dtex, and the burning residue is 33.4 percent (wherein SiO 2 30.6％、Al 2 O 3 2.8 percent) and the loss rate of the silicon flame retardant after 50 times of water washing is 2.3 percent.
Comparative example 1
Representative example 1 was chosen to remove Al from the two baths 2 SO 4 The remainder was the same as in example 1, except that as comparative example 1, a fiber fineness of 3.5dtex, dry break strength was produced1.98cN/dtex, 27.4% of burning residue and 62.7% of loss rate of the silicon flame retardant after washing 50 times, which shows that the two-bath crosslinking molding greatly improves the washing resistance of the flame retardant fiber.
Comparative example 2
Flame-retardant fibers were prepared according to the process of example 1 in patent CN102605452a, as comparative example 2, the loss rate of the silicon-based flame retardant after 50 test water washes was 74%, and the loss rate was higher than that of comparative example 1, because the coagulation bath of the present invention was retarded to be molded and the two baths were completely molded, and the silicon-based flame retardant was distributed more uniformly in the fibers; the process of comparative example 2 was carried out by adding the flame retardant directly into the coagulation bath and molding the resultant material once, and the uniformity of the silicon flame retardant in the fiber was poor and the washing resistance was also poor.
The proportions are mass proportions, and the percentages are mass percentages, unless otherwise specified; the raw materials are all commercially available.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An aluminosilicate flame-retardant regenerated cellulose fiber is characterized in that the cellulose content in the fiber is 60-80 wt%, and SiO is contained in the fiber 2 The content is 20 to 35 weight percent, al 2 O 3 The content is 0-5 wt%.
2. The preparation method of the aluminosilicate flame-retardant regenerated cellulose fiber is characterized by comprising the steps of flame-retardant viscose spinning solution preparation, coagulating bath treatment, two-bath cross-linking forming, refining and drying.
3. The method for preparing the aluminosilicate flame-retardant regenerated cellulose fiber according to claim 2, wherein the flame-retardant viscose spinning solution is prepared by adopting cellulose pulp as a raw material, and preparing cellulose xanthate through steps of dipping, squeezing, crushing, ageing, yellowing and the like; cellulose xanthate is dissolved in 4-8% sodium hydroxide solution, then precursor dissolving solution of silicon flame retardant is added, and the flame-retardant viscose spinning solution is prepared through filtration, ripening and deaeration.
4. The method for preparing aluminosilicate flame-retardant regenerated cellulose fiber according to claim 3, wherein the content of alpha cellulose in the flame-retardant viscose spinning solution is 6.2-7.8 wt%, and the silicon flame retardant is effective ingredient SiO 2 The content is 30-50wt% relative to the alpha cellulose; the NaOH content in the flame-retardant viscose spinning solution is 6.0-8.2 wt%.
5. The method for preparing the aluminosilicate flame-retardant regenerated cellulose fiber according to claim 2, wherein the coagulating bath treatment is that the flame-retardant viscose spinning solution is coagulated in the coagulating bath to obtain a nascent fiber tow;
the coagulating bath comprises H 2 SO 4 、ZnSO 4 、Na 2 SO 4 And a silicon-based flame retardant.
6. The method for preparing the aluminosilicate flame retardant regenerated cellulose fiber according to claim 5, wherein the content of each component in the coagulation bath is: h 2 SO 4 60-80 g/L ZnSO 4 50 to 60g/L of Na 2 SO 4 220-250 g/L, and the effective content of the silicon flame retardant SiO 2 0.1-1.2 g/L;
the temperature of the coagulating bath is controlled at 35-40 ℃, the time is 0.5-2.0S, and the drafting in the coagulating bath is controlled at 10-50%.
7. The method for preparing the aluminosilicate flame retardant regenerated cellulose fiber according to claim 2, wherein the two-bath cross-linking molding is carried out, wherein the primary fiber tows which are subjected to coagulation bath enter the two-bath cross-linking molding through interdisk drafting, and the two-bath time is 20-50S;
the interdisk draft is controlled to be 30-60%.
8. The method for producing an aluminosilicate flame retardant regenerated cellulose fiber according to claim 7, wherein said two baths are H containing aluminum salt 2 SO 4 Solution of Al salt 2 SO 4 Or AlCl 3 Or Al 2 SO 4 With AlCl 3 Is a mixture of (a) and (b).
9. The method for preparing the aluminosilicate flame retardant regenerated cellulose fiber according to claim 7, wherein the contents of each component in the two baths are: h 2 SO 4 20 to 60g/L of Al 3+ The concentration is 0.5-5 g/L; the temperature of the two baths is controlled between 55 and 90 ℃.
10. The method for preparing the aluminosilicate flame-retardant regenerated cellulose fiber according to claim 2, wherein the refining and drying steps are that the fiber after two-bath crosslinking molding is washed and cut into refining procedures, and the aluminosilicate flame-retardant regenerated cellulose fiber finished product is prepared through washing, desulfurization, bleaching, oiling, drying and packing.
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