CN102352539A - Manufacturing method of silicon-nitrogen containing environmental protection and flame retardant viscose staple fiber - Google Patents
Manufacturing method of silicon-nitrogen containing environmental protection and flame retardant viscose staple fiber Download PDFInfo
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- CN102352539A CN102352539A CN2011102119632A CN201110211963A CN102352539A CN 102352539 A CN102352539 A CN 102352539A CN 2011102119632 A CN2011102119632 A CN 2011102119632A CN 201110211963 A CN201110211963 A CN 201110211963A CN 102352539 A CN102352539 A CN 102352539A
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- retardant
- viscose
- silicon
- fire retardant
- glue
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- 229920000297 Rayon Polymers 0.000 title claims abstract description 78
- 239000003063 flame retardant Substances 0.000 title claims abstract description 44
- 239000000835 fiber Substances 0.000 title claims abstract description 39
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 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 16
- 230000007613 environmental effect Effects 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 238000009987 spinning Methods 0.000 claims abstract description 25
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 13
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000008234 soft water Substances 0.000 claims abstract description 7
- 238000002166 wet spinning Methods 0.000 claims abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003292 glue Substances 0.000 claims description 57
- 238000002485 combustion reaction Methods 0.000 claims description 17
- 239000003112 inhibitor Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 15
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000012757 flame retardant agent Substances 0.000 claims description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 229920006335 epoxy glue Polymers 0.000 claims description 9
- 238000006477 desulfuration reaction Methods 0.000 claims description 8
- 230000023556 desulfurization Effects 0.000 claims description 8
- 238000012805 post-processing Methods 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 7
- 238000013459 approach Methods 0.000 claims description 6
- 238000004061 bleaching Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 6
- 235000011152 sodium sulphate Nutrition 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 6
- 229960001763 zinc sulfate Drugs 0.000 claims description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 6
- 230000035800 maturation Effects 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 3
- 206010033546 Pallor Diseases 0.000 claims description 2
- 238000009897 hydrogen peroxide bleaching Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000007493 shaping process Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 239000004753 textile Substances 0.000 abstract description 8
- 238000005520 cutting process Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract 2
- 238000000465 moulding Methods 0.000 abstract 1
- 230000000979 retarding effect Effects 0.000 abstract 1
- 230000005070 ripening Effects 0.000 abstract 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 abstract 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 40
- 230000000694 effects Effects 0.000 description 6
- 230000009970 fire resistant effect Effects 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000012744 reinforcing agent Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000003197 gene knockdown Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Abstract
The invention discloses a manufacturing method of a silicon-nitrogen containing environmental protection and flame retardant viscose staple fiber. The method comprises the steps of: adding a fire retardant into a dissolver for mixing with viscose, then subjecting the mixture to ripening, spinning pretreatment, wet spinning, drafting, cutting, tomentum moulding, and post-treatment; preparing the fire retardant with a 5%-30% NaOH solution, a viscose auxiliary agent, a silicon-nitrogen fire retardant and sodium hexametaphosphate in a ratio of (1-10): (0.05-0.35): (3-18): (0.1-1) by weight; during spinning pretreatment, injecting a spinnability improving agent that is of 1.5%-3% of the weight of alpha cellulose in the viscosity solution before spinning; conducting curing with a fixation bath of soft water and a curing fire retardant that are in a ratio of (10%-80%): (90%-20%). Specifically, the viscose auxiliary agent is V-32, the silicon-nitrogen fire retardant is WS-801, the spinnability improving agent is WS-803, and the curing fire retardant is WS-802. The method of the invention can fully and uniformly mix the fire retardants and viscosity, improve the spinnability of wet spinning, avoid fire retardant loss, and the obtained fiber has good flame retarding effects and high strength, thus being able to serve as the raw material of textiles.
Description
Technical field
The present invention relates to a kind of silicon-nitrogen is environmental protection flame retardant viscose staple fibre manufacturing approach.
Background technology
Because viscose fiber fabric has good hygroscopicity, gas permeability, dyeability; Soft comfortable, and be can natural degradation feature of environmental protection cellulose fibre, thereby each enterprise one after another viscose glue as carrier; Add various fire retardant, the viscose modification is become Fire resistant viscose fiber.
Silicon is arranged is two kinds of Fire resistant viscose fiber, phosphorous flame-retardant viscoses to Chang Gui Fire resistant viscose fiber in the market.
Though silicon is the Fire resistant viscose fiber environmental protection, its spinnability is poor, and fiber strength is low, can not satisfy spinning and dress ornament requirement, can only use as nonwoven fabric and filler.
The phosphorous flame-retardant viscose can be used as the weaving raw material; But when burning, can emit high toxicity gas; And emit big smog during the phosphorus burning; Increased the seriousness that makes people chamber breath; Discarded object is also relatively more serious to the pollution of water quality soil; Therefore belong to not Recycled Fibers, so industry is badly in need of a kind of good flame retardation effect Fire resistant viscose fiber raw material of environmental protection again.
Summary of the invention
The object of the present invention is to provide a kind of silicon-nitrogen is environmental protection flame retardant viscose staple fibre manufacturing approach; Utilize the common viscose fiber production line; Adopt special process prescription and spinning technique method; Produce that flame retardant effect is lasting, washability is strong, and the weaved usefulness silicon-nitrogen with premium properties of viscose self is environment-friendly flame-retardant viscose fiber.
Silicon-nitrogen according to the invention is environmental protection flame retardant viscose staple fibre manufacturing approach, it is characterized in that comprising following processing step: fire retardant adds dissolving machine and mixes with viscose glue and pass through maturation then, spins pre-treatment, wet spinning, and drawing-off, cut-out, the fine hair shaping, concise, post processing;
Said fire retardant is by 5%～30% NaOH solution: viscose glue auxiliary agent: silicon-nitrogen combustion inhibitor: calgon=(1～10): (0.05～0.35): (3～18): the part by weight of (0.1～1) is allocated, and exchanges the retardant solution test proportion for preparing to confirm its composition;
Said retardant solution adds dissolving machine and the viscose glue blend step comprises: after the viscose glue dissolving of dissolving machine is good; Form and the glue amount according to viscose glue; Slowly add the good retardant solution of allotment by weight proportion, said part by weight is a mixing of viscose: retardant solution=100% that allotment is good
:(20%～36%); After adding retardant solution; The mixing speed of dissolving machine>=160 rev/min; Stir fast; Circular grinding 30 minutes to 90 minutes; Fire retardant and viscose glue are fully mixed, make the retardant solution of configuration can fully mix and reach better spinnability and flame retardant effect with viscose solution;
Said maturation step comprises: mixed viscose glue temperature is controlled in 16～28 ℃ the scope, and accomplished one filtration at 3 to 16 hours, deaeration, two roads filter;
The said pre-treatment step that spins is a spinnability improver of injecting relative viscose solution alpha cellulose weight 1.5%～3% before spinning, to improve spinnability;
The alpha cellulose weight ratio 7.0%～9.8% of the epoxy glue in the said wet spinning step; NaOH weight ratio 7.0%～8.5%; Falling ball viscosity 35 seconds～85 seconds; Degree of ripeness 6～20ml; 14～28 ℃ of glue temperature; Spinning bath is formed: sulfuric acid 75～125g/l; Zinc sulfate 15～50 g/l; Sodium sulphate 160～350 g/l; 40～52 ℃ of temperature; Shower nozzle specification: (1400～2200) hole * (aperture of 0.045mm～0.065mm);
Shower nozzle drawing-off-50%～60% in the said drafting step; Plasticizing drawing-off 15%～100%;
Said post-processing step comprises desulfurization, washing together, and bleaching, the washing of two roads is solidified, and the washing of three roads oils; Desulfurized step adopts NaOH or sodium sulfite desulfurization, and concentration is 0.5～8 g/l, 80 ± 5 ℃ of temperature; Blanching step adopts clorox or hydrogen peroxide bleaching, and concentration is 0.2～3 g/l, 30～50 ℃ of temperature, pH value 9.5～11.5; Fixation bath during curing schedule is formed: soft water: cured flame-retardant agent=(10%～80%): (90%～20%); 30～90 ℃ of temperature; Hardening time: 10 ± 5 minutes.Through this last handling process, make the fiber flame retardant effect further strengthen, have good textile performance simultaneously.
Viscose glue auxiliary agent according to the invention adopts V-32, and silicon-nitrogen combustion inhibitor adopts WS-801, and the proportion of WS-801 is 1.325～1.44, and the spinnability improver adopts WS-803, and WS-802 is adopted in the cured flame-retardant agent.
The dried fracture strength of the obtained fiber of the present invention >=2.00 CN/dtex; Wet breaking strength >=1.00 CN/dtex; Limited oxygen index >=28% can perform well in textile yarn and lining.
The specific embodiment
Allocate retardant solution earlier; Its method is: NaOH solution, the product viscose glue auxiliary agent V-32 of Nuo Baier Aksu company, calgon, the silicon-nitrogen combustion inhibitor WS-801 of allocating bucket adding 5%～30% by a certain percentage respectively to fire retardant; And constantly stir; That is: NaOH solution: viscose glue auxiliary agent V-32: calgon: silicon-nitrogen combustion inhibitor WS-801=(1～10): (0.05～0.35): (0.1～1): (3～18); Silicon-nitrogen combustion inhibitor WS-801 proportion: 1.325～1.44, exchange the retardant solution test proportion for preparing.After the viscose glue dissolving well of dissolving machine, form and the glue amount according to viscose glue, slowly add allotment retardant solution well by a certain percentage, concrete ratio is: mixing of viscose: retardant solution=100% that allotment is good
:(20%～36%), add retardant solution after, stir fast the mixing speed of dissolving machine>=160 rev/min, and circular grinding 30 minutes to 90 minutes, and fire retardant and viscose glue are fully mixed.Mixed viscose glue temperature is controlled in 16～28 ℃ the scope; Accomplished one filtration, deaeration, the filtration of two roads at 3 to 16 hours; Send spinning with epoxy glue afterwards; And before spinning injection about 2.5% spinnability improver WS-803 auxiliary agent, the shower nozzle specification is: (1400～2200) hole * (aperture of 0.045mm～0.065mm).Spinning glue is formed should be controlled at certain limit: first fine 7.0%～9.8%; Contain NaOH7.0%～8.5%; Falling ball viscosity 35 seconds～85 seconds; Degree of ripeness 6～20ml; 14～28 ℃ of glue temperature; The spinning bath composition is controlled at: sulfuric acid 70～125g/l; Zinc sulfate 15～50 g/l; Sodium sulphate 160～350 g/l; 40～52 ℃ of temperature; Degree of draft is: shower nozzle drawing-off-50%～60%; Plasticizing drawing-off 15%～100%; Fiber is through cutting off, and the fine hair grooving that slips gets into concise, adopts NaOH or sodium sulfite solution desulfurization; Concentration is 0.5～8 g/l; 80 ± 5 ℃ of temperature after washing (75～85 ℃ of temperature) is also squeezed together, adopt the bleaching of clorox or hydrogen peroxide solution; Concentration is 0.2～3 g/l; 30～50 ℃ of temperature, pH value 9.5～11.5 carries out washing of two roads and squeezing afterwards; Fiber gets into curing area, adopts cured flame-retardant agent WS-802 to solidify.Fixation bath is formed: soft water: cured flame-retardant agent WS-802=(10%～80%): (90%～20%); 30～90 ℃ of temperature; 10 ± 5 minutes hardening times, the more special-purpose NA100 type of the Fire resistant viscose fiber finish of producing through three road washings, squeezing, German Bu Saite company oil, squeezing, shredding, oven dry, etc. postprocessing working procedures obtain finished fiber.
The dried fracture strength of the obtained fiber of the present invention >=2.0 CN/dtex; Wet breaking strength >=1.0 CN/dtex; Limited oxygen index >=28% can perform well in textile yarn and lining.
Novel silicon-nitrogen is fire retardant viscose short filament; Silicon-nitrogen combustion inhibitor of selecting for use is that silicon-nitrogen that the great chemical company of domestic Xinxiang mayor produces is that WS-801 environment friendly flame retardant and WS-802 environment-friendly type are solidified fire retardant; Its flame retardant effect is lasting, washability is strong; And has a premium properties of viscose self; Powerful high, but textile performance might as well.Its fire retardant mechanism is: when running into flame, the part organic fiber becomes branch's burning, but inorganic silicon can not burn and can stop flame combustion, and silicon-nitrogen compound wherein has the hydration performance, can play the effect of shielding and knock down the flame.
Novel silicon-nitrogen is fire retardant viscose short filament; Silicon wherein is non-combustible matter; The cigarette amount discharges few during the nitrogen burning; Almost suitable through test with the smoke density of common viscose fiber; Discarded object can become nontoxic organic and inorganic mixture through natural degradation; Nitrogen is through the ammonia of photo-thermal and biodegradation generation and effective nutritional labeling that amine is plant, so it has the feature of environmental protection.
Embodiment 1:
Allocate retardant solution earlier; Its method is: add 10% NaOH solution, viscose glue auxiliary agent V-32, calgon, silicon-nitrogen combustion inhibitor WS-801 to fire retardant allotment bucket respectively by a certain percentage; And constantly stir; That is: 10% NaOH solution: viscose glue auxiliary agent V-32: calgon: silicon-nitrogen combustion inhibitor WS-801=8: 0.1: 0.2: 13; Silicon-nitrogen combustion inhibitor WS-801 proportion: 1.325～1.44, exchange the retardant solution test proportion for preparing.After the viscose glue dissolving well of dissolving machine, form and the glue amount according to viscose glue, slowly add allotment retardant solution well by a certain percentage, concrete ratio is: mixing of viscose: retardant solution=100% that allotment is good
:23%, add retardant solution after, stir fast the mixing speed of dissolving machine>=160 rev/min, and circular grinding 30 minutes, and fire retardant and viscose glue are fully mixed.Mixed viscose glue temperature is 26 ℃; Epoxy glue was accomplished one filtration, deaeration, the filtration of two roads in 14 hours; Send spinning with epoxy glue afterwards, and the spinnability reinforcing agent WS-803 auxiliary agent of injection 1.5% before spinning (fine to first), the shower nozzle specification is: 1900 holes * 0.065mm aperture.Spinning glue is formed: first fine 9.8%; Contain NaOH7.5%; Falling ball viscosity 45 seconds; Degree of ripeness 13ml; 25 ℃ of glue temperature; Spinning bath: sulfuric acid 120g/l; Zinc sulfate 18 g/l; Sodium sulphate 300 g/l; 49 ℃ of temperature; Degree of draft is: shower nozzle drawing-off 50%; Plasticizing drawing-off 30%; Fiber is through cutting off, and the fine hair grooving that slips gets into concise, adopts NaOH or sodium sulfite solution desulfurization; Concentration is 7g/l; 80 ℃ of temperature after washing together and squeezing, adopt liquor natrii hypochloritis's bleaching; Concentration is 2 g/l; 40 ℃ of temperature, pH value 11 carries out washing of two roads and squeezing afterwards; Fiber gets into curing area, adopts cured flame-retardant agent WS-802 to solidify.Fixation bath is formed: soft water: cured flame-retardant agent WS-802=75%:25%; 50 ℃ of temperature; 12 minutes hardening times, again through three roads wash, squeeze, oil, squeezing, shredding, oven dry, etc. postprocessing working procedures obtain finished fiber.
Dried fracture strength 2.20 CN/dtex of the obtained fiber of the present invention; Wet breaking strength 1.10 CN/dtex; Limited oxygen index 30.0% can perform well in textile yarn and lining.
Embodiment 2:
Allocate retardant solution earlier; Its method is: add 15% NaOH solution, viscose glue auxiliary agent V-32, calgon, silicon-nitrogen combustion inhibitor WS-801 to fire retardant allotment bucket respectively by a certain percentage; And constantly stir; That is: 15% NaOH solution: viscose glue auxiliary agent V-32: calgon: silicon-nitrogen combustion inhibitor WS-801=6: 0.5: 0.3:14; Silicon-nitrogen combustion inhibitor WS-801 proportion: 1.325～1.44, exchange the retardant solution test proportion for preparing.After the viscose glue dissolving well of dissolving machine, form and the glue amount according to viscose glue, slowly add allotment retardant solution well by a certain percentage, concrete ratio is: mixing of viscose: retardant solution=100% that allotment is good
:25%, add retardant solution after, stir fast the mixing speed of dissolving machine>=160 rev/min, and circular grinding 45 minutes, and fire retardant and viscose glue are fully mixed.Mixed viscose glue temperature is 26 ℃; Epoxy glue was accomplished one filtration, deaeration, the filtration of two roads in 15 hours; Send spinning with epoxy glue afterwards, and the spinnability reinforcing agent WS-803 auxiliary agent of injection 2.0% before spinning (fine to first), the shower nozzle specification is: 1900 holes * 0.06mm aperture.Spinning glue is formed: first fine 9.8%; Contain NaOH7.8%; Falling ball viscosity 40 seconds; Degree of ripeness 12ml; 25 ℃ of glue temperature; Spinning bath: sulfuric acid 118g/l; Zinc sulfate 15g/l; Sodium sulphate 320 g/l; 48 ℃ of temperature; Degree of draft is: shower nozzle drawing-off 45%; Plasticizing drawing-off 30%; Fiber is through cutting off, and the fine hair grooving that slips gets into concise, adopts NaOH or sodium sulfite solution desulfurization; Concentration is 6g/l; 80 ℃ of temperature after washing together and squeezing, adopt liquor natrii hypochloritis's bleaching; Concentration is 1.5 g/l; 40 ℃ of temperature, pH value 11 carries out washing of two roads and squeezing afterwards; Fiber gets into curing area, adopts cured flame-retardant agent WS-802 to solidify.Fixation bath is formed: soft water: cured flame-retardant agent WS-802=80%:20%; 60 ℃ of temperature; 10 minutes hardening times, again through three roads wash, squeeze, oil, squeezing, shredding, oven dry, etc. postprocessing working procedures obtain finished fiber.
Dried fracture strength 2.10 CN/dtex of the obtained fiber of the present invention; Wet breaking strength 1.05 CN/dtex; Limited oxygen index 28.5% can perform well in textile yarn and lining.
Embodiment 3:
Allocate retardant solution earlier; Its method is: add 20% NaOH solution, viscose glue auxiliary agent V-32, calgon, silicon-nitrogen combustion inhibitor WS-801 to fire retardant allotment bucket respectively by a certain percentage; And constantly stir; That is: 20% NaOH: viscose glue auxiliary agent V-32: calgon: silicon-nitrogen combustion inhibitor WS-801=4:0.8: 0.2: 15; Fire retardant 801 proportions: 1.325～1.44, exchange the retardant solution test proportion for preparing.After the viscose glue dissolving well of dissolving machine, form and the glue amount according to viscose glue, slowly add allotment retardant solution well by a certain percentage, concrete ratio is: mixing of viscose: retardant solution=100% that allotment is good
:25%, add retardant solution after, stir fast the mixing speed of dissolving machine>=160 rev/min, and circular grinding 60 minutes, and fire retardant and viscose glue are fully mixed.Mixed viscose glue temperature is 23 ℃; Epoxy glue was accomplished one filtration, deaeration, the filtration of two roads in 12 hours; Send spinning with epoxy glue afterwards, and the spinnability reinforcing agent WS-803 auxiliary agent of injection 2.5% before spinning (fine to first), the shower nozzle specification is: 1750 holes * 0.062mm aperture.Spinning glue is formed: first fine 9.8%; Contain NaOH8.0%; Falling ball viscosity 33 seconds; Degree of ripeness 13ml; 25 ℃ of glue temperature; Spinning bath: sulfuric acid 115g/l; Zinc sulfate 16 g/l; Sodium sulphate 330 g/l; 49 ℃ of temperature; Degree of draft is: shower nozzle drawing-off 35%; Plasticizing drawing-off 35%; Fiber is through cutting off, and the fine hair grooving that slips gets into concise, adopts NaOH or sodium sulfite solution desulfurization; Concentration is 7g/l; 80 ℃ of temperature after washing together and squeezing, adopt liquor natrii hypochloritis's bleaching; Concentration is 2 g/l; 40 ℃ of temperature, pH value 11 carries out washing of two roads and squeezing afterwards; Fiber gets into curing area, adopts cured flame-retardant agent WS-802 to solidify.Fixation bath is formed: soft water: cured flame-retardant agent WS-802=70%:30%; 55 ℃ of temperature; 12 minutes hardening times, again through three roads wash, squeeze, oil, squeezing, shredding, oven dry, etc. postprocessing working procedures obtain finished fiber.
The dried fracture strength of the obtained fiber of the present invention, 2.10 CN/dtex; Wet breaking strength 1.05CN/dtex; Limited oxygen index 29.5% can perform well in textile yarn and lining.
The simple deformation or the combination of every embodiment of the invention technical scheme and technical characterictic all should be thought to fall into protection scope of the present invention.
Claims (2)
1. a silicon-nitrogen is environmental protection flame retardant viscose staple fibre manufacturing approach, it is characterized in that comprising following processing step: fire retardant adds dissolving machine and mixes with viscose glue and pass through maturation then, spins pre-treatment, wet spinning, drawing-off, cut-out, fine hair shaping, post processing;
Said fire retardant is by 5%～30% NaOH solution: viscose glue auxiliary agent: silicon-nitrogen combustion inhibitor: calgon=(1～10): (0.05～0.35): (3～18): the part by weight of (0.1～1) is allocated, and exchanges the retardant solution test proportion for preparing to confirm its composition;
Said retardant solution adds dissolving machine and the viscose glue blend step comprises: after the viscose glue dissolving of dissolving machine is good; Form and the glue amount according to viscose glue; Slowly add the good retardant solution of allotment by weight proportion, said part by weight is a mixing of viscose: retardant solution=100% that allotment is good
:(20%～36%), add retardant solution after, stir fast the mixing speed of dissolving machine>=160 rev/min, circular grinding 30 minutes to 90 minutes fully mixes fire retardant and viscose glue;
Said maturation step comprises: mixed viscose glue temperature is controlled in 16～28 ℃ the scope, and accomplished one filtration at 3 to 16 hours, deaeration, two roads filter;
The said pre-treatment step that spins is a spinnability improver of injecting relative viscose solution alpha cellulose weight 1.5%～3% before spinning;
The alpha cellulose weight ratio 7.0%～9.8% of the epoxy glue in the said wet spinning step; NaOH weight ratio 7.0%～8.5%; Falling ball viscosity 35 seconds～85 seconds; Degree of ripeness 6～20ml; 14～28 ℃ of glue temperature; Spinning bath is formed: sulfuric acid 75～125g/l; Zinc sulfate 15～50 g/l; Sodium sulphate 160～350 g/l; 40～52 ℃ of temperature; Shower nozzle specification: (1400～2200) hole * (aperture of 0.045mm～0.065mm);
Shower nozzle drawing-off-50%～60% in the said drafting step; Plasticizing drawing-off 15%～100%;
Said post-processing step comprises desulfurization, washing together, and bleaching, the washing of two roads is solidified, and the washing of three roads oils; Desulfurized step adopts NaOH or sodium sulfite desulfurization, and concentration is 0.5～8 g/l, 80 ± 5 ℃ of temperature; Blanching step adopts clorox or hydrogen peroxide bleaching, and concentration is 0.2～3 g/l, 30～50 ℃ of temperature, pH value 9.5～11.5; Fixation bath during curing schedule is formed: soft water: cured flame-retardant agent=(10%～80%): (90%～20%); 30～90 ℃ of temperature; Hardening time: 10 ± 5 minutes.
2. silicon-nitrogen according to claim 1 is environmental protection flame retardant viscose staple fibre manufacturing approach; It is characterized in that: said viscose glue auxiliary agent adopts V-32; Silicon-nitrogen combustion inhibitor adopts WS-801; The proportion of WS-801 is 1.325～1.44; The spinnability improver adopts WS-803, and WS-802 is adopted in the cured flame-retardant agent.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0336004A2 (en) * | 1988-04-05 | 1989-10-11 | Kohjin Co., Ltd. | High functional regenerated cellulose composition |
| CN101070633A (en) * | 2007-05-17 | 2007-11-14 | 山东海龙股份有限公司 | Method for preparing cellulose and silicon dioxide composite coloured fiber and coloured fiber made thereby |
| KR20090025979A (en) * | 2007-09-07 | 2009-03-11 | 주식회사 코오롱 | Flame-retardant cellulose filament fiber, tire cord, and method for preparing the same |
| CN101387013A (en) * | 2008-05-14 | 2009-03-18 | 中原工学院 | Environment friendly flame-retardant viscose fiber manufacturing technology |
| CN101724926A (en) * | 2009-11-18 | 2010-06-09 | 马晓宁 | Spinning process of environment-friendly flame retarding flat viscose yarn |
-
2011
- 2011-07-27 CN CN2011102119632A patent/CN102352539B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0336004A2 (en) * | 1988-04-05 | 1989-10-11 | Kohjin Co., Ltd. | High functional regenerated cellulose composition |
| CN101070633A (en) * | 2007-05-17 | 2007-11-14 | 山东海龙股份有限公司 | Method for preparing cellulose and silicon dioxide composite coloured fiber and coloured fiber made thereby |
| KR20090025979A (en) * | 2007-09-07 | 2009-03-11 | 주식회사 코오롱 | Flame-retardant cellulose filament fiber, tire cord, and method for preparing the same |
| CN101387013A (en) * | 2008-05-14 | 2009-03-18 | 中原工学院 | Environment friendly flame-retardant viscose fiber manufacturing technology |
| CN101724926A (en) * | 2009-11-18 | 2010-06-09 | 马晓宁 | Spinning process of environment-friendly flame retarding flat viscose yarn |
Non-Patent Citations (1)
| Title |
|---|
| 张瑞文等: "新型阻燃剂用于粘胶纤维共混改性的研究", 《2010年中国阻燃学术年会》 * |
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