CN103334177A - Flame-retardant corn protein fiber production method and product thereof - Google Patents

Flame-retardant corn protein fiber production method and product thereof Download PDF

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CN103334177A
CN103334177A CN2013103281159A CN201310328115A CN103334177A CN 103334177 A CN103334177 A CN 103334177A CN 2013103281159 A CN2013103281159 A CN 2013103281159A CN 201310328115 A CN201310328115 A CN 201310328115A CN 103334177 A CN103334177 A CN 103334177A
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polyvinyl alcohol
corn protein
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CN103334177B (en
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韩晓根
李建伟
张玲
尚金萍
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韩晓根
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Abstract

The invention relates to a flame-retardant corn protein fiber production method and a product thereof. The product is produced through the following steps: dissolving corn protein powder in water, adding sodium phosphate, sodium hydroxide and acetamide and heating and stirring to prepare corn protein solution; mixing the corn protein solution with soaked polyvinyl alcohol, adding formaldehyde, glutaraldehyde, benzoyl peroxide, decabromodiphenyl ether, antimony trioxide, reactive dye, boric acid and sodium tetraborate at different temperatures and stirring to obtain spinnable solution, wherein the sizes of the decabromodiphenyl ether and the antimony trioxide is not greater than 100 nm; filtering and performing vacuum deaerationon the spinnable solution; and spinning by using the conventional wet spinning process. In the fiber provided by the invention, a fire retardant is uniformly dispersed in the fiber, does not seep or lose easily and has an excellent fire retardation effect; and meanwhile, the fiber has satisfactory dry and wet breaking strength, dry and wet elongation at break and color fastness.

Description

A kind of fire-retardant Zein fibers production method and products thereof
Technical field:
The present invention relates to a kind of azelon production method and products thereof, relate in particular to production method of a kind of Zein fibers with flame retardant effect and products thereof.
Background technology:
Zein fibers belongs to a kind of artificial synthetic fiber, is treated zein and high polymer are carried out copolymerization, blend the fiber that forms through spinning.The present inventor once disclosed a kind of Zein fibers and production method thereof in CN19522225A.
There is the fire of half to be caused by textiles in the life.China's fire causes direct or indirect loss to reach 10,000,000,000 yuan every year, and only the fire in Henan Province just causes hundreds of people's death.Artificial fibre and synthetic fiber all are inflammable usually, and the overwhelming majority will decompose and burn below 300 ℃.Zein fibers belongs to a kind of artificial fibre, and it belongs to a kind of synthetic fiber of easy burning equally.
Fire resistance fibre refers to have the fiber of anti-flammability.At present the production method of fire resistance fibre is carried out subsequent treatment after mostly being greatly fibrillation being weaved again, namely the finishing agent that contains fire retardant is coated to fiber surface in the presence of certain binder, thereby formation has the fiber of flame retardant effect.But in the fire resistance fibre that forms by this class methods, fire retardant is relatively poor relatively at the adhesive force of fiber surface, As time goes on, oozes out easily, flows out, and causes the durability of flame retardant effect can not be satisfactory.Simultaneously, because the extra use of finishing agent, binder has to consider the problem that they bring for health.Equally, these class methods also can cause production stage to increase problems such as production cost rising.
Summary of the invention:
Scope of the present invention only by claims regulation, is not limit by the statement of this joint summary of the invention on any degree.
One object of the present invention is to provide a kind of method of producing fire-retardant Zein fibers, comprises the steps:
A) the corn protein powder is water-soluble, make mass fraction and be 25% protein solution, heating is also fully stirred, and adds following component in the time of 50 ℃-80 ℃, and addition is with respect to protein solution:
Sodium phosphate 0.5-1.0g/L
NaOH 0.3-0.4%
Acetamide 2-4 weight portion/every 160-200 weight portion protein solution
Keep down stirring 1-3 hour at 80 ℃;
B) use demineralized water that polyvinyl alcohol is softened immersion, obtain the polyvinyl alcohol that moisture is 88-92%;
C) take by weighing the corn protein solution of the 160-200 weight portion that step a) obtains and the polyvinyl alcohol of the 800-840 weight portion that step b) obtains, its mixing is obtained the spinning solution of 1000 weight portions, stir and add following component when being heated to 55 ℃-75 ℃, addition with respect to the quality of spinning solution is:
Formaldehyde: 0.4-0.6%
Glutaraldehyde: 0.3-0.6%
Dibenzoyl peroxide: 0.01-0.05%
At 75 ℃-95 ℃, add following component, addition with respect to the quality of spinning solution is:
Deca-BDE: 10-16%
Antimonous oxide: 6-8%
REACTIVE DYES: 0.8-1.4%
Boric acid: 0.2-0.4%
Sodium tetraborate: 0.4-0.6%
Fully stirring spinning solution and heating make its temperature reach 93-95 ℃, keep 3-4 hour, obtain spinnable solution, and wherein, the particle size of described deca-BDE and antimonous oxide is not more than 100 nanometers;
D) use the above filter screen of 400 orders that spinnable solution is filtered, and vacuum defoamation 3-4 hour;
E) adopt conventional wet spinning technology to carry out spinning.
Use preferably in step b) that the degree of polymerization is 1775 ± 75, alcoholysis degree is the fibre-grade polyvinyl alcohol of 99.8-100%.
Preferred, employed polyvinyl alcohol is 90% through the moisture after soaking.
Preferably, in step c), described REACTIVE DYES is reactive red LS-B, a kind of or its combination of reactive yellow LS-R and reactive navy blue LS-G.
Preferably, in step c), before adding spinning solution, deca-BDE and antimonous oxide are fully ground the back cross sieve more than 320 orders, REACTIVE DYES uses the methylene dinaphthalene disodium sulfonate to grind dispersion treatment and by the above strainer filtering of 600 orders.
Preferred, in step c), the weight of REACTIVE DYES is 1.6-14 times of the used weight of dispersant methylene dinaphthalene disodium sulfonate.
Preferred, in step c), use 600-800 purpose filter screen that the REACTIVE DYES after disperseing is filtered.
Preferably, in step d), use 400-600 purpose filter screen that spinning solution is carried out filtration more than 4 roads.
Carry out spinning according to conventional wet spinning technology, preferred parameter is: The hole diameter of spinneret 0.07-0.12mm, draw ratio 60, spray silk speed 6.8-7.0 mm/second, spinning linear speed 5.5 mm/second.
Further to silk carry out dry heat drafting, crosslinked, the conventional operations such as typing, cut-out of washing, oil, dry, curl just can obtain finished silk.
The production technology of fire-retardant Zein fibers of the present invention is simple, has saved in the traditional treatment method step to the follow-up interpolation fire retardant of fabric, and has not needed additionally to use binder and finishing agent, and production method environmental protection and production cost are effectively controlled.
The Zein fibers that another object of the present invention is to provide a kind of good flame retardation effect, flame retardant effect is durable and have good fibre property, described Zein fibers is prepared by above method.
In the fire-retardant Zein fibers by this method preparation, fire retardant deca-BDE and antimony trioxide can produce the cooperative flame retardant effect, and flame retardant effect is very good.Simultaneously, fire retardant is dispersed in fibrous inside, be difficult for oozing out, running off, but fire retardation has good persistence.The fibre property of fiber of the present invention does not significantly descend because of the adding of fire retardant, and it still has gratifying dried, wet breaking strength, do, wet elongation at break and COLOR FASTNESS.Therefore, the cloth that fiber of the present invention is made into can be made lovely luster, comfortable and easy to wear and have the fabric of good fire retardant performance, and market prospects are huge.
The specific embodiment:
Elaborate the present invention below, but do not limit the present invention in the scope of the described specific embodiment.
The preparation of corn protein solution
In reactor, add demineralized water and refining corn protein powder, press the weight proportion of 3:1.The corn protein solution for preparing is added in the stirred autoclave, stir then and heat, in the time of 50 ℃-80 ℃, add sodium phosphate, NaOH and acetamide.
The addition of sodium phosphate is every liter of albumen stoste of 0.5-1.0g, and the addition of NaOH is the 0.3-0.4% of albumen stock solution quality, and the purpose that adds the two is for the protein solution that alkalizes.
Acetamide can make the non-polar group that is wrapped in protein molecule inside come out, thus some surface active properties such as the emulsibility of change protein, emulsion stability, foaminess, foam stability.The acetamide addition is 2-4 weight portion/every 160-200 weight portion protein solution.
This protein solution is heated to 80 ℃ keeps down stirring 1-3 hour, finish the linearization process to corn protein.
The immersion of polyvinyl alcohol
The purpose of using demineralized water that polyvinyl alcohol is soaked is to remove slag remaining in the polyvinyl alcohol and useless acid group, is that polyvinyl alcohol is softened processing simultaneously.Can reach 88-92% through soaking the moisture of softening the polyvinyl alcohol after handling, be beneficial to preparation and the spinning process of follow-up spinning solution.The present invention preferably uses the fibre-grade polyvinyl alcohol of the degree of polymerization 1775 ± 75, alcoholysis degree 99.8-100%, when its moisture is 90%, and bating effect the best.
Demineralized water used in the present invention can provide by the general industry water softening plant.
The preparation of spinning solution
Take by weighing the corn protein solution 160-200 weight portion and the soaked polyvinyl alcohol 800-840 weight portion that make, in reactor, they are mixed, obtain the spinning solution of 1000 weight portions.
When stirring this spinning solution and being heated to 55 ℃-75 ℃, to wherein adding formaldehyde, glutaraldehyde and dibenzoyl peroxide.Formaldehyde and glutaraldehyde as crosslinking agent can with protein on amino group form adduct, form complicated highly cross-linked structure at last and improve fibre strength and heat resistance.The addition of formaldehyde is 0.4-0.6% with respect to the quality of spinning solution, and the addition of glutaraldehyde is 0.3-0.6% with respect to the quality of spinning solution.Dibenzoyl peroxide uses as initator, and its addition is 0.01-0.05% with respect to the quality of spinning solution.
When continuing to be heated with stirring to 75 ℃-95 ℃, add fire retardant, REACTIVE DYES, boric acid and sodium tetraborate.
Fire retardant used in the present invention is deca-BDE and antimonous oxide.Wherein, deca-BDE can discharge hydrogen bromide in the time-division solution of being heated and produce flame retardant effect, and antimonous oxide can strengthen the active free radical of catching the participation combustion reaction, and can produce the certain physical barriering effect, act synergistically thereby produce, strengthened the flame retardant effect of deca-BDE.For with the abundant blend of fibrous material, the particle size of the fire retardant among the present invention should be not more than 100 nm.Preferably, use high shear dispersion grinding equipment grinds and the screen cloth more than mistake 320 orders fully before adding fire retardant.
Among the present invention, the deca-BDE addition is the 10-16% with respect to the quality of spinning solution, and the antimonous oxide addition is the 6-8% with respect to the spinning solution quality.
The purpose that adds REACTIVE DYES to spinning solution is for corn fire resistance fibre of the present invention is dyeed.Contain the active group that can form covalent bonds with relevant radical reaction in the fiber in the reactive dyestuff molecule.For antibiotic Zein fibers of the present invention, suitable REACTIVE DYES should be can react with Zein fibers and polyvinyl alcohol, have a kind than high colour-fast rate.The inventor finds that reactive red LS-B, reactive yellow LS-R, reactive navy blue LS-G are particularly suitable REACTIVE DYES.
The chemical constitution of reactive red LS-B is:
Figure 461117DEST_PATH_IMAGE001
The chemical constitution of reactive yellow LS-R is: X-(CH 2) 3-X, wherein X represents following group:
The chemical constitution of reactive navy blue LS-G is: Y-CO-NH-Z, and wherein Y represents following group:
Figure 95678DEST_PATH_IMAGE003
Z represents following group:
Figure 490887DEST_PATH_IMAGE004
The total addition of REACTIVE DYES is the 0.8-1.4% of spinning solution.This moment the finished product Zein fibers bright-colored, be difficult for fading, and the adding of dyestuff is very little to the fibre machinery Effect on Performance.Dyestuff need evenly disperse in spinning solution, so the present invention uses dispersant that REACTIVE DYES is carried out dispersion treatment in advance.Dispersant refers to improve the auxiliary agent of solid material dispersive property.Dispersant and solid material are ground jointly, can stop material particles to condense again and keep the stable of dispersion liquid.For method of the present invention, suitable dispersant is the methylene dinaphthalene disodium sulfonate, and the quality of REACTIVE DYES is 1.6-14 times of dispersant quality.Can use common grinding dispersing apparatus to carry out described dispersion treatment.Described REACTIVE DYES also should filter to remove slag in the past at the adding spinning solution by the filter screen more than 600 orders after dispersion treatment, consider that from the angle of cost and time the 600-800 mesh filter screen is suitable.
The purpose that adds boric acid and sodium tetraborate is that pH value and the viscosity of regulating spinning solution are beneficial to the wet spinning operation, and the addition of boric acid is 0.2-0.4% with respect to the spinning solution quality, and the addition of sodium tetraborate is 0.4-0.6% with respect to the spinning solution quality.At this moment, the pH of spinning solution is 4.6-4.8, and viscosity is 420-460 second (industrial rotary-type viscosimeter records).
Fully stirring spinning solution and heating make its temperature reach 93-95 ℃, keep 3-4 hour, obtain spinnable solution.
The wet spinning operation
Use the above filter screen of 400 orders that spinnable solution is filtered, from effect and cost consideration, it is suitable using 4 roads above 400-600 purpose filter screen.
Vacuum defoamation 3-4 hour to remove the bubble in the spinning solution.
Adopt conventional wet spinning technology to carry out spinning, The hole diameter of spinneret is 0.07-0.12mm, draw ratio 60, spray silk speed 6.8-7.0 mm/second, spinning linear speed 5.5 mm/second.
Subsequent handling
By conventional means to spinning process gained fiber carry out dry heat drafting, crosslinked, wash, oil, oven dry, the typing of curling, operations such as cut-out obtain finished silk.
Embodiment 1
25% the corn protein solution of preparation 160kg, wherein the addition of sodium phosphate, NaOH and acetamide is respectively 0.5g/L protein solution, 0.3% and 2kg, and adding temperature is 50 ℃.Stir and be heated to and keep again under 80 ℃ stirring 1 hour, finish the linearization process to corn protein.
Use demineralized water that the fibre-grade polyvinyl alcohol of the 67.2kg degree of polymerization 1775 ± 75, alcoholysis degree 99.8-100% is soaked, obtain moisture and be 92% polyvinyl alcohol 840kg.
The 100kg deca-BDE and the 60kg antimony trioxide that are of a size of 100nm are added in the high shear disperse mill, and the speed of dispersion grinding is 2000 rev/mins, and milling time is 4 hours, and it is standby that the mixture that obtains is crossed 320 mesh sieves.
To amount to reactive red LS-B, the reactive yellow LS-R of 8kg and three kinds of dyestuffs of reactive navy blue LS-G according to the ratio that satisfies the color matching demand, 3:2:3 for example, join in the 5kg methylene dinaphthalene disodium sulfonate, rotating speed with 2000 rpms grinds dispersion 4 hours in the multi-functional dispersion machine of SDF400 type then, and it is standby that the mill base after grinding is crossed 600 mesh filter screens.
Polyvinyl alcohol after the 160kg corn protein solution that will prepare in reactor and 840kg soak mixes, and obtains the spinning solution of 1000kg.When stirring this spinning solution and being heated to 55 ℃, add formaldehyde 4kg, glutaraldehyde 3kg and dibenzoyl peroxide 0.1kg.Continue agitating heating, when temperature reaches 75 ℃, add the flame-retardant mixture, REACTIVE DYES dispersion liquid, boric acid 2kg, the sodium tetraborate 4kg that prepare.When being heated to 93 ℃, make spinning solution keep stirring 3 hours, obtain spinnable solution.
Use 4 roads, 400 mesh filter screens that spinnable solution is filtered also vacuum defoamation 3 hours.
Adopt conventional wet spinning technology to carry out spinning, The hole diameter of spinneret is 0.07mm, draw ratio 60, spray silk speed 6.8 mm/second, spinning linear speed 5.5 mm/second.
By conventional means to spinning process gained fiber carry out dry heat drafting, crosslinked, the operations such as typing, cut-out of washing, oil, dry, curl obtain finished silk.The index of finished silk related mechanical properties is recorded in the table 1.
Embodiment 2
25% the corn protein solution of preparation 180kg, wherein the addition of sodium phosphate, NaOH and acetamide is respectively 0.75g/L protein solution, 0.35% and 3kg, and adding temperature is 65 ℃.Stir and be heated to and keep again under 80 ℃ stirring 2 hours, finish the linearization process to corn protein.
Use demineralized water that the fibre-grade polyvinyl alcohol of the 82kg degree of polymerization 1775 ± 75, alcoholysis degree 99.8-100% is soaked, obtain moisture and be 90% polyvinyl alcohol 820kg.
The 130kg deca-BDE and the 70kg antimony trioxide that are of a size of 60nm are added in the high shear disperse mill, and the speed of dispersion grinding is 2000 rev/mins, and milling time is 4 hours, and it is standby that the flame-retardant mixture that obtains is crossed 500 mesh sieves.
To amount to reactive red LS-B, the reactive yellow LS-R of 11kg and three kinds of dyestuffs of reactive navy blue LS-G according to the ratio 3:2:3 that satisfies the color matching demand, join in the 1.4kg methylene dinaphthalene disodium sulfonate, rotating speed with 2000 rpms grinds dispersion 4 hours in the multi-functional dispersion machine of SDF400 type then, and it is standby that the mill base after grinding is crossed 700 mesh filter screens.
Polyvinyl alcohol after the 180kg corn protein solution that will prepare in reactor and 820kg soak mixes, and obtains the spinning solution of 1000kg.When stirring this spinning solution and being heated to 65 ℃, add formaldehyde 5kg, glutaraldehyde 4.5kg and dibenzoyl peroxide 0.3kg.Continue agitating heating, when temperature reaches 85 ℃, add the flame-retardant mixture, REACTIVE DYES dispersion liquid, boric acid 3kg, the sodium tetraborate 5kg that prepare.When being heated to 94 ℃, make spinning solution keep stirring 3.5 hours, obtain spinnable solution.
Use 4 roads, 500 mesh filter screens that spinnable solution is filtered also vacuum defoamation 3.5 hours.
Adopt conventional wet spinning technology to carry out spinning, The hole diameter of spinneret is 0.095mm, draw ratio 60, spray silk speed 6.9 mm/second, spinning linear speed 5.5 mm/second.
By conventional means to spinning process gained fiber carry out dry heat drafting, crosslinked, the operations such as typing, cut-out of washing, oil, dry, curl obtain finished silk.The index of finished silk related mechanical properties is recorded in the table 1.
Embodiment 3
25% the corn protein solution of preparation 200kg, wherein the addition of sodium phosphate, NaOH and acetamide is respectively 1.0g/L protein solution, 0.4% and 4kg, and adding temperature is 80 ℃.Under 80 ℃, keep again stirring 3 hours, finish the linearization process to corn protein.
Use demineralized water that the fibre-grade polyvinyl alcohol of the 96kg degree of polymerization 1775 ± 75, alcoholysis degree 99.8-100% is soaked, obtain moisture and be 88% polyvinyl alcohol 800kg.
The 160kg deca-BDE and the 80kg antimony trioxide that are of a size of 20nm are added in the high shear disperse mill, and the speed of dispersion grinding is 2000 rev/mins, and milling time is 4 hours, and it is standby that the flame-retardant mixture that obtains is crossed 800 mesh sieves.
To amount to reactive red LS-B, the reactive yellow LS-R of 14kg and three kinds of dyestuffs of reactive navy blue LS-G according to the ratio 3:2:3 that satisfies the color matching demand, join in the 1kg methylene dinaphthalene disodium sulfonate, rotating speed with 2000 rpms grinds dispersion 4 hours in the multi-functional dispersion machine of SDF400 type then, and it is standby that the mill base after grinding is crossed 800 mesh filter screens.
Polyvinyl alcohol after the 200kg corn protein solution that will prepare in reactor and 800kg soak mixes, and obtains the spinning solution of 1000kg.When stirring this spinning solution and being heated to 75 ℃, add formaldehyde 6kg, glutaraldehyde 6kg and dibenzoyl peroxide 0.5kg.Continue agitating heating, when temperature reaches 95 ℃, add the flame-retardant mixture, REACTIVE DYES dispersion liquid, boric acid 4kg, the sodium tetraborate 6kg that prepare.Make spinning solution keep stirring 4 hours at 95 ℃, obtain spinnable solution.
Use 4 roads, 600 mesh filter screens that spinnable solution is filtered also vacuum defoamation 4 hours.
Adopt conventional wet spinning technology to carry out spinning, The hole diameter of spinneret is 0.12mm, draw ratio 60, spray silk speed 7.0 mm/second, spinning linear speed 5.5 mm/second.
By conventional means to spinning process gained fiber carry out dry heat drafting, crosslinked, the operations such as typing, cut-out of washing, oil, dry, curl obtain finished silk.The index of finished silk related mechanical properties is recorded in the table 1.
Comparative Examples
Comparative Examples is operated identical with embodiment 1 except not adding flame-retardant mixture.The index of finished silk related mechanical properties is recorded in the table 1.
With reference to the oxygen index (OI) of the above finished silk of mensuration viscose staple fibre fire resistance determination of test method of FZT 50016-2011 standard record, outcome record is in table 1.
Measure the COLOR FASTNESS of above finished silk according to the method for GB/T 3920-2008 standard record, outcome record is in table 1.
Table 1
? Embodiment 1 Embodiment 2 Embodiment 3 Comparative Examples
Do fracture strength 3.7 CN/dtex 3.8 CN/dtex 3.7 CN/dtex 3.8 CN/dtex
Wet breaking strength 2.7 CN/dtex 2.9 CN/dtex 2.6 CN/dtex 2.9 CN/dtex
Dried elongation at break 18.9% 18.0% 19.6% 20.7%
Wet elongation at break 20.3% 19.8% 20.7% 21.0%
Oxygen index (OI) 29 31 33 11
COLOR FASTNESS 4-5 grades 4-5 grades 4-5 grades 4-5 grades
By above experimental result as can be known, Zein fibers of the present invention has good flame, and the adding of fire retardant does not simultaneously obviously reduce the fibre machinery performance of Zein fibers.
And COLOR FASTNESS is splendid after the stock-dye of the present invention, can make various flame-retardant textiles bright-colored, that be difficult for fading, has wide value.

Claims (11)

1. method of producing fire-retardant Zein fibers may further comprise the steps:
A) the corn protein powder is water-soluble, make mass fraction and be 25% protein solution, heating is also fully stirred, and adds following component in the time of 50 ℃-80 ℃, and addition is with respect to protein solution:
Sodium phosphate 0.5-1.0g/L
NaOH 0.3-0.4%
Acetamide 2-4 weight portion/every 160-200 weight portion protein solution
Keep down stirring 1-3 hour at 80 ℃;
B) use demineralized water that polyvinyl alcohol is softened immersion, obtain the polyvinyl alcohol that moisture is 88-92%;
C) take by weighing the corn protein solution of the 160-200 weight portion that step a) obtains and the polyvinyl alcohol of the 800-840 weight portion that step b) obtains, its mixing is obtained the spinning solution of 1000 weight portions, stir and add following component when being heated to 55 ℃-75 ℃, addition with respect to the quality of spinning solution is:
Formaldehyde: 0.4-0.6%
Glutaraldehyde: 0.3-0.6%
Dibenzoyl peroxide: 0.01-0.05%
At 75 ℃-95 ℃, add following component, addition with respect to the quality of spinning solution is:
Deca-BDE: 10-16%
Antimonous oxide: 6-8%
REACTIVE DYES: 0.8-1.4%
Boric acid: 0.2-0.4%
Sodium tetraborate: 0.4-0.6%
Fully stirring spinning solution and heating make its temperature reach 93 ℃-95 ℃, keep 3-4 hour, obtain spinnable solution, and wherein, the particle size of described deca-BDE and antimonous oxide is not more than 100 nanometers;
D) use the above filter screen of 400 orders that spinnable solution is filtered, and vacuum defoamation 3-4 hour;
E) adopt conventional wet spinning technology to carry out spinning.
2. the method for claim 1, described polyvinyl alcohol are that the degree of polymerization is 1775 ± 75, alcoholysis degree is the fibre-grade polyvinyl alcohol of 99.8-100%.
3. the method for claim 2, described polyvinyl alcohol is 90% through the moisture after soaking.
4. the method for claim 1, REACTIVE DYES described in the step c) is reactive red LS-B, a kind of or its combination of reactive yellow LS-R and reactive navy blue LS-G.
5. the method for claim 1, in the step c), before adding spinning solution, deca-BDE and antimonous oxide fully to be ground the back cross sieve more than 320 orders, REACTIVE DYES uses the methylene dinaphthalene disodium sulfonate to grind dispersion treatment and by the above strainer filtering of 600 orders.
6. the method for claim 5, the weight of REACTIVE DYES described in the step c) be the used weight of described methylene dinaphthalene disodium sulfonate 1.6-14 doubly.
7. the method for claim 5 is filtered the REACTIVE DYES after disperseing by 600-800 purpose filter screen in the step c).
8. the method for claim 1 uses 400-600 purpose filter screen that spinnable solution is carried out filtration more than 4 roads in the step d).
9. the method for claim 1, the parameter in the step e) is: The hole diameter of spinneret 0.07-0.12mm, draw ratio 60, a spray silk speed 6.8-7.0 mm/second, spinning linear speed 5.5 mm/second.
10. the described arbitrary method of claim 1-9, it comprises that further dry heat drafting, crosslinked, the conventional operations such as typing, cut-out of washing, oil, dry, curl are to obtain finished fiber.
11. a fire-retardant Zein fibers, it is by either party's method preparation of claim 1-10.
CN201310328115.9A 2013-07-31 2013-07-31 Flame-retardant corn protein fiber production method and product thereof Active CN103334177B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2475879A (en) * 1946-02-09 1949-07-12 Du Pont Process for the continuous spinning and stretching of zein filaments
CN1286325A (en) * 1999-09-01 2001-03-07 李官奇 Synthetic plant protein filaments
CN1524980A (en) * 2003-02-28 2004-09-01 李官奇 Synthetic fiber containing animal hair protein and manufacturing method thereof
CN1800455A (en) * 2005-01-06 2006-07-12 李官奇 Protein fiber spinning dope and its production method
CN1952225A (en) * 2006-04-28 2007-04-25 韩晓根 Maize protein colored textile fiber and method for producing same
CN102817101A (en) * 2012-07-31 2012-12-12 上海全宇生物科技遂平有限公司 Hair keratin composite fiber and spinning method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2475879A (en) * 1946-02-09 1949-07-12 Du Pont Process for the continuous spinning and stretching of zein filaments
CN1286325A (en) * 1999-09-01 2001-03-07 李官奇 Synthetic plant protein filaments
CN1524980A (en) * 2003-02-28 2004-09-01 李官奇 Synthetic fiber containing animal hair protein and manufacturing method thereof
CN1800455A (en) * 2005-01-06 2006-07-12 李官奇 Protein fiber spinning dope and its production method
CN1952225A (en) * 2006-04-28 2007-04-25 韩晓根 Maize protein colored textile fiber and method for producing same
CN102817101A (en) * 2012-07-31 2012-12-12 上海全宇生物科技遂平有限公司 Hair keratin composite fiber and spinning method thereof

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