CN1435516A - Technique for processing regenerated keratin functional fibre - Google Patents
Technique for processing regenerated keratin functional fibre Download PDFInfo
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- CN1435516A CN1435516A CN 02155407 CN02155407A CN1435516A CN 1435516 A CN1435516 A CN 1435516A CN 02155407 CN02155407 CN 02155407 CN 02155407 A CN02155407 A CN 02155407A CN 1435516 A CN1435516 A CN 1435516A
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Abstract
A functional fibre of regenerated ceratin is prepared through preparing ceratin solution from goat or sheep wool, camel or yak hair, feather, leather leftover, etc, adding one or more of metal oxide, organic metal compound, chitin, chitosan, cyclodextrin, polyether and polyacrylic acid, which have the antistatic, antibacterial, deodorizing, drying, heating lagging and hydroscopc functions, and spinning.
Description
Technical field
The invention belongs to a kind of regeneration keratin merit fiber process technology of macromolecular material and engineering Application Areas.
Background technology
With macromolecular material manufacturing chemistry fiber is generally current in the world way, utilizes the various textiless of artificial fibre processing the present age, also is seen everywhere on market.In recent years, utilize milk fibre, the fibre and soya of albumen processing also to begin to take shape.The present invention produces from natural keratin raw material resource to have functional keratin protein regenerated fiber.At present, domestic existing alkaline method is produced the keratin fiber technology.By retrieval, immediate with the present invention be " technology of regenerating ceratin fibres " (number of patent application: 99116699, publication number: 1293266), this invention is the manufacture method of extracting albumen and be processed as the protein renaturation fiber from the keratin raw material.This patent main technique flow process is: the crosslinked → sealing free amine group → albumen spinning solution → spinning → protein renaturation fiber of raw material → degreasing impurity elimination → dissolving → protein.It is characterized in that with various keratin such as various animal wools (comprising toe feathering under the woollen mill, pig hair, chicken and duck hair, ox hair etc.), useless silk, waste leathers as the azelon raw material; To the dissolution mechanism of keratin fibers such as wool adopt the dissolving of alkalescence (NaOH) solution and adopt go back the oxygen chloropropane, formaldehyde is made crosslinking agent.But not only molecular weight is low for the polypeptide that is obtained, row yielding is low, and all has low, process crosslinked afterwards protein sex change, the more high defective of industrialization cost of keratin protein content in the fiber.
Summary of the invention
In China, above-mentioned listed keratin protein resource extent is considerable, yet for a long time owing to the limitation of technology, this resource is not fully used.These are toe feathering or because average fiber length is short, the discrete length degree is big down, or can not be used as waste product and handle directly for the weaving use because quality is thick and stiff, fiber is short.If therefore these raw materials are fully used, be transformed into the functional regeneration keratin protein fiber of difference in functionalitys such as having antibacterial and deodouring, antistatic, will bring benefit to the mankind, and, promote the development of new fiber for China's fiber industry increases the novel functional fiber of a class.At existing technical deficiency in the aforementioned background art, the keratin protein functional fibre that the present invention produces contains a high proportion of keratin protein, not only have some good characteristics of natural cashmere fiber, wool fibre, and have antibacterial deodourizing, different multiple function such as antistatic again.
Meaning of the present invention is: the present invention is devoted to making full use of of leftover bits and pieces raw material that national annual number produces in ten thousand tons wool industry, a large amount of thick and stiff keratin protein raw material that animal husbandry forms, and keratin protein functional fibre function, that have independent intellectual property right such as obtain having antibacterial and deodouring, antistatic, for making the novel functional regeneration keratin protein fiber of a class, China man-made fibres industry provides key technology.The present invention adopts acid process dissolving keratin protein raw material and is prepared into solution that (number of patent application: 02155362.9), this solution has keratin protein content height, characteristics that row yielding is high; Contain a high proportion of keratin protein in the keratin protein functional fibre; The fiber applications characteristics not only show some good characteristics of wool, cashmere fiber, have simultaneously antibacterial deodourizing, antistatic etc. all multi-functional again.The shortage of goat cashmere resource and the contradiction of the market demand can be alleviated and remedy to the invention of keratin protein functional fibre and through engineering approaches and Industry Promotion, can promote to have the development of the tencel industry of China's independent intellectual property right again.
The present invention is a kind of manufacturing technology of the keratin functional fibre of regenerating, it is characterized in that: with goats hair, camel hair, yak hair, the pig hair, the wool and the scurf of animal coarse wool such as chicken and duck feather and on-woven value, waste leather, animal coffin isogonism protein material is a raw material, select the dissolution process of effective solvent and original creation, obtain being suitable for the keratin solution (application number: 02155362.9) of spinning, selection is by having antibacterial and deodouring, antistatic, dry sensation, the heat lag performance, the metal oxide of functions such as high-hygroscopicity, organo-metallic compound, chitin, shitosan, cyclodextrin, polyethers, the nanoscale function dispersion liquid that polyacrylic acid etc. prepare, join in the keratin solution that is suitable for spinning, produce by wet spinning or dry-wet spinning and have antibacterial and deodouring, antistatic, dry sensation, the heat lag performance, the regeneration keratin functional fibre of function combination high-hygroscopicity or the like difference in functionality or multiple; Its main technique flow process is: keratin solution → blended polymer → filtration → stable → deaeration → injection is sneaked into functional dispersion liquid → spinning → coagulating bath → as-spun fibre → stretching → curling → drying → cut-out → oven dry → regeneration keratin functional fibre → finished product; The perhaps functional dispersion liquid of keratin solution → blended polymer → blend → filtration → stable → deaeration → spinning → coagulating bath → as-spun fibre → stretching → curl → drying → cut-out → oven dry → regeneration keratin functional fibre → finished product.
Below critical process of the present invention is described in further detail:
(1), the preparation of blended polymer solution:
1, produce keratin protein solution: some kilograms, standby.
2, preparation solvent system: (20-35%) water of the calcium chloride of zinc chloride+(0-20%)+(80-45%).
3, preparation blended polymer solution: polyacrylonitrile, polyvinyl alcohol etc. are added in the above-mentioned solvent system, under following listed condition, dissolve; Add standby keratin protein solution and mix, form blended polymer solution.
(1) polyacrylonitrile blended thing dissolving (copolymer or homopolymers):
Polyacrylonitrile 10-18%
Solution temperature 40-80 ℃
Time 2-3 hour
(2) dissolving of polyvinyl alcohol blend:
Polyvinyl alcohol 10-20%
Solution temperature 40-80 ℃
Time 2-3 hour
(2) preparation of chitin and shitosan dispersion liquid: chitin, shitosan and cyclodextrin can directly be dissolved in as in (one) described solvent system.
Chitin or shitosan or cyclodextrin 10-30%
Temperature 40-80 ℃
Time 1-2 hour
(3) preparation of polyethers solution: polyethers can directly be dissolved in as in (one) described solvent system.
Polyethers 20-40%
Temperature 40-60 ℃
Time 1-2 hour
(4) preparation of functional dispersion liquid
Functional metal oxide is fully disperseing to obtain functional dispersion liquid by ball mill under the effect of surfactants such as Dispersant MF, NNO in the solvent system described in ().
Metal oxide 1-15%
The consumption of Dispersant MF, NNO and surfactant is functional metal oxide 0.5%-3%
Temperature 30-40
Time 30-50 hour
(5) wet spinning and post processing: mix by top (one) resulting blended polymer solution or with the function solution that makes among (two), (three), (four), obtain as-spun fibre through spinning machine wet method or dry-wet spinning; Perhaps inject that function solution that (two), (three), (four) make carries out wet method or dry-wet spinning obtains as-spun fibre before spinning on the spinning machine of injection device having, then, drawn, washing, oven dry obtain finished fiber again.
1, spinning condition:
Concentration of dope 10-20%
50-80 ℃ of spinning solution temperature
Coagulation bath composition 0-30% aqueous sodium persulfate solution
Coagulation bath temperature 20-30 ℃
Spinning speed 20-60 rice/minute
2, stretching and post-treatment condition:
Stretch bath is formed: 0-2% hydrogen peroxide or peracetic acid
90-95 ℃ of stretch bath temperature
Draw ratio 1.8-2.5 doubly
Washing temperature 40-50 ℃
Bake out temperature 110-120 ℃
The specific embodiment
[embodiment 1] this example can obtain a kind of antibacterial and antimildew function fiber.
Operate according to the following steps:
1, it is standby to get goats hair keratin protein solution 120g.
2, preparation solvent: with molecular weight is 5.6 ten thousand polyacrylonitrile (20g) at 35% zinc chloride, 20% calcium chloride, 45%H
2In 80 ℃ of stirring dissolvings fully in 2 hours down, make solution in the solvent that O formed (200g).
3, preparation chitosan solution: be 200,000 shitosan (3g) with molecular weight at 35% zinc chloride, 20% calcium chloride, 45%H
2In the aqueous solution that O formed (30g), under 80 ℃ of temperature, stirred 2 hours, obtain chitosan solution.
4, preparation spinning solution: above-mentioned three kinds of solution stirring are mixed, placed 2 hours down at 60 ℃, and vacuumizing and defoaming 2 hours, obtain spinning solution, wait for the spinning use.
5, adopt the dry wet spinning machine spinning.
Spinneret orifice hole count 50
60 ℃ of spinning solution temperature
Coagulation bath composition 25% aqueous sodium persulfate solution
30 ℃ of coagulation bath temperatures
40 meters/minute of spinning speeds
Stretch bath is formed 1% hydrogen peroxide
Temperature 90-95 ℃ of stretch bath (water)
Draw ratio 2
50 ℃ of washing temperature
120 ℃ of bake out temperatures.
[embodiment 2] this example can obtain the anti-static function fiber.
Operate according to the following steps
1, with goats hair keratin protein solution 120g
2, with molecular weight 5.6 ten thousand polyacrylonitrile (20g) at 35% zinc chloride, 20% chlorination, 45%H
2Stir dissolving fully in 2 hours down in 80 ℃ in the aqueous solution that O formed (200g).
3, functional metal oxide (the antistatic powder of FUMAT-A600) 4g with 1% Dispersant MF under 40 ℃ by ball mill at 35% zinc chloride, 20% calcium chloride, 45%H
2Fully disperse in the solution that O formed (40g) to obtain functional dispersion liquid in 40 hours, wait to spin preceding injection.
4, keratin protein solution and polyacrylonitrile solution are mixed, placed 2 hours down, and vacuumizing and defoaming 2 hours, obtain spinning solution, wait for that spinning uses at 60 ℃.
5, adopt the dry wet spinning machine spinning, and by injection device function of injecting dispersion liquid before spinning.
Spinneret orifice hole count 50
60 ℃ of spinning solution temperature
Coagulation bath composition 25% aqueous sodium persulfate solution
30 ℃ of coagulation bath temperatures
40 meters/minute of spinning speeds
Stretch bath is formed 1% hydrogen peroxide
90～95 ℃ of stretch bath (water) temperature
Draw ratio 2
50 ℃ of washing temperature
120 ℃ of bake out temperatures.
[embodiment 3] this example can obtain deodorizing keratin functional fibre
Operate according to the following steps:
1, it is standby to get goats hair keratin protein solution 150g.
2, preparation solvent: with molecular weight is 5.6 ten thousand polyacrylonitrile homopolymers (30g) at 35% zinc chloride, 20% calcium chloride, 45%H
2In 80 ℃ of stirring dissolvings fully in 2 hours down, make solution in the solvent that O formed (200g).
3, preparation cyclodextrin solution: cyclodextrin (5g) is at 35% zinc chloride, 20% calcium chloride, 45%H
2In the aqueous solution that O formed (30g), under 50 ℃ of temperature, stirred 2 hours, obtain cyclodextrin solution.
4, preparation spinning solution: above-mentioned three kinds of solution stirring are mixed, placed 2 hours down at 60 ℃, and vacuumizing and defoaming 2 hours, obtain spinning solution, wait for the spinning use.
5, adopt the dry wet spinning machine spinning.
Spinneret orifice hole count 30
60 ℃ of spinning solution temperature
Coagulation bath composition 25% aqueous sodium persulfate solution
25 ℃ of coagulation bath temperatures
40 meters/minute of spinning speeds
Stretch bath is formed 1% hydrogen peroxide
90～95 ℃ of stretch bath (water) temperature
Draw ratio 2
50 ℃ of washing temperature
110 ℃ of bake out temperatures.
[embodiment 4] this example can obtain far infrared keratin functional fibre
Operate according to the following steps
1, with goats hair keratin protein solution 120g
2, with polyvinyl alcohol (20g) at 35% zinc chloride, 20% calcium chloride, 45%H
2Stir dissolving fully in 2 hours down in 80 ℃ in the aqueous solution that O formed (200g).
3, functional metal oxide titanium dioxide 5g fully disperseing to obtain functional dispersion liquid in 40 hours by ball mill under 40 ℃, waits to spin preceding injection with 1% Dispersant MF in the solution of the above-mentioned polyvinyl alcohol of 50g.
4, keratin protein solution and remaining poly-vinyl alcohol solution are mixed, placed 2 hours down, and vacuumizing and defoaming 2 hours, obtain spinning solution, wait for that spinning uses at 60 ℃.
5, adopt the dry wet spinning machine spinning, and inject the poly-vinyl alcohol solution of titanium dioxide by injection device before spinning.
Spinneret orifice hole count 30
60 ℃ of spinning solution temperature
Coagulation bath composition 25% aqueous sodium persulfate solution
30 ℃ of coagulation bath temperatures
40 meters/minute of spinning speeds
Stretch bath is formed 1% hydrogen peroxide
90～95 ℃ of stretch bath (water) temperature
Draw ratio 2
50 ℃ of washing temperature
110 ℃ of bake out temperatures.
[embodiment 5] this example can obtain heat lag keratin functional fibre
Operate according to the following steps
1, with goats hair keratin protein solution 500g
2, with polyvinyl alcohol (100g) at 35% zinc chloride, 20% calcium chloride, 45%H
2Stir dissolving fully in 2 hours down in 80 ℃ in the aqueous solution that O formed (800g).
3, with polyvinyl alcohol (5g), zinc chloride, 20% chlorination, the 45%H of polyethylene glycol (molecular weight 10000,20g) 35%
2In 60 ℃ of stirring dissolvings fully in 2 hours down, wait to spin preceding injection in the aqueous solution that O formed (100g).
4, keratin protein solution and poly-vinyl alcohol solution are mixed, placed 2 hours down, and vacuumizing and defoaming 2 hours, obtain spinning solution, wait for that spinning uses at 60 ℃.
5, adopt the dry wet spinning machine spinning, and inject polyvinyl alcohol and polyethylene glycol blending solution by injection device before spinning.
Spinneret orifice hole count 30
60 ℃ of spinning solution temperature
Coagulation bath composition 25% aqueous sodium persulfate solution
30 ℃ of coagulation bath temperatures
40 meters/minute of spinning speeds
Stretch bath is formed 1% hydrogen peroxide
90～95 ℃ of stretch bath (water) temperature
Draw ratio 2
50 ℃ of washing temperature
100 ℃ of bake out temperatures.
Claims (12)
1. process technology of keratin functional fibre of regenerating, it is characterized in that, with the wool of animal coarse wool, feather and on-woven values such as goats hair, camel hair, yak hair, pig hair, chicken and duck feather and scurf, waste leather, animal coffin isogonism protein material is raw material, select the dissolution process of effective solvent and original creation, obtain being suitable for the keratin solution (number of patent application: 02155362.9) of spinning; In being suitable for the keratin solution of spinning, add by having antibacterial and deodouring, antistatic, dry sensation, heat lag, the metal oxide of difference in functionalitys such as high-hygroscopicity, organo-metallic compound, chitin, shitosan, cyclodextrin, polyethers, the nanoscale function dispersion liquid that polyacrylic acid etc. prepare, produce by wet spinning or dry-wet spinning and to have antibacterial and deodouring, antistatic, dry sensation, the heat lag performance, the regeneration keratin functional fibre of difference in functionality such as high-hygroscopicity or the combination of multiple function, its main technique flow process is: keratin solution → blended polymer → filtrations → stable → deaeration → injection is sneaked into functional dispersion liquid → spinning → coagulating bath → as-spun fibre → stretching → curling → drying → cut-out → oven dry → regeneration keratin functional fibre → finished product; The perhaps functional dispersion liquid of keratin solution → blended polymer → blend → filtration → stable → deaeration → spinning → coagulating bath → as-spun fibre → stretching → curl → drying → cut-out → oven dry → regeneration keratin functional fibre → finished product.
2. the process technology of a kind of keratin functional fibre of regenerating according to claim 1, it is characterized in that, the solvent system of spinning solution is a metal salt solution, can select one or both slaines wherein such as zinc chloride, calcium chloride, thiocyanic acid are received, lithium bromide for use, and make certain density solvent system after altogether molten with water.
3. according to the process technology of the described a kind of keratin functional fibre of regenerating of claim 1-2, it is characterized in that, preparation blended polymer solution, polyacrylonitrile, polyvinyl alcohol etc. are added in the above-mentioned solvent system, dissolving under certain conditions, add standby keratin protein solution then and mix, form blended polymer solution.
4. the process technology of a kind of keratin functional fibre of regenerating according to claim 1, it is characterized in that, the nanoscale function dispersion liquid that selection is prepared by the metal oxide with difference in functionalitys such as antibacterial and deodouring, antistatic, dry sensation, heat lag performance, high-hygroscopicities, organo-metallic compound, chitin, shitosan, cyclodextrin, selection polyethers, polyacrylic acid etc., its functional metal oxide can be selected titanium dioxide, zirconia, zinc oxide, calcium oxide etc. for use.
5. according to the process technology of the described a kind of keratin functional fibre of regenerating of claim 1-4, it is characterized in that, the typical constituent of fiber is keratin protein (45-75%), blended polymer (50-20%), metal oxide (1-5%) or chitin or shitosan or cyclodextrin (1-5%).
6. according to the process technology of the described a kind of keratin functional fibre of regenerating of claim 1-5, it is characterized in that its typical functions is presented as one or more functions such as antistatic, dry sensation, cooling feeling, far infrared by selecting metal oxide (1-5%) for use.
7. according to the described keratin regenerating functional of claim 1-5 fibre manufacturing technology, it is characterized in that it is functional by selecting for use chitin, shitosan, cyclodextrin etc. to embody one or more functions such as antibiotic, moisture absorption, deodorization, health care.
8. according to the process technology of the described a kind of keratin functional fibre of regenerating of claim 1-5, it is characterized in that it is functional by selecting for use polyethers etc. to embody heat lag, high-hygroscopicity or the like one or more functions.
9. the process technology of a kind of keratin functional fibre of regenerating according to claim 1, it is characterized in that, prepare functional metal oxide dispersion liquid, its manufacture method be functional metal oxide under the effect of surfactants such as Dispersant MF, NNO, make it in solvent system of the present invention, fully disperse to obtain functional dispersion liquid by ball mill.
10. the process technology of a kind of keratin functional fibre of regenerating according to claim 1, it is characterized in that, functional dispersion liquid by blend or before spinning injection sneak into spinning solution, and make the as-spun fibre of keratin protein functional fibre by wet method or dry-wet spinning.
11. the process technology of a kind of keratin functional fibre of regenerating according to claim 1 is characterized in that, the aqueous solution of its coagulating bath selection water or slaine such as sodium chloride, sodium sulphate.
12. the process technology of a kind of keratin functional fibre of regenerating according to claim 1 is characterized in that hydrogen peroxide, peracetic acid etc. are a kind of aqueous solution of peroxide wherein.
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| CN115151235A (en) * | 2020-01-21 | 2022-10-04 | 纽泰克温图斯公司 | Continuous production of keratin fibers |
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2002
- 2002-12-12 CN CN 02155407 patent/CN1435516A/en active Pending
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