CN1884641A - Method for preparing regenerated protein fiber using ion liquid dissolving animal hair - Google Patents
Method for preparing regenerated protein fiber using ion liquid dissolving animal hair Download PDFInfo
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Abstract
The invention discloses a biological protein wool fiber preparing method, which comprises the following steps: blending animal fur and fiber to produce soluble liquid at 90-120 deg.c in the ion liquid with positive and negative ion of fusing condition at 100 deg.c and positive ion to form salt; solidifying in the water, carbinol, alcohol, cyanoethyl or (NH4)2SO4 solution; adding adjuvant in the soluble liquid; solidifying in the water, carbinol, alcohol, cyanoethyl or 30 percent (NH4)2SO4 solution; evolving biological protein fur fiber.
Description
Technical field
The present invention relates to a kind of method for preparing spinning solution, particularly relate to a kind of method of using ion liquid dissolving animal hair to prepare regenerated protein.
Background technology
In human back to nature, today of advocating green, cleaner production, natural fabric and environmental protection textiles are subject to people's attention.Natural fabrics such as wool are distinctive to the affine health-care function of Human Physiology with it, make that this fibrid and regenerated protein thereof are paid close attention to by people always.Because the restriction of natural fabric resource, developing its reconstituted product becomes current hot issue.
China has the 4080000 wool spinning sand working ability of splitting at present, need about 350,000 tons clean hair raw materials every year, though homemade clean trichatrophia is combined into 12.74 ten thousand tons, but at most just 110,000 tons of the wools that actual purchase comes up, only account for 30% of demand, since the nineties, needed 230,000 tons of import wools every year on average,, calendar year 2001 in 2000 outer hair import volume about 300,000 tons, nearly about 340,000 tons of the quota amount of wool in 2002 and wool tops.The guiding price of purchasing fine hair to peasants and herdsmen in 2000 is: first-class (100 minutes) white goat wool per kilogram 240-320 unit.Wool purchase guiding price, thin one clean mao of per kilogram 25-28 unit; Change a clean hair and be 20-22 unit; The clean hair of high-quality soil species 10-12 unit.
Wool is the livestock products of China's supply demand gap maximum, needs ten thousand tons of clean hairs of 30-35 China's woolen industry year, and wherein domestic wool only can satisfy about 1/3,2/3 wool dependence on import.Ministry for Foreign Economic Relation and Trade of China's approval of import in this year wool index is 33.7 ten thousand tons, is worth 5,000,000,000 dollars, amounts to 40,000,000,000 yuan of RMB.
But because the restriction of hair quality, animal feeding management and textile technology, annual all have a large amount of staple fibres, crude fibre wool comforter to discard, and the wool leftover bits and pieces raw material number that the annual wool textile industry of China produces is in ten thousand tons.This has not only caused the waste of azelon resource, and contaminated environment.In addition, a large amount of poultry hair (as the pig hair) is because quality is thick and stiff, and fiber is short, can not be commonly used for fertilizer directly for weaving usefulness.Therefore the regeneration of the discarded animal fiber of research is to the effective utilization and the crucial meaning of having protected national resource.
Nineteen fifty once had the people to dissolve wool and spinning abroad in copper ammon solution, carbonyl diamide, caustic alkali or ammonia solution.Britain Coutaulds company claims with ferrous sulfate, hydrogen peroxide and acid (sulfuric acid, phosphoric acid and acetic acid) oxidation wool, dissolves its keratin again in weak aqua ammonia or aqueous caustic.Employing Peracetic acid such as Alexander are made oxidant, and wool is dissolved in caustic alkali, ammonium chloride and the carbonyl diamide solution.Japan has studied and extracted keratin from wool nineteen ninety-five, studies the membranization technology of keratin solution in 1996, begins to have established keratic regenerated fiber Study on Technology in 1997.
Find out that from above present existing method mainly is after animal wool is carried out oxidation or reduction, to interrupt peptide chain by caustic alkali or ammonia solution again, makes the hair dissolving.Treatment step is many, uses the reagent environmental pollution, and the PrPC molecular weight that makes is low.
Summary of the invention
Animal fiber such as the wool that the objective of the invention is to go out of use in the fabrication processes, cashmere, camel's hair, the rabbit hair, mohair, yak hair and can not be directly used in animal fiber inferior such as pig hair, the leather etc. of weaving processing, comprise shabby fuzz fabric, utilize that a kind of novel dissolvent---ionic liquid dissolves it, make lysate (azelon stoste).This lysate is 30% (NH4) in water, methyl alcohol, ethanol, second cyanogen or weight percent concentration
2SO
4Solidify in the solution, separate out the animal wool regenerated protein; Perhaps in lysate, add the protein fibre that auxiliary agent is spun into various models.Especially keratin protein is abundant in the animal wool, the cystine height, thus excellent with fibre strength height, good luster, good springiness, the dyeing of this protein synthesis, and process regeneration spinning can spin the short silk and the long filament of various fiber numbers, improve quality, widened the purposes of animal fiber.
Technical scheme of the present invention is as follows:
Use ion liquid dissolving animal hair provided by the invention prepares the method for regenerated protein, and its step is as follows:
1) will through clean, air-dry or being lower than 80 ℃ of animal wool raw materials of oven dry down, directly or through after the preliminary treatment mix with ionic liquid, under 90-120 ℃, dissolve lysate, i.e. azelon stoste;
The weight portion proportioning of described animal wool raw material and ionic liquid is 1: 5～20;
Described ionic liquid is the salt by zwitterion and cation composition that is molten condition under 100 ℃, and described anion is halide ion Cl-, Br-, I-or acetate ion; CATION is N-N-methylimidazole CATION, 1-ethyl, 3-methylimidazole CATION, 1-allyl, 3-methylimidazole CATION, 1-allyl, 3-methylimidazole CATION or 1-butyl, 3-methylimidazole CATION or 1-methyl-3-butyl imidazole CATION;
2) with step 1) gained lysate (azelon stoste) be 30% (NH4) then in water, methyl alcohol, ethanol, second cyanogen or weight percent concentration
2SO
4Solidify in the solution, just separate out the animal wool regenerated protein;
Perhaps, adding accounts for the glycerine of lysate volume 0.1-1.0% or/and the isopropyl alcohol auxiliary agent makes the mixed liquor that contains auxiliary agent in the step 1) lysate; And then the mixed liquor that the step 3) gained is contained auxiliary agent is 30% (NH4) in water, methyl alcohol, ethanol, second cyanogen or weight percent concentration
2SO
4Carry out coagulating bath in the solution, just separate out the animal wool regenerated protein.
Described raw material is wool, felt, camel hair, camel hair suede, the rabbit hair or animal fiber pig hair inferior, the leather that goes out of use in the fabrication processes.
The preliminary treatment of the animal wool raw material in the described step 1) is: it is 10-50% urea, 2-6%SDS and 2-6%NaHSO that the animal wool raw material is immersed in weight percent concentration
3Mixed solution in, carry out immersion treatment 0.5-2h under 50-100 ℃.
Described step 1) ionic liquid and animal wool raw material all need pass through dried before mixing.
Be dissolved as heating for dissolving in the described step 1), its mode of heating is oil bath heating, baking oven for heating or electric furnace heating; Carrying out batch (-type) in the heating process stirs; Accumulation heat time heating time is 0.5-16h.
The method that use ion liquid dissolving animal hair of the present invention prepares regenerated protein has following advantage:
(1) can make full use of discarded animal wool or woolen knitwear the like waste, raw material is easy to get, and is inexpensive, and can reduce the discarded object pollution on the environment;
(2) step of the present invention is easy, and is easy to operate.
The specific embodiment
Below by embodiment the present invention is further specified.
Embodiment 1
1) will directly mix, but on the electric furnace of temperature adjustment, heat while stirring through the raw wool of cleaning, natural airing, carry out heating for dissolving and got amber lysate in 60 minutes with ionic liquid;
The solid-liquid ratio of the weight of described raw wool and ionic liquid volume is 1: 20;
Described ionic liquid is the 1-butyl by zwitterion and cation composition that is molten condition under 100 ℃, the ionic liquid of 3 methylimidazole chlorates;
2) lysate of step 1) gained is clamp-oned carried out coagulating bath in the water then, just separate out the animal wool regenerated protein.
Embodiment 2
To carry out preliminary treatment through the camel hair raw material after cleaning: promptly, be 20% urea, 3%SDS and 3%NaHSO in weight percent concentration with the camel hair raw material
3Mixed solution in, carry out immersion treatment 0.5h under 100 ℃; Its pretreated feed liquid weight part ratio is 1: 10;
To mix with ionic liquid through pretreated camel hair raw material, and under 100 ℃, heat (heat in the constant temperature oven, and stir frequently) dissolving 12h and get amber lysate; The solid-liquid ratio of described camel hair raw material weight and ionic liquid volume is 1: 2;
Described ionic liquid is the 1-butyl by zwitterion and cation composition that is molten condition under 100 ℃, 3-methylimidazole Bromide;
In above-mentioned lysate, add the glycerine that accounts for lysate volume 0.1%, then this glycerinated mixed liquor is poured in the methyl alcohol, promptly obtain the cotton-shaped regenerated protein of sheet.
Embodiment 3
To carry out preliminary treatment through the rabbit hair raw material after cleaning: promptly, be 20% urea, 3%SDS and 3%NaHSO in weight percent concentration with rabbit hair raw material
3Mixed solution in, carry out immersion treatment 1.0h under 70 ℃; Its pretreated feed liquid weight part ratio is 1: 10;
To mix with ionic liquid through pretreated rabbit hair raw material, and heat under 110 ℃ of oil baths, and stir frequently, dissolving 6h gets amber lysate; The solid-liquid ratio of described rabbit hair raw material weight and ionic liquid volume is 1: 5;
Described ionic liquid is the 1-allyl by zwitterion and the cation composition-3-methyl imidazolium chloride salt that is molten condition under 100 ℃;
In above-mentioned lysate, add the glycerine that accounts for lysate volume 1.0%, then this glycerinated mixed liquor is poured in the second cyanogen, promptly obtain the cotton-shaped regenerated protein of sheet.
Embodiment 4
To carry out preliminary treatment through the yak hair raw material after cleaning: promptly, be 50% urea, 3%SDS and 3%NaHSO in weight percent concentration with the yak hair raw material
3Mixed solution in, carry out immersion treatment 1.0h under 70 ℃; Its pretreated feed liquid weight part ratio is 1: 30;
To mix with ionic liquid through pretreated yak hair raw material, and heat under 110 ℃ of oil baths, and stir frequently, dissolving 6h gets amber lysate; The solid-liquid ratio of described yak hair raw material weight and ionic liquid volume is 1: 10;
Described ionic liquid is the 1-allyl by zwitterion and the cation composition-3-methyl imidazolium chloride salt that is molten condition under 100 ℃;
Add the isopropyl alcohol that accounts for lysate volume 1.0% in above-mentioned lysate, the mixed liquor that then this is contained isopropyl alcohol is poured in the second cyanogen, promptly obtains the cotton-shaped regenerated protein of sheet.
Embodiment 5
To carry out preliminary treatment through the raw wool after cleaning: promptly, be 20% urea, 3%SDS and 3%NaHSO in weight percent concentration with raw wool
3Mixed solution in, carry out immersion treatment 1.0h under 70 ℃; Its pretreated feed liquid weight part ratio is 1: 30;
To mix with ionic liquid through pretreated raw wool, and heat under 100 ℃ of oil baths, and stir frequently, dissolving 16h gets amber lysate; The solid-liquid ratio of described raw wool weight and ionic liquid volume is 1: 5;
Described ionic liquid is the 1-methyl by zwitterion and the cation composition-3-methyl iodate imidazole salts that is molten condition under 100 ℃;
In above-mentioned lysate, add the isopropyl alcohol that accounts for lysate volume 0.3%, then solution is poured in the water, promptly obtain the cotton-shaped regenerated protein of sheet.
Embodiment 6
To carry out preliminary treatment through the raw wool after cleaning: promptly, be 30% urea, 3%SDS and 3%NaHSO in weight percent concentration with raw wool
3Mixed solution in, carry out immersion treatment 1.0h under 70 ℃; Its pretreated feed liquid weight part ratio is 1: 10;
To mix with ionic liquid through pretreated raw wool, and heat under 100 ℃ of oil baths, and stir frequently, dissolving 6h gets amber lysate; The solid-liquid ratio of described raw wool weight and ionic liquid volume is 1: 15;
Described ionic liquid is the 1-methyl by zwitterion and the cation composition-3-methyl imidazolium chloride salt that is molten condition under 100 ℃;
Pour above-mentioned gained solution into 30% (NH4) then
2SO
4In the water, promptly obtain the cotton-shaped regenerated protein of sheet.
Embodiment 7
1) will directly mix, but on the electric furnace of temperature adjustment, heat while stirring through the raw wool of cleaning, natural airing, carry out heating for dissolving and got amber lysate in 60 minutes with ionic liquid;
The solid-liquid ratio of the weight of described raw wool and ionic liquid volume is 1: 10;
Described ionic liquid is the ionic liquid of the 1-butyl by zwitterion and cation composition-3-methylimidazole acetate of being molten condition under 100 ℃;
2) lysate of step 1) gained is clamp-oned carried out coagulating bath in the water then, just separate out the animal wool regenerated protein.
Claims (5)
1, a kind of method of using ion liquid dissolving animal hair to prepare regenerated protein, its step is as follows:
1) will through clean, air-dry or being lower than 80 ℃ of animal wool raw materials of oven dry down, directly or through after the preliminary treatment mix with ionic liquid, under 90-120 ℃, dissolve lysate;
Described animal wool raw material and ionic liquid weight portion proportioning are 1: 5～20;
Described ionic liquid is the salt by zwitterion and cation composition that is molten condition under 100 ℃, and described anion is halide ion Cl-, Br-, I-or acetate ion; CATION is N-N-methylimidazole CATION, 1-ethyl, 3-methylimidazole CATION, 1-allyl, 3-methylimidazole CATION, 1-allyl, 3-methylimidazole CATION or 1-butyl, 3-methylimidazole CATION or 1-methyl-3-butyl imidazole CATION;
2) with step 1) gained lysate be 30% (NH4) then in water, methyl alcohol, ethanol, second cyanogen or weight percent concentration
2Solidify in the SO4 solution, separate out the animal wool regenerated protein;
Perhaps, adding accounts for the glycerine of lysate volume 0.1-1.0% or/and the isopropyl alcohol auxiliary agent makes the mixed liquor that contains auxiliary agent in the step 1) lysate; And then the mixed liquor that the step 3) gained is contained auxiliary agent is 30% (NH4) in water, methyl alcohol, ethanol, second cyanogen or weight percent concentration
2Solidify in the SO4 solution, separate out the animal wool regenerated protein.
2, the method for preparing regenerated protein by the described use ion liquid dissolving animal hair of claim 1, it is characterized in that described raw material is wool, felt, camel hair, camel hair suede, the rabbit hair or animal fiber pig hair inferior, the leather that goes out of use in the fabrication processes.
3, the method for preparing regenerated protein by the described use ion liquid dissolving animal hair of claim 1, it is characterized in that the preliminary treatment of the animal wool raw material in the described step 1) is: it is 10-50% urea, 2-6%SDS and 2-6%NaHSO that the animal wool raw material is immersed in weight percent concentration
3Mixed solution in, carry out immersion treatment 0.5-2h under 50-100 ℃.
4, prepare the method for regenerated protein by the described use ion liquid dissolving animal hair of claim 1, it is characterized in that, described step 1) ionic liquid and animal wool raw material all pass through dried before mixing.
5, prepare the method for regenerated protein by the described use ion liquid dissolving animal hair of claim 1, it is characterized in that, be dissolved as heating for dissolving in the described step 1), the mode of heating of heating for dissolving is oil bath heating, baking oven for heating or electric furnace heating; Carrying out batch (-type) in the heating process stirs; Accumulation heat time heating time is 0.5-16h.
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| CN101092445B (en) * | 2007-06-13 | 2011-09-14 | 哈尔滨工程大学 | Method for crystallizing protein by using ion liquid |
| CN102277754A (en) * | 2011-06-28 | 2011-12-14 | 湖南工程学院 | Method of wool surface modification and low temperature dyeing |
| CN102534864A (en) * | 2011-11-19 | 2012-07-04 | 青岛科技大学 | Preparation method of alkylation chitosan fiber |
| CN103102694A (en) * | 2013-03-07 | 2013-05-15 | 河南鼎大生物科技有限公司 | Method for preparation and wet spinning of regenerative keratin and silk-fibroin blended solution |
| CN103102695A (en) * | 2013-03-07 | 2013-05-15 | 河南鼎大生物科技有限公司 | Method for preparation and wet spinning of regenerative keratin solution |
| CN103710775A (en) * | 2013-12-18 | 2014-04-09 | 中国科学院过程工程研究所 | Preparation method of ionic liquid keratin spinning solutions |
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| CN103710775B (en) * | 2013-12-18 | 2016-02-24 | 中国科学院过程工程研究所 | A kind of preparation method of ionic liquid keratin spinning solution |
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| CN108404875A (en) * | 2018-03-28 | 2018-08-17 | 齐鲁工业大学 | A kind of preparation method of ox hair protein sponge sorbing material for tanning dyeing waste liquid |
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| CN112898403A (en) * | 2021-04-23 | 2021-06-04 | 郑州中科新兴产业技术研究院 | Method for extracting keratin |
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| CN114318865B (en) * | 2021-12-30 | 2022-12-27 | 江南大学 | Wool pretreatment liquid and application thereof |
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