CN104005114A - Preparation method for wool keratin regenerated cellulose fiber - Google Patents
Preparation method for wool keratin regenerated cellulose fiber Download PDFInfo
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- CN104005114A CN104005114A CN201410186804.5A CN201410186804A CN104005114A CN 104005114 A CN104005114 A CN 104005114A CN 201410186804 A CN201410186804 A CN 201410186804A CN 104005114 A CN104005114 A CN 104005114A
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Abstract
A provided preparation method for wool keratin regenerated cellulose fiber comprises the concrete steps: firstly preparing a viscose-rayon spinning solution, then preparing a wool keratin solution, then mixing the viscose-rayon spinning solution and the wool keratin solution, then adding a crosslinking agent, mixing and performing wet-process spinning, so as to obtain wool keratin regenerated cellulose fiber. The wool keratin regenerated cellulose fiber prepared by employing the method has the protein content of 6% or more, and the production technology is simple in process and high in production efficiency.
Description
Technical field
The invention belongs to weaving production technical field, be specifically related to a kind of preparation method of wool keratin regenerated celulose fibre.
Background technology
Natural keratin is extensively present in nature, source is abundant, and the keratin raw material of the annual nearly hundreds of thousands ton of China (as hair, feather, scale etc.) go out of use, a large amount of keratic discarded serious waste that not only cause resource, also can work the mischief to ecological environment.Therefore, keratin is recycled, not only can protection of the environment, can also obtain good economic benefit.Natural keratin itself has the performance of many excellences, as good mechanical performance, the chemical property that is better than synthetic material, good biodegradability and compatibility etc., make it in many mechanics of biological tissue, play basic supporting role, this is also people's required key propertys that have when using various regrown material.Therefore, keratin is made to new and high technology and product, there is potential using value, can be widely used in the fields such as food, biology, medical treatment, environmental protection, agricultural.
In recent years, wool keratin and regenerated fiber blend fibroblast become the focus of research.On the one hand, waste wool and other animal hairs dissolved to recycling and be spun into fiber with cellulose solution blend, can economize on resources, improving the value of discarded hair; On the other hand, develop tencel and meet the user demand of modern to fabric, therefore there is good researching value.
The at present research of keratin and viscose glue blending fiber is more, but be mostly keratin and viscose glue in conjunction with aspect variant.Common are and take ionic liquid method that the method for keratin and cellulose blending is prepared to blended liquid and solution; Take to add the method for initator to make keratin and cellulose generation graft reaction.In addition taking in addition to add the method for crosslinking agent is cross-linking reaction to occur between keratin and cellulose prepare wool keratin and cellulose blending fibre.But because prepared keratin solution molecular weight is lower, less with cellulosic adhesion, make the fixation rate of albumen on fiber on the low side, thereby the protein content in prepared regenerating ceratin fibres cellulose fiber is lower, cannot reaches the Expected Results of regenerating ceratin fibres cellulose fiber.The dissolving of the Master's thesis < < waste wool of the Zhang Meng of Donghua University and with the research > > of cellulose blending in propose a kind of utilize ion liquid dissolving wool produce keratin solution and with viscose glue blending after carry out spinning method, this method has environment friendly and pollution-free feature, but ionic liquid is expensive, reach 8000 yuan/Kg, cannot apply on a large scale.In the Master's thesis < < keratin protein of the Li Minghua of University Of Qingdao and the research > > of prezenta graft copolymerization fibroblast and performance thereof, adopt alkaline process to dissolve wool and produce keratin solution, this method technique is simple, but the keratin solution yield obtaining is lower, lower than 80%, molecular weight of albumen is lower, and on the fiber that causes making, protein content is lower.Institutes Of Technology Of Zhejiang pays in the preparation and property research > > that learns loyal master thesis < < cellulose and keratin composite and proposes to take reducing process to prepare keratin solution also and cellulose blending, in the made protein solution of this method, molecular weight of albumen is relatively high, but albumen productive rate is also relatively low, and reaction condition is gentle, consuming time longer, affect production efficiency.
Generally, the disulfide bond in keratin molecule makes to occur between peptide chain inside and peptide chain crosslinked, forms space network, makes natural keratin hard degradation, brings difficulty to keratic extraction in hair.Common solvent or the gentle soda acid keratin in all can not dissolve hair fiber, more intense soda acid energy dissolve hair albumen, can be between saboteur peptide chain be ruptured in active force and keratin two, tertiary structure, the product obtaining is the albumen of molecular weight often, or even polypeptide, and productive rate is on the low side.Make that molecular weight is higher, the good keratin of dissolubility, can only be by opened disulfide bond optionally, destroy the methods such as hydrogen bond and realize.
Extract at present keratic method and roughly have Mechanical Method, chemical method and bioanalysis etc.But these methods have the shortcomings such as albumen yield is lower, and molecular weight of albumen is less than normal, complex process more, not only can cause the wasting of resources, also can have influence on the indexs such as protein content final in fiber and fiber strength simultaneously.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of wool keratin regenerated celulose fibre, in the wool keratin regenerated celulose fibre that the present invention prepares, protein content can reach more than 6%, and the technological process of production is simple, and production efficiency is high.
A preparation method for wool keratin regenerated celulose fibre, comprises the following steps:
Step 1, Making viscose spinning solution;
Step 2, prepares wool keratin solution: with distilled water preparation wool protein powder solution, to adding sulphur in solution, be then reductant, after stirring, add again keratinase, pH value of solution is adjusted to 7.5～8.0, is warming up to 50～60 ℃, after insulation, filtration obtains keratin solution;
Step 3, mixes step 1 gained rayon spinning stoste and step 2 gained keratin solution, then adds crosslinking agent, carries out wet spinning after mixing.
As foregoing invention further preferably, in described step 2, the crude protein content of wool protein powder used is greater than 80%.
As foregoing invention further preferably, in described step 2, the wool protein powder liquid quality fraction of preparation is 8～12%.
As foregoing invention further preferably, the sulphur adding in described step 2 be reductant account for wool protein powder mass percent 0.5～1.5%.
As foregoing invention further preferably, the keratinase adding in described step 2 accounts for 0.5～1.5% of wool protein powder mass percent.
As foregoing invention further preferably, keratin solution and rayon spinning stock solution quality percentage used in described step 3 are 5～10%.
As foregoing invention further preferably, the crosslinking agent adding in described step 3 accounts for 5～10% of methylcellulose content in rayon spinning stoste.
As foregoing invention further preferably, the sulphur in described step 2 is a kind of that reductant can be in sodium sulfite, sodium hydrogensulfite or sodium thiosulfate.
As foregoing invention further preferably, the crosslinking agent in described step 3 can be the mixture of two or three in the chloro-2-propyl alcohol of 1,3-bis-, ethylene glycol diglycidylether or polyethyleneglycol diglycidylether.
The present invention adopts keratinase to be hydrolyzed to wool protein, first uses the disulfide bond of reductant opening angle protein macromolecule interchain, destroys its network structure, then adds keratinase to degrade to it; On the one hand destroyed network structure between keratin molecule adding of reductant, be more conducive to the hydrolysis of keratinase, raising the degradation efficiency of enzyme; Because biology enzyme has the features such as efficient, single-minded, reaction condition is gentle, the keratin solution hydrolysis degree obtaining is less on the other hand, and hydrolysate molecular weight more greatly and relatively concentrated, is conducive to the set with fiber more.In traditional fiber manufacture process, hydroformylation is to add in postchannel process, increase technological process, hydroformylation also makes formaldehyde overflow simultaneously has injury to human body, injury for fear of the fiber after acetal liquid in hydroformylation process and hydroformylation to human body, the present invention, by adding crosslinking agent in the wet spinning stage, increases the crosslinked set effectiveness of albumen on fiber, without process hydroformylation step, the technological process of the production of shortening, has improved production efficiency.
Adopt protein content in the wool keratin regenerated celulose fibre that the present invention prepares can reach more than 6%, overcome the lower shortcoming of protein content in the fiber that the method difference because of degraded wool keratin causes.In spinning process, add crosslinking agent, effectively albumen is anchored on fiber, not only can improve the content of albumen in fiber, can also guarantee after washing repeatedly in fiber that protein content can obviously not decline.Take method that bioanalysis is combined with reducing process to the wool extraction of degrading, first utilize reductant to carry out preliminary treatment to wool protein, with keratinase, it is degraded again, the keratin solution range of molecular weight distributions making is less, and molecular weight is relatively large, avoid the waste because too much running off and cause of protein, also reduced the consumption of auxiliary agent simultaneously, also solved the expensive problem that causes the higher difficult industrialization of production cost of auxiliary agent; This method, without through hydroformylation step, has shortened the technological process of production, has improved production efficiency.
The specific embodiment
Embodiment 1
Contrast chemical method, biological enzyme and the prepared keratin solution of the present invention.
Chemical method be mainly by acid and alkali hydrolysis method make protein macromolecule chain fracture or by redox method make in protein macromolecule () disulfide bonds arrive the object of dissolving.Mainly contain acid and alkali hydrolysis method, oxidizing process and reducing process etc.
Biological enzyme is to utilize the selectivity of keratinase to make its keratin degrading make the object of keratin solution.
The method that the present invention adopts biological enzyme to be combined with reducing process, first adds reductant to open the disulfide bond of (interior) between protein molecular, then adds keratinase effect to make keratin solution.
As can be known from the above table, not only dissolved efficiency is high for the prepared keratin solution of the present invention, and protein molecular is relatively large.
Embodiment 2
The preparation of viscose solution: adopt the Cotton Pulp of the degree of polymerization 500, the fine mass content 93.5% of first, prepare spinning viscose solution through operations such as dipping, squeezing, pulverizing, experienced, yellow, continuous-dissolution, filtration, deaerations successively.Make the fine mass content 8.9% of first, NaOH mass content 6.2%, viscosity (falling ball method) 45s, degree of ripeness (10%NH
4cl) 8.4ml, is stand-by viscose solution.
Falling ball method: 2mm steel ball falls the required time of 20cm from described viscose solution.
The preparation of keratin protein solution: in reactor, the keratin solution that is 8% with distilled water preparation mass fraction, first accounts for to adding in solution the NaHSO that wool protein powder mass percent is 1%
3, then account for to adding in reactor solution the keratinase that wool protein powder mass fraction is 1%, with NaOH regulator solution pH to 7.5-8.0, then solution is warming up to 50-60 ℃, insulation reaction 1h.The glyceryl tristearate dispersant that adds wool protein opaque amount 0.1%, stirring at normal temperature reaction 2h can obtain the gluten protein solution of clear.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, below 0.2Mpa, prepares keratin protein solution.
Viscose solution mixes with protein solution: adoption rate pump adds keratin protein solution in above-mentioned stand-by viscose solution quantitatively, and mixes.Keratin protein solution adopt syringe pump with the speed injection of 6 liters/min in dynamic mixer, in blender, add the polyethyleneglycol diglycidylether that accounts for the fine quality 10% of first simultaneously, it is mixed with viscose solution, and the flow of viscose solution is 50 liters/min.Wherein, keratic quality is 8.5% of the fine weight of first.
Wet spinning: the mixed solution of keratin solution and viscose glue is sent into wet spinning operation and carry out spinning.Spinning head specification is 21000 holes * 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 ℃, and plasticizing-bath temperature is 95 ℃.Coagulation bath composition is: sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.69dtex; Dry strong 2.10cN/dtex; Wet strong 1.42cN/dtex; Dryly stretch 18.1%, protein content is 6.36%.
Spinnability: can reduce in spinning process because the excessive end breakage rate making of front pressure of spinning that degree of hydrolysis is poor during protein dissolution brings more greatly because of protein body while making spinning increases.If adopt the method for filtering can make again protein content lower.Method of the present invention reduces end breakage rate and reaches 99%, has greatly improved the spinnability of fiber.
Determining the protein quantity: with reference to FZ/T54028-2010 (viscose protein content test method).
Embodiment 3
The preparation of viscose solution: adopt the Cotton Pulp of the degree of polymerization 520, the fine mass content 92.5% of first, prepare spinning viscose solution through operations such as dipping, squeezing, pulverizing, experienced, yellow, continuous-dissolution, filtration, deaerations successively.Make the fine mass content 8.7% of first, NaOH mass content 6.3%, viscosity (falling ball method) 63s, degree of ripeness (10%NH
4cl) 8.6ml, is stand-by viscose solution.
The preparation of precrosslink gluten protein matter solution: in reactor, the wool protein powder solution that is 10% with distilled water preparation mass fraction, first accounts for to adding in solution the Na that keratin quality percentage is 1%
2sO
3, then account for to adding in reactor solution the keratinase that wool protein powder mass fraction is 0.5%, with NaOH regulator solution pH to 7.5-8.0, then solution is warming up to 50-60 ℃, insulation reaction 1h.Add and account for wool protein opaque amount 0.5% calgon and 0.5% stearic acid list glyceride, stirring at normal temperature reaction 3h can obtain the keratin solution of clear.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, below 0.2Mpa, prepares keratin protein solution.
Viscose solution mixes with protein solution: adoption rate pump adds keratin solution in above-mentioned stand-by viscose solution quantitatively, and mixes.Keratin solution adopt syringe pump with the speed injection of 6 liters/min in dynamic mixer, in blender, add the ethylene glycol diglycidylether that accounts for the fine quality 7% of first simultaneously, it is mixed with viscose solution, the flow of viscose solution is 52 liters/min.Wherein, keratic quality is 8.1% of the fine weight of first.
Wet spinning: the mixed solution of keratin solution and viscose glue is sent into wet spinning operation and carry out spinning.Spinning head specification is 21000 holes * 0.05mm, and spinning speed is 52m/min, and coagulation bath temperature is 54 ℃, and plasticizing-bath temperature is 96 ℃.Coagulation bath composition is: sulfuric acid 120g/L, sodium sulphate 320g/L, zinc sulfate 12g/L.The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.65dtex; Dry strong 2.05cN/dtex; Wet strong 1.31cN/dtex; Dryly stretch 16.6%, keratin content is 6.85%.
Embodiment 4
The preparation of viscose solution: adopt the Cotton Pulp of the degree of polymerization 500, the fine mass content 92.3% of first, prepare spinning viscose solution through operations such as dipping, squeezing, pulverizing, experienced, yellow, continuous-dissolution, filtration, deaerations successively.Make the fine mass content 8.7% of first, NaOH mass content 5.8%, viscosity (falling ball method) 59s, degree of ripeness (10%NH
4cl) 8.8ml, is stand-by viscose solution.
The preparation of precrosslink gluten protein matter solution: in reactor, the wool protein solution that is 10% with distilled water preparation mass fraction, first accounts for to adding in solution the Na that wool protein quality percentage is 1%
2s
2o
3, then account for to adding in reactor solution the keratinase that wool protein quality mark is 0.5%, with NaOH regulator solution pH to 7.5-8.0, then solution is warming up to 50-60 ℃, insulation reaction 1h.。Add and account for wool protein opaque amount 0.4% calgon and 0.05% glyceryl tristearate, stirring at normal temperature reaction 2.5h can obtain the keratin solution of clear.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, below 0.2Mpa, prepares keratin protein solution.
Viscose solution mixes with protein solution: adoption rate pump adds keratin solution in above-mentioned stand-by viscose solution quantitatively, and mixes.Keratin solution adopt syringe pump with the speed injection of 3 liters/min in dynamic mixer, in blender, add the crosslinking agent ethylene glycol diglycidylether that accounts for the fine quality 5% of first simultaneously, it is mixed with viscose solution, and the flow of viscose solution is 51 liters/min.Wherein, keratic quality is 8.0% of the fine weight of first.
Wet spinning: the mixed solution of keratin solution and viscose glue is sent into wet spinning operation and carry out spinning.Spinning head specification is 21000 holes * 0.05mm, and spinning speed is 50m/min, and coagulation bath temperature is 54 ℃, and plasticizing-bath temperature is 98 ℃.Coagulation bath composition is: sulfuric acid 125g/L, sodium sulphate 330g/L, zinc sulfate 12.5g/L.The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.73dtex; Dry strong 2.16cN/dtex; Wet strong 1.37cN/dtex; Dryly stretch 16.5%, protein content is 6.57%.
Reference examples 1
The difference of the present embodiment and embodiment 2 is: chemical method, the prepared keratin solution of biological enzyme in embodiment 1 are used for to spinning.
Embodiment 2～4 is tested with reference examples 1 gained sample, and result is as follows:
| ? | Protein addition (to the fine meter of first)/% | Protein content/% on fiber |
| Acid and alkali hydrolysis method | 8 | 0.798 |
| Reducing process | 8 | 1.265 |
| Biological enzyme | 8 | 2.537 |
| Embodiment 2 | 8 | 6.41 |
| Embodiment 3 | 8 | 6.31 |
| Embodiment 4 | 8 | 6.37 |
From the above results, in the prepared fiber of the present invention, protein content is more than 6%, higher than protein content in the prepared fiber of method of other degraded wool keratins.
Reference examples 2
The difference of the present embodiment and embodiment 4 is: in wet spinning step, do not add crosslinking agent.
Embodiment and reference examples 2 gained samples are tested, and result is as follows:
From the above results, embodiment gained sample protein matter content is more than 6%, far away higher than reference examples sample, and after washing repeatedly embodiment sample protein matter content still more than 6%.In reference examples owing to not adding crosslinking agent, caused low percentages of protein on fiber, may be due to crosslinking agent and spinning solution compatibility better, there is difunctional and can form linear structure, linear two ends are connected with albumen with fiber respectively, thereby have strengthened set effectiveness.
Claims (9)
1. a preparation method for wool keratin regenerated celulose fibre, is characterized in that: comprise the following steps:
Step 1, Making viscose spinning solution;
Step 2, prepares wool keratin solution: with distilled water preparation wool protein powder solution, to adding sulphur in solution, be then reductant, after stirring, add again keratinase, pH value of solution is adjusted to 7.5～8.0, is warming up to 50～60 ℃, after insulation, filtration obtains keratin solution;
Step 3, mixes step 1 gained rayon spinning stoste and step 2 gained keratin solution, then adds crosslinking agent, carries out wet spinning after mixing.
2. the preparation method of wool keratin regenerated celulose fibre according to claim 1, is characterized in that: in described step 2, the crude protein content of wool protein powder used is greater than 80%.
3. the preparation method of wool keratin regenerated celulose fibre according to claim 1, is characterized in that: in described step 2, the wool protein powder liquid quality fraction of preparation is 8～12%.
4. the preparation method of wool keratin regenerated celulose fibre according to claim 3, is characterized in that: the sulphur adding in described step 2 be reductant account for wool protein powder mass percent 0.5～1.5%.
5. the preparation method of wool keratin regenerated celulose fibre according to claim 4, is characterized in that: the keratinase adding in described step 2 accounts for 0.5～1.5% of wool protein powder mass percent.
6. the preparation method of wool keratin regenerated celulose fibre according to claim 1, is characterized in that: keratin solution and rayon spinning stock solution quality percentage used in described step 3 are 5～10%.
7. the preparation method of wool keratin regenerated celulose fibre according to claim 1, is characterized in that: the crosslinking agent adding in described step 3 accounts for 5～10% of methylcellulose content in rayon spinning stoste.
8. the preparation method of wool keratin regenerated celulose fibre according to claim 1, is characterized in that: the sulphur in described step 2 is a kind of that reductant can be in sodium sulfite, sodium hydrogensulfite or sodium thiosulfate.
9. the preparation method of wool keratin regenerated celulose fibre according to claim 1, it is characterized in that: the crosslinking agent in described step 3 can be the mixture of two or three in the chloro-2-propyl alcohol of 1,3-bis-, ethylene glycol diglycidylether or polyethyleneglycol diglycidylether.
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| CN106757766A (en) * | 2016-12-15 | 2017-05-31 | 宜宾屏山辉瑞油脂有限公司 | A kind of collagen fabric cellulose fiber spunlace non-woven cloth and its production method |
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| CN106835492A (en) * | 2016-12-15 | 2017-06-13 | 宜宾屏山辉瑞油脂有限公司 | A kind of cashmere protein cellulose fiber spunlace non-woven cloth and its production method |
| CN109735949A (en) * | 2019-01-12 | 2019-05-10 | 太原理工大学 | A kind of anti-ultraviolet wet absorption fever protein tencel fiber and preparation method thereof |
| CN114990726A (en) * | 2022-06-27 | 2022-09-02 | 青岛融美发制品集团有限公司 | Production process for shape memory protein composite fiber |
| WO2023120697A1 (en) * | 2021-12-24 | 2023-06-29 | 株式会社ファーマフーズ | Recycled cellulose fibers, method for producing same, and fiber structure of same |
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| CN106835492B (en) * | 2016-12-15 | 2019-07-16 | 宜宾屏山辉瑞油脂有限公司 | A kind of production method of cashmere protein cellulose fiber spunlace non-woven cloth |
| CN109735949A (en) * | 2019-01-12 | 2019-05-10 | 太原理工大学 | A kind of anti-ultraviolet wet absorption fever protein tencel fiber and preparation method thereof |
| CN109735949B (en) * | 2019-01-12 | 2021-07-30 | 山西瑞赛格纺织科技有限公司 | Ultraviolet-resistant, moisture-absorbing and heating protein tencel fiber and preparation method thereof |
| WO2023120697A1 (en) * | 2021-12-24 | 2023-06-29 | 株式会社ファーマフーズ | Recycled cellulose fibers, method for producing same, and fiber structure of same |
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