CN103510179A - Preparation method for gluten protein regenerated cellulose fiber - Google Patents
Preparation method for gluten protein regenerated cellulose fiber Download PDFInfo
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Abstract
The invention discloses a preparation method for a gluten protein regenerated cellulose fiber. The method comprises the following steps: preparing a viscose spinning stock solution, preparing a gluten protein solution, preparing 8-12 percent by mass of a gluten flour solution, adding sodium hydroxide taking 4-10 percent by mass of the gluten flour solution and a dispersing agent taking 0.1 to 1 percent by mass of the gluten flour solution, stirring and reacting for 5 to 6 h at normal temperature, adding a cross-linking agent, reacting for 0.5 to 2 h at the normal temperature, obtaining the gluten protein solution after filtering, mixing the prepared gluten protein solution and the viscose spinning stock solution, and then performing wet spinning. The gluten protein regenerated cellulose fiber prepared through the method overcomes the problems of high production cost and difficulty in industrialization caused by high price of an auxiliary agent; by adopting an auxiliary agent with low price to perform protein pre-cross-linking, the loss of protein is avoided, and the protein content of the fiber is increased; and the method does not need a hydroformylation step, shortens the production technology process, and improves the production efficiency.
Description
Technical field
The present invention relates to raw material and manufacture method, particularly a kind of preparation method of gluten protein regenerated celulose fibre for textile industry.
Background technology
Gluten protein is the earliest as the byproduct of wheat starch production, used as fodder together with fiber etc.In Gluten, protein content is more than 80%, and amino acid ratio of components is more complete, is nutritious, inexpensive vegetable protein, for food aspect as strong gluten flour additive.According to the dissolution characteristics of protein in wheat berry, it is divided into four kinds of protein such as albumin, globulin, gliadin (gliadin) and glutenin.Gluten protein is a kind of reproducible natural polymer albumen, has biodegradability and biocompatibility, particularly aspect the non-food stuff Application in Chemical Engineering of gluten protein.Utilize the method modifying glutelin albumen such as physics, chemistry, enzyme process, can obtain novel high polymer functional material.This research has great importance to plant resources higher value application, also, for people make rational use of resources, reduces production costs, and realizes Green Chemistry new way is provided.
In azelon process, protein loss rate is large at present, and albumen can not finely anchor on fiber, even if spin in fiber, contains albumen, through the albumen of road (dyeing and printing process) arrangement later, also can run off gradually.
Chinese invention patent 201210137635.7 discloses a kind of wheat gluten fiber and manufacture method thereof, this patent utilization wheat itself is as material, cellulose in wheat bran is carried out to quaternization and obtain alkali cellulose, then by the alcohol soluble protein obtaining and glutenin under the effect of crosslinking agent, by wet spinning, spin fiber.The spinning glue spinnability that this method obtains is not good enough, and crosslinking agent prices are rather stiff (approximately 4500 yuan of 100mg).Chinese patent 200810136626.X has announced a kind of manufacture method of protein cellulose fiber, and the method, without through hydroformylation, is directly mixed protein solution with viscose solution, finally adopt wet spinning.Although the method has been avoided the pollution of formaldehydes solvent and residual, the number of dropouts of protein is larger.Chinese invention patent 200410010327.3 discloses a kind of manufacture method of soybean fiber cellulose fiber, and it is that the viscose glue that soybean protein spinning solution is produced with conventional method mixes, and carries out hydroformylation processing after wet spinning in acetal liquid again.The fiber spinnability that this method is manufactured is poor, and the acetal liquid in hydroformylation processing procedure also has certain injury to human body.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of loss of avoiding protein, improve fiber protein content, the preparation method to the useful gluten protein regenerated celulose fibre of health.
The present invention is by the following technical solutions:
A preparation method for gluten protein regenerated celulose fibre, comprises the steps:
(1) produce rayon spinning stoste;
(2) produce gluten protein solution: preparation mass percent is 8-12% Gluten solution, then add and account for the NaOH of solution quality percentage 4-10% and the dispersant that accounts for Gluten mass percent 0.1～1%, stirring at normal temperature reaction 5-6h, add crosslinking agent to react at normal temperatures 0.5-2h, after filtering, obtain gluten protein solution;
(3) the gluten protein solution making is mixed to rear wet spinning with rayon spinning stoste.
Gluten is natural polymer albumen, and amino acid ratio of components is more complete, has biodegradability and biocompatibility, for people make rational use of resources, reduces production costs, and realizes Green Chemistry new way is provided.Azelon skin-friendly is good, and skin is had to maintenance effect, and has soyeux feel and gloss, and in fiber, albumen increase can further improve these effects undoubtedly.The present invention adds after NaOH and dispersant make preliminary gluten protein solution in step (2), not directly itself and rayon spinning stoste to be mixed with to fiber, but add again crosslinking agent to carry out albumen precrosslink in preliminary gluten protein solution, its effect is to increase the crosslinked set of albumen on fiber, avoid the loss of protein, improve the protein content of fiber, the spinnability of fortifying fibre.
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, for step is avoided the injury to human body of fiber after acetal liquid in hydroformylation process and hydroformylation, the present invention improves adhering to of albumen by the precrosslink of step (2), and add described crosslinking agent in the wet spinning stage, further increase the crosslinked set effectiveness of albumen on fiber, without process hydroformylation step, the technological process of the production of shortening, has improved production efficiency.
As preferably, described step also adds hydrolysising protease in (2).The present invention adopts hydrolysising protease to be hydrolyzed to Gluten, adopt biological respinse to improve protein hydrolysis degree, reduce the network structure of gluten protein, disulfide bond in destruction protein is removed it and is cross-linked, make albumen can better be dispersed in solution system, improve the utilization rate of albumen, make protein body be hydrolyzed into nanometer or Subnano-class particle diameter, can better add fiber to gets on, objective raising fibrin utilization rate, can not destroy the rear protein of hydrolysis or amino acid, guaranteed that hydrolysate can participate in cross-linking reaction process better simultaneously yet.
As preferably, add hydrolysising protease regulator solution pH to 8-10, be then warming up to 50～60 ℃ of reaction 5-6h, repeated hydrogenation sodium oxide molybdena and dispersant afterwards, under alkali condition, hydrolysis effect is better, only needs a small amount of hydrolysising protease to be fully hydrolyzed, and improves protein utilization rate.
As preferably, hydrolysising protease accounts for the 0.1%-0.5% of Gluten mass percent.
Adopt hydrolysising protease to be hydrolyzed to Gluten, adopt biological respinse to improve protein hydrolysis degree, reduce the network structure of gluten protein, disulfide bond in destruction protein is removed it and is cross-linked, make albumen can better be dispersed in solution system, improve the utilization rate of albumen, make protein body be hydrolyzed into nanometer or Subnano-class particle diameter, can better add fiber to gets on, objective raising fibrin utilization rate, can not destroy the rear protein of hydrolysis or amino acid, guaranteed that hydrolysate can participate in cross-linking reaction process better simultaneously yet.Adding NaOH is for further protein hydrolysate, only adopts high-concentration sodium hydroxide solution to be hydrolyzed, and is difficult to destroy its network structure.By enzyme hydrolysis and diluted alkaline, processing two-step method is easy to obtain stable protein solution.And after NaOH and dispersant all add, then carry out stirring reaction, disperse more even.
As preferably, the described dispersant of step (2) is calgon, stearic acid list glyceride, one or more in glyceryl tristearate.
As preferably, the crosslinking agent described in step (2) accounts for the 1-3% of Gluten mass percent.
As preferably, in described step (3), gluten protein solution and rayon spinning stoste are 1:100～12:100 in mass ratio.
As preferably, in described step (3), also add the crosslinking agent that accounts for the 3-10% of the fine quality of first in rayon spinning stoste, described crosslinking agent is: the mixture of one or both in the chloro-2-propyl alcohol of 1,3-bis-, ethylene glycol diglycidylether, polyethyleneglycol diglycidylether.
As preferably, described crosslinking agent is: the mixture of one or both in the chloro-2-propyl alcohol of 1,3-bis-, ethylene glycol diglycidylether, polyethyleneglycol diglycidylether.
Crosslinking agent of the present invention and spinning solution compatibility are better, have difunctional and can form linear structure, and linear two ends are connected with albumen with fiber respectively, and set effectiveness is better; Also can prevent that spinning solution should excessively be cross-linked to form netted micelle.
First fibre described in the present invention is alpha cellulose, claims again alpha-cellulose, refer to cellulosic material in 20 ℃ are dipped in 17.5% or 18% sodium hydroxide solution after 45 minutes undissolved part.
The gluten protein regenerated celulose fibre that adopts the inventive method to prepare has overcome the problem that causes the higher difficult industrialization of production cost because auxiliary agent is expensive; Adopt hydrolysising protease and sodium hydroxide solution protein hydrolysate, to improve the degree of hydrolysis of albumen; Adopt cheap auxiliary agent to carry out albumen precrosslink simultaneously, avoid the loss of protein, improved the protein content of fiber; This method, without through hydroformylation step, has shortened the technological process of production, has improved production efficiency.
The specific embodiment
Below by specific embodiment, the present invention is further described in detail.
Embodiment 1: the preparation method one of gluten protein regenerated celulose fibre
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 precrosslink gluten protein matter solution:
In reactor, the Gluten solution that is 8% with distilled water preparation mass fraction, to adding in reactor solution, to account for Gluten mass fraction be 0.1% hydrolysising protease, regulator solution pH to 8, is then warming up to solution 50 ℃, insulation reaction 5h.To adding in solution after reaction, to account for liquid quality fraction be 10% NaOH, adds the glyceryl tristearate dispersant that accounts for Gluten quality 0.1%, and stirring at normal temperature reaction 5h can obtain the gluten protein solution of clear.To adding in gained protein solution, account for 1 of glutelin opaque mass content 1.5% again, the chloro-2-propyl alcohol of 3-bis-and the polyethyleneglycol diglycidylether that accounts for glutelin opaque mass content 1.5%, insulation reaction 0.5h, adopt sheet frame filter to filter through double-deck fine cloth, pressure, below 0.2Mpa, prepares gluten protein matter solution.
Viscose solution mixes with protein solution: adoption rate pump adds precrosslink protein solution in above-mentioned stand-by viscose solution quantitatively, and mixes.The protein solution of precrosslink 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.In final mixed solution, the quality of gluten protein is 7.3% of the fine quality of first.
Wet spinning: the mixed solution of precrosslink protein 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 120g/L, sodium sulphate 330g/L, zinc sulfate 11g/L.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.69dtex; Dry strong 2.04cN/dtex; Wet strong 1.3cN/dtex; Dryly stretch 17.6%, protein content is 6.28%.
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 end breakage rate of the present invention obviously reduces, and has greatly improved the spinnability of fiber.
Determining the protein quantity: with reference to FZ/T54028-2010 (viscose protein content test method).
Embodiment 2: the preparation method two of gluten protein regenerated celulose fibre
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 Gluten solution that is 12% with distilled water preparation mass fraction, to adding in reactor solution, to account for Gluten mass fraction be 0.5% hydrolysising protease, regulator solution pH to 10, is then warming up to solution 60 ℃, insulation reaction 6h.To adding in solution after reaction, to account for liquid quality fraction be 4% NaOH, adds and account for Gluten quality 0.5% calgon and 0.5% stearic acid list glyceride, and stirring at normal temperature reaction 6h can obtain the gluten protein solution of clear.To adding in gained protein solution, account for 1 of glutelin opaque mass content 0.5% again, the chloro-2-propyl alcohol of 3-bis-and the ethylene glycol diglycidylether that accounts for glutelin opaque mass content 0.5%, insulation reaction 2h, adopt sheet frame filter to filter through double-deck fine cloth, pressure, below 0.2Mpa, prepares gluten protein matter solution.
Viscose solution mixes with protein solution: adoption rate pump adds precrosslink protein solution in above-mentioned stand-by viscose solution quantitatively, and mixes.The protein solution of precrosslink 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, and the flow of viscose solution is 52 liters/min.Wherein, the quality of gluten protein is 8.1% of the fine quality of first.
Wet spinning: the mixed solution of precrosslink protein 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 125g/L, sodium sulphate 325g/L, zinc sulfate 12g/L.The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.58dtex; Dry strong 2.11cN/dtex; Wet strong 1.26cN/dtex; Dryly stretch 17.6%, protein content is 7.04%.
Embodiment 3: the preparation method three of gluten protein regenerated celulose fibre
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 8.6% of first, NaOH mass content 6.1%, viscosity (falling ball method) 63s, degree of ripeness (10%NH
4cl) 8.3ml, is stand-by viscose solution.
The preparation of precrosslink gluten protein matter solution:
In reactor, the Gluten solution that is 10% with distilled water preparation mass fraction, to adding in reactor solution, to account for Gluten mass fraction be 0.1% hydrolysising protease, regulator solution pH to 9, is then warming up to solution 55 ℃, insulation reaction 5.5h.To adding in solution after reaction, to account for liquid quality fraction be 7% NaOH, adds and account for Gluten quality 0.4% calgon and 0.05% glyceryl tristearate, and stirring at normal temperature reaction 5.5h can obtain the gluten protein solution of clear.To adding in gained protein solution, account for 1 of glutelin opaque mass content 0.3% again, the chloro-2-propyl alcohol of 3-bis-, account for the ethylene glycol diglycidylether of glutelin opaque mass content 0.8% and account for the polyethyleneglycol diglycidylether of glutelin opaque mass content 0.4%, insulation reaction 1h, adopt sheet frame filter to filter through double-deck fine cloth, pressure, below 0.2Mpa, prepares gluten protein matter solution.
Viscose solution mixes with protein solution: adoption rate pump adds precrosslink protein solution in above-mentioned stand-by viscose solution quantitatively, and mixes.The protein solution of precrosslink 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 3% of first simultaneously, it is mixed with viscose solution, and the flow of viscose solution is 50 liters/min.Wherein, the quality of gluten protein is 7.6% of the fine quality of first.
Wet spinning: the mixed solution of precrosslink protein 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 126g/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 1.63dtex; Dry strong 2.24cN/dtex; Wet strong 1.23cN/dtex; Dryly stretch 16.8%, protein content is 6.46%.
Reference examples 1
According to the same method of embodiment 1, prepare gluten protein solution, different is after hydrolysis completes, and directly obtains preliminary gluten protein solution, no longer adds crosslinking agent 1, and the chloro-2-propyl alcohol of 3-bis-and polyethyleneglycol diglycidylether carry out insulation reaction.
Conclusion: add crosslinking agent after hydrolysis, can further improve the protein content of gluten protein solution.
Reference examples 2
According to the same method of embodiment 2, prepare gluten protein solution, different is not enzyme-added, directly adds NaOH and dispersant hydrolysis, then adds crosslinking agent to obtain gluten protein solution.
Conclusion: reference examples 2 is directly hydrolyzed with high-concentration sodium hydroxide solution, and its action time is longer, and alkali consumption is higher.
Embodiment 2 first adds an enzyme hydrolysis part, makes protein become fine particle; Then add dilute alkali and continue hydrolysis, further the hydrolysis of hydro-oxidation sodium does not destroy protein, makes on the contrary the content of protein improve.
Reference examples 3
According to the same method of embodiment 1, prepare gluten protein solution, different is in the step of in the end wet spinning, does not add crosslinking agent, carries out wet spinning after mixing.
Conclusion: in the end, in the step of wet spinning, add crosslinking agent, can obviously improve the content of protein on fiber, and on fiber, albumen endurance quality is better.
In addition, the invention is not restricted to above-mentioned embodiment, as long as within not exceeding scope of the present invention, can take variety of way to implement the present invention.
Claims (8)
1. a preparation method for gluten protein regenerated celulose fibre, is characterized in that comprising the steps:
(1) produce rayon spinning stoste;
(2) produce gluten protein solution: preparation mass percent is 8-12% Gluten solution, then add and account for the NaOH of solution quality percentage 4-10% and the dispersant that accounts for Gluten mass percent 0.1 ~ 1%, stirring at normal temperature reaction 5-6h, add crosslinking agent to react at normal temperatures 0.5-2h, after filtering, obtain gluten protein solution;
(3) the gluten protein solution making is mixed to rear wet spinning with rayon spinning stoste.
2. the preparation method of gluten protein regenerated celulose fibre according to claim 1, is characterized in that: described step also adds hydrolysising protease in (2).
3. the preparation method of gluten protein regenerated celulose fibre according to claim 2, is characterized in that: hydrolysising protease accounts for the 0.1%-0.5% of Gluten mass percent.
4. the preparation method of gluten protein regenerated celulose fibre according to claim 1, is characterized in that: the described dispersant of step (2) is calgon, stearic acid list glyceride, one or more in glyceryl tristearate.
5. the preparation method of gluten protein regenerated celulose fibre according to claim 1, is characterized in that: the crosslinking agent described in step (2) accounts for the 1-3% of Gluten mass percent.
6. the preparation method of gluten protein regenerated celulose fibre according to claim 1, is characterized in that: in described step (3), gluten protein solution and rayon spinning stoste are 1:100～12:100 in mass ratio.
7. the preparation method of gluten protein regenerated celulose fibre according to claim 1, it is characterized in that: in described step (3), also add the crosslinking agent that accounts for the 3-10% of the fine quality of first in rayon spinning stoste, described crosslinking agent is: the mixture of one or both in the chloro-2-propyl alcohol of 1,3-bis-, ethylene glycol diglycidylether, polyethyleneglycol diglycidylether.
8. the preparation method of gluten protein regenerated celulose fibre according to claim 1, it is characterized in that: described crosslinking agent is: the mixture of one or both in the chloro-2-propyl alcohol of 1,3-bis-, ethylene glycol diglycidylether, polyethyleneglycol diglycidylether.
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| CN104451929A (en) * | 2014-11-20 | 2015-03-25 | 江苏金太阳纺织科技有限公司 | Cooling regenerative cellulose fiber and preparation method thereof |
| CN105088583B (en) * | 2015-07-08 | 2017-01-18 | 立天集团有限公司 | Ecological sizing method for linen viscose blended yarn |
| CN105088583A (en) * | 2015-07-08 | 2015-11-25 | 立天集团有限公司 | Ecological sizing method for linen viscose blended yarn |
| CN105056287A (en) * | 2015-07-29 | 2015-11-18 | 李文新 | Acarus-killing, antibacterial and medical bandage |
| CN105105922A (en) * | 2015-07-29 | 2015-12-02 | 李文新 | Method of preparing medical acarus killing and anti-microbial bandage |
| CN105105922B (en) * | 2015-07-29 | 2018-03-09 | 张作玮 | A kind of preparation method of except mite antibacterial medical bandage |
| CN106350896A (en) * | 2016-08-29 | 2017-01-25 | 山东银鹰化纤有限公司 | Novel preparing method for vegetable protein viscose |
| CN107164828A (en) * | 2017-07-10 | 2017-09-15 | 唐卫兵 | The preparation method of corn gluten protein modified function fiber |
| CN112176441A (en) * | 2020-09-15 | 2021-01-05 | 立肯诺(上海)新材料科技有限公司 | Preparation method of pearl protein fiber |
| CN112176441B (en) * | 2020-09-15 | 2023-04-14 | 立肯诺(上海)新材料科技有限公司 | Preparation method of pearl protein fiber |
| CN114622296A (en) * | 2022-02-28 | 2022-06-14 | 上海食未生物科技有限公司 | Method for continuously preparing edible fiber scaffold for cell culture meat |
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