CN103484962B - Gluten fiber preparation method - Google Patents
Gluten fiber preparation method Download PDFInfo
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- CN103484962B CN103484962B CN201310458285.9A CN201310458285A CN103484962B CN 103484962 B CN103484962 B CN 103484962B CN 201310458285 A CN201310458285 A CN 201310458285A CN 103484962 B CN103484962 B CN 103484962B
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Abstract
The invention relates to a gluten fiber preparation method which comprises steps as follows: (1), preparation of a spinning solution; (2), spinning with a wet method; (3) solidification; (4) crosslinking treatment of citric acid; (5), secondary drafting; and (6), thermal treatment for sizing. The gluten fiber preparation method has the advantages of low production cost and simple and efficient production process of gluten fiber.
Description
Technical field
The present invention relates to a kind of preparation method of protein fibre, particularly relating to a kind of is the method that protein fibre prepared by raw material with Gluten, belongs to technical field of polymer materials.
Background technology
China be global textile industry intensively, textile industry is the conventional column industry of China's national economy and important people's livelihood industry, weaving production capacity generally close to the half in the world.At present, China's textiles consumer need turns to type of enjoying to consume by living type consumption, main body of consumption is become gradually from textile production base, people grow with each passing day for the demand of high-quality textiles, high quality fiber are especially had to the demand of the protein fibre of good affinity to human body equally in continuous increase.Conventional traditional natural protein fibre comprises lint class and silk fibrid.The wearability that this two types of fibers is good with comfortableness, good luster, elegant style etc. are outstanding and be subject to the favor of consumer, but its resource-constrained, price are high, in global textile fabric total quantity consumed, only account for about 3.5%.Therefore, people start the research and development of azlon very early.At present, the azlon realizing industrialization comprising soybean fiber and milk protein fiber etc. is not all soybean protein regenerated fiber or the milk protein regenerated fiber of 100%, wherein containing have an appointment 55 ~ 75% synthetic high polymer, these fibers are difficult to meet the requirement of high-end textiles for fiber quality.
Chinese patent: publication number CN1370856 discloses a kind of azlon and manufacture method thereof, it uses keratin as the preparation method of the azlon of raw material, but the large intermolecular disulfide bond substantial amounts of keratin, in the layoutprocedure of spinning solution, protein is difficult to abundant swelling stretching, extension, fiber strength can not be guaranteed, use the materials such as mercaptoethanol poisonous in a large number or TGA in the preparation process of fiber, production process is complicated and security is not enough.Chinese patent: publication number CN102634860A discloses a kind of wheat protein fiber and manufacture method thereof, the method does that the celloglobulin content prepared is low, and preparation process uses sodium hydroxide solution, sulfuric acid solution in a large number, and production process is polluted large.
Summary of the invention
For above-mentioned shortcoming, the object of the present invention is to provide the simple preparation method with efficient gluten fiber of the low and production technology of a kind of production cost.
Technology contents of the present invention is: a kind of preparation method of gluten fiber, it comprises the steps:
(1), spinning solution preparation
Gluten being dissolved in molar concentration is in the urea liquid of 5 ~ 15mol/L, makes solution temperature be that 20 ~ 50 DEG C of condition lower seals leave standstill 5 ~ 40h, obtain spinning solution after stirring; The mass ratio of described Gluten and urea liquid is 1:2.5 ~ 1:5;
(2), wet spinning
Spinning solution step (1) obtained is carry out drawing-off spinning under the condition of 60 ~ 90 DEG C in temperature, is tentatively become the glutelin strand of silk;
(3), solidify
At normal temperatures, the glutelin strand of preliminary one-tenth silk obtained in step (2) is immersed Na
2sO
4tentatively solidify in solution, setting time is 15 ~ 45min, obtains the glutelin strand solidified; Na
2sO
4the mass percent concentration of solution is 5 ~ 15%; The glutelin strand of preliminary one-tenth silk and Na
2sO
4the mass ratio of solution is 1:2 ~ 1:10;
(4), citric acid crosslinking Treatment
Obtain hygrometric state gluten fiber by carrying out crosslinking Treatment in the glutelin strand solidified obtained in step (3) immersion citric acid solution, crosslinking temperature is 40 ~ 60 DEG C, and crosslinking time is 1 ~ 3h; The molar concentration of citric acid solution is 0.8 ~ 1mol/L, and pH value is 8 ~ 10; The glutelin strand solidified and the mass ratio of citric acid solution are 1:2 ~ 1:20;
(5), secondary drawing-off
Hygrometric state gluten fiber obtained in step (4) is carried out secondary drawing-off, and drafting multiple is 2 ~ 6 times, and the fiber after drawing-off dries obtained gluten fiber first product in 60 ~ 85 DEG C of hot blasts;
(6), sizing heat treatment
Gluten fiber first product obtained in step (5) is carried out sizing heat treatment 1 ~ 3h in the hot-air of 100 ~ 145 DEG C, obtains finished product gluten fiber.
In the preparation method of above-mentioned gluten fiber, also containing mass percent concentration in the urea liquid in step (1) is the Na of 0.5 ~ 1.5%
2sO
3reductant; The mass ratio of Gluten and urea liquid optimization is 1:3 ~ 1:4, and the time of repose of optimization is 10 ~ 12h; Contain a large amount of disulfide bond between glutenin molecule, in alcohol soluble protein molecule in glutelin, disulfide bond is at Na
2sO
3easily fragment into sulfydryl under the effect of reductant, two sulfydryls again oxidizedly can form disulfide bond again simultaneously; When the sulfydryl of the oxidized disulfide bond again formed divides the period of the day from 11 p.m. to 1 a.m greatly from difference, protein macromolecule generation self-crosslinking; The heighten degree that the dwell temperature that spinning solution is suitable and time of repose make protein macromolecule dissolve and stretch, intermolecular contacts, entanglement degree are suitable, good spinnability.
In the preparation method of above-mentioned gluten fiber, in step (2), drawing-off spinning temperature is optimized for 70 DEG C ~ 80 DEG C.
In the preparation method of above-mentioned gluten fiber, optimizing drafting multiple in step (5) is 3 ~ 4 times.
In the preparation method of above-mentioned gluten fiber, in step (6), sizing heat treatment temperature is optimized for 115 ~ 120 DEG C.
Wheat is China staple crops, and wheat aft-loaded airfoil and comprehensive utilization have important function to the development of Chinese national economy and social stability.In recent years due to the development of food, chemical industry, biology, pharmaceuticals industry, the purposes of wheaten starch constantly expands, and its output increases year by year.As Wheat Starch Processing Industry, take wheat as Gluten and the gluten powder of the byproduct such as fermentation industry of raw material, its output increases year by year, current Chinese festiva output reaches more than 100,000 tons, and world's annual production reaches more than 500,000 tons, wide material sources, with low cost.Protein content in Gluten is more than 80%, and major protein components is wherein alcohol soluble protein and glutenin, and both respectively account for about 40%.Alcohol soluble protein molecular weight, the intermolecular hydrogen bond lower by bond energy and hydrophobic bond interact; Glutenin molecular weight is comparatively large, intermolecular connected by disulfide bond.The interaction of two kinds of protein makes wheat gluten have better ductility and hydrothermal stability than other plant albumen.
Citric acid and 2-hydroxy propane-1,2,3 tricarboxylic acids are a kind of important organic acids; It is extensively present in occurring in nature, exists in a large number in the fruit of a lot of fruits and vegetables especially Citrus; The current mankind, by fermentation process, are that raw material carries out suitability for industrialized production citric acid with carbohydrate.Citric acid can produce crosslinked action to protein, cellulose, and cross-linking process is efficient, nontoxic; Carboxyl in citric acid can react with the amino in protein as when catalyst at alkali, produces crosslinked action to protein macromolecule.
The present invention is advantageously: the cost of production gluten fiber of the present invention is low and production technology is simple and efficient; Not only tensile mechanical properties is good for the gluten fiber that the present invention produces, and can be degradable, good biocompatibility, can be applicable to the fields such as the manufacture of high-quality textiles and biology, medicine, organizational project; The present invention not only makes a large amount of remaining glutelin get utilization, and fills up the demand gap of textile industry for high-quality protein fibre.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
(1), spinning solution preparation
100Kg Gluten being dissolved in quality is in the urea liquid of Gluten 3 times, makes solution temperature be that 40 DEG C of condition lower seals leave standstill 12h, obtain spinning solution after stirring; Wherein the molar concentration of urea liquid is 9mol/L, and containing mass percent concentration in described urea liquid is the Na of 1%
2sO
3reductant;
(2), wet spinning
Spinning solution step (1) obtained is carry out drawing-off spinning under the condition of 70 DEG C in temperature, is tentatively become the glutelin strand of silk;
(3), solidify
At normal temperatures, the glutelin strand of preliminary one-tenth silk obtained in step (2) is immersed Na
2sO
4tentatively solidify in solution, setting time is 30min, obtains the glutelin strand solidified; Na
2sO
4the mass percent concentration of solution is 8%; The glutelin strand of preliminary one-tenth silk and Na
2sO
4the mass ratio of solution is 1:6;
(4), citric acid crosslinking Treatment
Obtain hygrometric state gluten fiber by carrying out crosslinking Treatment in the glutelin strand solidified obtained in step (3) immersion citric acid solution, crosslinking temperature is 40 DEG C, and crosslinking time is 2h; The molar concentration of citric acid solution is 0.8mol/L, and pH value is 9; The glutelin strand solidified and the mass ratio of citric acid solution are 1:10;
(5), secondary drawing-off
Hygrometric state gluten fiber obtained in step (4) is carried out secondary drawing-off, and drafting multiple is 4 times, and the fiber after drawing-off dries obtained gluten fiber first product in 65 DEG C of hot blasts;
(6), sizing heat treatment
Gluten fiber first product obtained in step (5) is carried out sizing heat treatment 1.5h in the hot-air of 120 DEG C, obtains finished product gluten fiber.
Embodiment 2
(1), spinning solution preparation
100Kg Gluten being dissolved in quality is in the urea liquid of Gluten 4 times, makes solution temperature be that 50 DEG C of condition lower seals leave standstill 10h, obtain spinning solution after stirring; Wherein the molar concentration of urea liquid is 9mol/L, and containing mass percent concentration in described urea liquid is the Na of 0.8%
2sO
3reductant;
(2), wet spinning
Spinning solution step (1) obtained is carry out drawing-off spinning under the condition of 80 DEG C in temperature, is tentatively become the glutelin strand of silk;
(3), solidify
At normal temperatures, the glutelin strand of preliminary one-tenth silk obtained in step (2) is immersed Na
2sO
4tentatively solidify in solution, setting time is 15min, obtains the glutelin strand solidified; Na
2sO
4the mass percent concentration of solution is 10%; The glutelin strand of preliminary one-tenth silk and Na
2sO
4the mass ratio of solution is 1:8;
(4), citric acid crosslinking Treatment
Obtain hygrometric state gluten fiber by carrying out crosslinking Treatment in the glutelin strand solidified obtained in step (3) immersion citric acid solution, crosslinking temperature is 50 DEG C, and crosslinking time is 1.5h; The molar concentration of citric acid solution is 1mol/L, and pH value is 10; The glutelin strand solidified and the mass ratio of citric acid solution are 1:9;
(5), secondary drawing-off
Hygrometric state gluten fiber obtained in step (4) is carried out secondary drawing-off, and drafting multiple is 3 times, and the fiber after drawing-off dries obtained gluten fiber first product in 80 DEG C of hot blasts;
(6), sizing heat treatment
Gluten fiber first product obtained in step (5) is carried out sizing heat treatment 3h in the hot-air of 115 DEG C, obtains finished product gluten fiber.
Embodiment 3
(1), spinning solution preparation
100Kg Gluten being dissolved in quality is in the urea liquid of Gluten 5 times, makes solution temperature be that 20 DEG C of condition lower seals leave standstill 40h, obtain spinning solution after stirring; Wherein the molar concentration of urea liquid is 9mol/L, and containing mass percent concentration in described urea liquid is the Na of 1.5%
2sO
3reductant;
(2), wet spinning
Spinning solution step (1) obtained is carry out drawing-off spinning under the condition of 90 DEG C in temperature, is tentatively become the glutelin strand of silk;
(3), solidify
At normal temperatures, the glutelin strand of preliminary one-tenth silk obtained in step (2) is immersed Na
2sO
4tentatively solidify in solution, setting time is 45min, obtains the glutelin strand solidified; Na
2sO
4the mass percent concentration of solution is 15%; The glutelin strand of preliminary one-tenth silk and Na
2sO
4the mass ratio of solution is 1:6;
(4), citric acid crosslinking Treatment
Obtain hygrometric state gluten fiber by carrying out crosslinking Treatment in the glutelin strand solidified obtained in step (3) immersion citric acid solution, crosslinking temperature is 60 DEG C, and crosslinking time is 3h; The molar concentration of citric acid solution is 0.9mol/L, and pH value is 8; The glutelin strand solidified and the mass ratio of citric acid solution are 1:12;
(5), secondary drawing-off
Hygrometric state gluten fiber obtained in step (4) is carried out secondary drawing-off, and drafting multiple is 6 times, and the fiber after drawing-off dries obtained gluten fiber first product in 85 DEG C of hot blasts;
(6), sizing heat treatment
Gluten fiber first product obtained in step (5) is carried out sizing heat treatment 1h in the hot-air of 145 DEG C, obtains finished product gluten fiber.
Above-mentioned explanation fully discloses the specific embodiment of the present invention.It is pointed out that any change be familiar with person skilled in art and the specific embodiment of the present invention is done
All do not depart from the scope of claims of the present invention.Correspondingly, the scope of claim of the present invention is also not limited only to previous embodiment.
Claims (5)
1. a preparation method for gluten fiber, it comprises the steps:
(1), spinning solution preparation
Gluten being dissolved in molar concentration is in the urea liquid of 5 ~ 15mol/L, makes solution be that 20 ~ 50 DEG C of condition lower seals leave standstill 5 ~ 40h in temperature, obtain spinning solution after stirring; The mass ratio of described Gluten and urea liquid is 1:2.5 ~ 1:5;
(2), wet spinning
Spinning solution step (1) obtained is carry out drawing-off spinning under the condition of 60 ~ 90 DEG C in temperature, is tentatively become the glutelin strand of silk;
(3), solidify
At normal temperatures, the glutelin strand of preliminary one-tenth silk obtained in step (2) is immersed Na
2sO
4tentatively solidify in solution, setting time is 15 ~ 45min, obtains the glutelin strand solidified; Na
2sO
4the mass percent concentration of solution is 5 ~ 15%; The glutelin strand of preliminary one-tenth silk and Na
2sO
4the mass ratio of solution is 1:2 ~ 1:10;
(4), citric acid crosslinking Treatment
Obtain hygrometric state gluten fiber by carrying out crosslinking Treatment in the glutelin strand solidified obtained in step (3) immersion citric acid solution, crosslinking temperature is 40 ~ 60 DEG C, and crosslinking time is 1 ~ 3h; The molar concentration of citric acid solution is 0.8 ~ 1mol/L, and pH value is 8 ~ 10; The glutelin strand solidified and the mass ratio of citric acid solution are 1:2 ~ 1:20;
(5), secondary drawing-off
Hygrometric state gluten fiber obtained in step (4) is carried out secondary drawing-off, and drafting multiple is 2 ~ 6 times, and the fiber after drawing-off dries obtained gluten fiber first product in 60 ~ 85 DEG C of hot blasts;
(6), sizing heat treatment
Gluten fiber first product obtained in step (5) is carried out sizing heat treatment 1 ~ 3h in the hot-air of 100 ~ 145 DEG C, obtains finished product gluten fiber.
2. the preparation method of gluten fiber according to claim 1, is characterized in that also containing mass percent concentration in the urea liquid in step (1) is the Na of 0.5 ~ 1.5%
2sO
3reductant; The mass ratio of Gluten and urea liquid is 1:3 ~ 1:4, and time of repose is 10 ~ 12h.
3. the preparation method of gluten fiber according to claim 1, is characterized in that in step (2), drawing-off spinning temperature is 70 DEG C ~ 80 DEG C.
4. the preparation method of gluten fiber according to claim 1, is characterized in that in step (5), drafting multiple is preferably 3 ~ 4 times.
5. the preparation method of gluten fiber according to claim 1, is characterized in that in step (6), sizing heat treatment temperature is 115 ~ 120 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101117389A (en) * | 2007-07-20 | 2008-02-06 | 浙江大学 | Aqueous solvent composition for dissolving wheat preservation protein and use thereof |
| CN101660215A (en) * | 2009-09-23 | 2010-03-03 | 陈福库 | Protein and cellulose composite fiber and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101117389A (en) * | 2007-07-20 | 2008-02-06 | 浙江大学 | Aqueous solvent composition for dissolving wheat preservation protein and use thereof |
| CN101660215A (en) * | 2009-09-23 | 2010-03-03 | 陈福库 | Protein and cellulose composite fiber and manufacturing method thereof |
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