CN1837424B - Method for manufacturing functional fiber with protein and acrylonitrile - Google Patents
Method for manufacturing functional fiber with protein and acrylonitrile Download PDFInfo
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- CN1837424B CN1837424B CN2005100174358A CN200510017435A CN1837424B CN 1837424 B CN1837424 B CN 1837424B CN 2005100174358 A CN2005100174358 A CN 2005100174358A CN 200510017435 A CN200510017435 A CN 200510017435A CN 1837424 B CN1837424 B CN 1837424B
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Abstract
This invention discloses a Method for preparation of functional fibre containing protein and acrylonitrile, which comprises the following steps: adding raw material containing protein and acrylonitrile into metal salt solution; making them grafted copolymerization, ripened, deaerated, spun, congealed, desalted, drafted, washed, dried, curled and cut to get the fibre; adding alkali, metallic oxide, oxidant, reducer into at least one liquid of desalting liquor and washing liquor. The fibre has the character of synthon, that is, of the tactility of cashmere and the gloss of pure silk, and of good hygroscopicity, subtle touch, air perviousness; in accordance with needs, making the fibre combined with materials containing different elements to produce the fibre with the function of bacteriostasis, ultraviolet resistance, electromagnetic wave absorption, or far infrared.
Description
Technical field
The invention belongs to the manufacture method of synthetic fiber, relate in particular to the manufacture method of synthetic fiber with functional effect.
Background technology
Application number is to disclose a kind of plant animal protein and acrylonitrile graft copolymer fibre in 03148421.2 the patent application document, and provide the manufacture method of this fiber, learn that by content described herein this fiber has the same feel of cashmere, gloss that real silk is the same, and have moisture absorption, characteristics such as smooth, ventilative; But that this fiber does not have is antibacterial, prevent ultraviolet ray, radiation proof, absorption electromagnetic wave function and have far-infrared functional and the function of negative oxygen ion radiation.
Summary of the invention
The purpose of this invention is to provide the method that a kind of manufacturing contains the functional fiber of protein and acrylonitrile, promptly utilize fiber that this method produces to remove and has the feel of cashmere, the gloss of real silk, and have moisture absorption, characteristics such as smooth, ventilative; Also have antibacterial, prevent ultraviolet ray, radiation proof, absorption electromagnetic wave function and have far-infrared functional and the function of negative oxygen ion radiation.
The objective of the invention is to be achieved through the following technical solutions:
A kind of manufacture method that contains the functional fiber of protein and acrylonitrile, be to add in the metal salt solution with the raw material that comprises protein and acrylonitrile, make their graft copolymerization and after maturation, deaeration, spinning, solidify, desalination, drawing-off, washing, drying, curl, cut off and form, in desalination body lotion or water lotion, add metal oxide, the metal oxide that adds in the desalination body lotion is calcium oxide, magnesia or barium monoxide, and the metal oxide that adds in water lotion is silver oxide, calcium oxide or iron oxide.
Contain protein and acrylonitrile therefore it has the characteristic of synthetic fiber owing to make raw material that this fiber adopts, promptly have the feel of cashmere, the gloss of real silk, and have good moisture absorption, characteristics such as smooth, ventilative; Owing to be to add alkali at least a liquid at desalination body lotion and water lotion in this fiber process of manufacturing, metal oxide, oxidant or reductant, in the time of in these materials add acid desalination body lotion, then form salt, they and fiber complexing are together, they still can combine with fiber when these materials join water lotion, it is functional to cause fiber to produce, allow fiber combine as required, then can produce or have antibacterial with the material that contains different elements, or has a ultraviolet ray of preventing, or has a radiation proof, or the fiber that has the absorption electromagnetic wave and have red function far away.
The specific embodiment
Embodiment 1: with milk casein 8 weight portions, soybean protein 12 weight portions, put into the solution of the acrylonitrile that contains 70 weight portions, they are stirred, then in their mixed liquor, add again and contain 10 weight portions, concentration is 10% solder(ing)acid, after stirring, they were dissolved 8 hours mutually, then make temperature reduce to 10 ℃, add oxidant sodium peroxydisulfate and reductant sodium sulfite again, the addition of oxidant is 0.3% of the dried solid amount of acrylonitrile, the addition of reductant is 5 times of oxidant content, allow above-mentioned substance react again 1 hour, carry out graft copolymerization, then left standstill 6 hours, carry out wet spinning after 3 hours through deaeration, entering concentration by the spun silk of spinning machine is 10%, temperature be 20 ℃ contain zinc chloride solidify solution after, enter temperature again and be in 20 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the NaOH of 10 weight portions, but this body lotion still is acid, and its pH value is 4, and the fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 80 ℃ the neutral hot water and wash, the fiber after washing is drying again, be finished product after the typing.
Embodiment 2: with milk casein 10 weight portions, soybean protein 10 weight portions, acrylonitrile 65 weight portions, add and contain 15 weight portions, concentration is 15% solder(ing)acid, after stirring, under 60 ℃ temperature, make their mutual swellings 7 hours, then make temperature reduce to 12 ℃, add oxidant ammonium persulfate and reductant sodium hydrogensulfite again, the amount that adds oxidant is 1% of the dried solid amount of acrylonitrile, the reductant addition is 3 times of oxidant, allow above-mentioned substance react 1 hour, carry out graft copolymerization, then left standstill 72 hours, carry out wet spinning after 10 hours through deaeration, entering concentration by the spun silk of spinning machine is after 20% temperature is 20 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 40 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the sodium sulfite of 15 weight portions, but the pH value of this body lotion is 5, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 100 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the silver oxide of 5 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 3: with milk casein 40 weight portions, soybean protein 10 weight portions, acrylonitrile 45 weight portions, add and contain 5 weight portions, concentration is 5% solder(ing)acid, after stirring, under 90 ℃ temperature, make their mutual swellings 1 hour, then make temperature reduce to 8 ℃, add oxidant potassium peroxydisulfate and reductant potassium bisulfite again, the amount that adds oxidant is 3% of the dried solid amount of acrylonitrile, the reductant addition is 10 times of oxidant, allow above-mentioned substance react 1 hour, carry out graft copolymerization, then left standstill 50 hours, carry out wet spinning after 40 hours through deaeration, entering concentration by the spun silk of spinning machine is after 50% temperature is 10 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 40 ℃ the desalination body lotion and enter desalting processing, the pH value of this body lotion is 3.5, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 100 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the peroxyformic acid of 20 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 4: with milk casein 20 weight portions, soybean protein 40 weight portions, put into the solution that contains 30 parts by weight of acrylonitrile, they are stirred, then in their mixed liquor, add again and contain 10 weight portions, concentration is 10% solder(ing)acid, after stirring, they were dissolved 3 hours mutually, then make temperature reduce to 20 ℃, add oxidant sodium peroxydisulfate and reductant potassium sulfite again, the addition of oxidant is 2% of the dried solid amount of acrylonitrile, the addition of reductant is 15 times of oxidant content, allow above-mentioned substance react again 2 hours, carry out graft copolymerization, then left standstill 40 hours, carry out wet spinning after 30 hours through deaeration, entering concentration by the spun silk of spinning machine is 30%, temperature be 30 ℃ contain zinc chloride solidify solution after, enter temperature again and be in 50 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the sodium hydrogensulfite of 20 weight portions, but this body lotion still is acid, and its pH value is 4.5, and the fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 90 ℃ the neutral hot water and wash, the fiber after washing is drying again, be finished product after the typing.
Embodiment 5: with milk casein 15 weight portions, soybean protein 30 weight portions, acrylonitrile 43 weight portions, add and contain 12 weight portions, concentration is 8% solder(ing)acid, after stirring, under 80 ℃ temperature, make their mutual swellings 4 hours, then make temperature reduce to 40 ℃, add oxidant ammonium persulfate and reductant sodium sulfite again, the amount that adds oxidant is 5% of the dried solid amount of acrylonitrile, the reductant addition is 4 times of oxidant, allow above-mentioned substance react 1.5 hours, carry out graft copolymerization, then left standstill 20 hours, carry out wet spinning after 25 hours through deaeration, entering concentration by the spun silk of spinning machine is after 40% temperature is 15 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 30 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the calcium oxide of 10 weight portions, the pH value of this body lotion is 3.1, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 80 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the potassium hydroxide of 10 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 6: with milk casein 30 weight portions, soybean protein 15 weight portions, acrylonitrile 47 weight portions, add and contain 8 weight portions, concentration is 5% solder(ing)acid, after stirring, under 75 ℃ temperature, make their mutual swellings 5 hours, then make temperature reduce to 30 ℃, add oxidant potassium peroxydisulfate and reductant sodium hydrogensulfite again, the amount that adds oxidant is 1.5% of the dried solid amount of acrylonitrile, the reductant addition is 8 times of oxidant, allow above-mentioned substance react 1.5 hours, carry out graft copolymerization, then left standstill 60 hours, carry out wet spinning after 35 hours through deaeration, entering concentration by the spun silk of spinning machine is after 25% temperature is 35 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 40 ℃ the desalination body lotion and enter desalting processing, the pH value of this body lotion is 4.3, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 95 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the potassium borohydride of 15 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 7: with milk casein 10 weight portions, soybean protein 10 weight portions, put into the solution of the acrylonitrile that contains 80 weight portions, they are stirred, then in their mixed liquor, add again and contain 15 weight portions, concentration is 25% solder(ing)acid, after stirring, they were dissolved 0.5 hour mutually, then make temperature reduce to 50 ℃, add oxidant potassium peroxydisulfate and reductant sodium sulfite again, the addition of oxidant is 4% of the dried solid amount of acrylonitrile, the addition of reductant is 6 times of oxidant content, allow above-mentioned substance react again 0.5 hour, carry out graft copolymerization, then left standstill 55 hours, carry out wet spinning after 20 hours through deaeration, entering concentration by the spun silk of spinning machine is 38%, temperature be 5 ℃ contain zinc chloride solidify solution after, enter temperature again and be in 60 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the magnesia of 5 weight portions, the pH value of this body lotion is 2.5, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 100 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the potassium sulfite of 8 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 8: with milk casein 10 weight portions, soybean protein 40 weight portions, acrylonitrile 40 weight portions, add and contain 10 weight portions, concentration is 35% solder(ing)acid, after stirring, under 50 ℃ temperature, make their mutual swellings 6 hours, then make temperature reduce to 15 ℃, add oxidant ammonium persulfate and reductant sodium hydrogensulfite again, the amount that adds oxidant is 1.3% of the dried solid amount of acrylonitrile, the reductant addition is 12 times of oxidant, allow above-mentioned substance react 2 hours, carry out graft copolymerization, then left standstill 65 hours, carry out wet spinning after 35 hours through deaeration, entering concentration by the spun silk of spinning machine is 15%, after temperature is 40 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 70 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the potassium peroxydisulfate of 8 weight portions, but the pH value of this body lotion is 2, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 90 ℃ the neutral hot water and wash, the fiber after washing is drying again, be finished product after the typing.
Embodiment 9: with milk casein 35 weight portions, soybean protein 18 weight portions, put into the solution that contains 40 parts by weight of acrylonitrile, they are stirred, then in their mixed liquor, add again and contain 7 weight portions, concentration is 6% solder(ing)acid, after stirring, they were dissolved 5.5 hours mutually, then make temperature reduce to 5 ℃, add oxidant sodium peroxydisulfate and reductant sodium sulfite again, the addition of oxidant is 2.5% of the dried solid amount of acrylonitrile, the addition of reductant is 7 times of oxidant content, allow above-mentioned substance react again 1.5 hours, carry out graft copolymerization, then left standstill 45 hours, carry out wet spinning after 48 hours through deaeration, entering concentration by the spun silk of spinning machine is 30%, temperature be 25 ℃ contain zinc chloride solidify solution after, enter temperature again and be in 35 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the magnesia of 5 weight portions, the pH value of this body lotion is 1.5, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 98 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the potassium bisulfite of 12 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 10: with milk casein 40 weight portions, soybean protein 40 weight portions, acrylonitrile 20 weight portions, add and contain 15 weight portions, concentration is 55% solder(ing)acid, after stirring, under 85 ℃ temperature, make their mutual swellings 3.5 hours, then make temperature reduce to 45 ℃, add oxidant ammonium persulfate and reductant sodium hydrogensulfite again, the amount that adds oxidant is 3.5% of the dried solid amount of acrylonitrile, the reductant addition is 5 times of oxidant, allow above-mentioned substance react 1 hour, carry out graft copolymerization, then left standstill 15 hours, carry out wet spinning after 20 hours through deaeration, entering concentration by the spun silk of spinning machine is after 45% temperature is 13 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 55 ℃ the desalination body lotion and enter desalting processing, the pH value of desalination body lotion is 5, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 90 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the calcium oxide of 10 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 11: with milk casein 25 weight portions, soybean protein 10 weight portions, acrylonitrile 60 weight portions, add and contain 5 weight portions, concentration is 3% solder(ing)acid, after stirring, under 80 ℃ temperature, make their mutual swellings 7 hours, then make temperature reduce to 25 ℃, add oxidant potassium peroxydisulfate and reductant potassium bisulfite again, the amount that adds oxidant is 4.5% of the dried solid amount of acrylonitrile, the reductant addition is identical with oxidant content, allow above-mentioned substance react 1.5 hours, carry out graft copolymerization, then left standstill 70 hours, carry out wet spinning after 30 hours through deaeration, entering concentration by the spun silk of spinning machine is 5%, after temperature is 18 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 25 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the NaOH of 5 weight portions, the pH value of this body lotion is 3, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 100 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the silver oxide of 3 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 12: with milk casein 18 weight portions, soybean protein 13 weight portions, put into the solution that contains 50 parts by weight of acrylonitrile, they are stirred, then in their mixed liquor, add again and contain 20 weight portions, concentration is 50% solder(ing)acid, after stirring, they were dissolved 7.5 hours mutually, then make temperature reduce to 10 ℃, add oxidant sodium peroxydisulfate and reductant potassium sulfite again, the addition of oxidant is 3% of the dried solid amount of acrylonitrile, the addition of reductant is 3 times of oxidant content, allow above-mentioned substance react again 2 hours, carry out graft copolymerization, then left standstill 35 hours, carry out wet spinning after 45 hours through deaeration, entering concentration by the spun silk of spinning machine is 20%, temperature be 20 ℃ contain zinc chloride solidify solution after, enter temperature again and be in 35 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the potassium hydroxide of 10 weight portions, but this body lotion still is acid, and its pH value is 4, and the fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 95 ℃ the neutral hot water and wash, the fiber after washing is drying again, be finished product after the typing.
Embodiment 13: with milk casein 28 weight portions, soybean protein 33 weight portions, acrylonitrile 38 weight portions, add and contain 11 weight portions, concentration is 30% solder(ing)acid, after stirring, under 55 ℃ temperature, make their mutual swellings 7 hours, then make temperature reduce to 10 ℃, add oxidant ammonium persulfate and reductant sodium sulfite again, the amount that adds oxidant is 0.8% of the dried solid amount of acrylonitrile, the reductant addition is 13 times of oxidant, allow above-mentioned substance react 2 hours, carry out graft copolymerization, then left standstill 10 hours, carry out wet spinning after 2 hours through deaeration, entering concentration by the spun silk of spinning machine is 35%, after temperature is 0 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 45 ℃ the desalination body lotion and enter desalting processing, the pH value of this body lotion is 2.5, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 85 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the NaOH of 5 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 14: with milk casein 33 weight portions, soybean protein 22 weight portions, acrylonitrile 40 weight portions, add and contain 15 weight portions, concentration is 35% solder(ing)acid, after stirring, under 75 ℃ temperature, make their mutual swellings 3 hours, then make temperature reduce to 45 ℃, add oxidant potassium peroxydisulfate and reductant sodium hydrogensulfite again, the amount that adds oxidant is 2% of the dried solid amount of acrylonitrile, the reductant addition is 7 times of oxidant, allow above-mentioned substance react 1 hour, carry out graft copolymerization, then left standstill 60 hours, carry out wet spinning after 5 hours through deaeration, entering concentration by the spun silk of spinning machine is 18%, after temperature is 35 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 15 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the potassium hydroxide of 15 weight portions, but the pH value of this body lotion is 3.5, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 88 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the iron oxide of 8 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 15: with milk casein 13 weight portions, soybean protein 28 weight portions, put into the solution of the acrylonitrile that contains 48 weight portions, they are stirred, then in their mixed liquor, add again and contain 10 weight portions, concentration is 5% solder(ing)acid, after stirring, they were dissolved 1.5 hours mutually, then make temperature reduce to 55 ℃, add oxidant potassium peroxydisulfate and reductant sodium sulfite again, the addition of oxidant is 1% of the dried solid amount of acrylonitrile, the addition of reductant is 9 times of oxidant content, allow above-mentioned substance react again 1.5 hours, carry out graft copolymerization, then left standstill 20 hours, carry out wet spinning after 43 hours through deaeration, entering concentration by the spun silk of spinning machine is 8%, temperature be 28 ℃ contain zinc chloride solidify solution after, enter temperature again and be in 25 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the barium monoxide of 15 weight portions, the pH value of this body lotion is 2, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 90 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the ammonium persulfate of 10 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Embodiment 16: with milk casein 22 weight portions, soybean protein 22 weight portions, acrylonitrile 51 weight portions, add and contain 5 weight portions, concentration is 20% solder(ing)acid, after stirring, under 60 ℃ temperature, make their mutual swellings 6 hours, then make temperature reduce to 35 ℃, add oxidant ammonium persulfate and reductant sodium hydrogensulfite again, the amount that adds oxidant is 2.8% of the dried solid amount of acrylonitrile, the reductant addition is 12 times of oxidant, allow above-mentioned substance react 2 hours, carry out graft copolymerization, then left standstill 50 hours, carry out wet spinning after 40 hours through deaeration, entering concentration by the spun silk of spinning machine is 40%, after temperature is 8 ℃ containing zinc chloride and solidify solution, enter temperature again and be in 30 ℃ the desalination body lotion and enter desalting processing, being added with in the desalination body lotion and doing solid amount is the sodium peroxydisulfate of 10 weight portions, but the pH value of this body lotion is 2, fiber after desalination is done the steam drawing-off again, then enter temperature again and be in 95 ℃ the hot water and wash, being added with in the water lotion and doing solid amount is the potassium hydroxide of 5 weight portions, and the fiber after washing is drying again, be finished product after the typing.
Claims (1)
1. manufacture method that contains the functional fiber of protein and acrylonitrile, be to add in the metal salt solution with the raw material that comprises protein and acrylonitrile, make their graft copolymerization and after maturation, deaeration, spinning, solidify, desalination, drawing-off, washing, drying, curl, cut off and form, it is characterized in that: in desalination body lotion or water lotion, add metal oxide, the metal oxide that adds in the desalination body lotion is calcium oxide, magnesia or barium monoxide, and the metal oxide that adds in water lotion is silver oxide, calcium oxide or iron oxide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2005100174358A CN1837424B (en) | 2005-03-22 | 2005-03-22 | Method for manufacturing functional fiber with protein and acrylonitrile |
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| CN2005100174358A CN1837424B (en) | 2005-03-22 | 2005-03-22 | Method for manufacturing functional fiber with protein and acrylonitrile |
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| CN1837424A CN1837424A (en) | 2006-09-27 |
| CN1837424B true CN1837424B (en) | 2010-10-27 |
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| CN2005100174358A Expired - Fee Related CN1837424B (en) | 2005-03-22 | 2005-03-22 | Method for manufacturing functional fiber with protein and acrylonitrile |
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| CN101173373B (en) * | 2006-11-03 | 2010-05-26 | 邵阳纺织机械有限责任公司 | Method for producing protein fibre filament yarn with PVA or PAN as carrier |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1468986A (en) * | 2003-07-01 | 2004-01-21 | 张建华 | Animal protein and acrylonitrile grafting copolymerizing fiber and its production process |
| CN1478929A (en) * | 2003-07-01 | 2004-03-03 | 郝小生 | Animal and vegetable protein and acrylonitrile grafting copolymerization fiber and its manufacturing method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1468986A (en) * | 2003-07-01 | 2004-01-21 | 张建华 | Animal protein and acrylonitrile grafting copolymerizing fiber and its production process |
| CN1478929A (en) * | 2003-07-01 | 2004-03-03 | 郝小生 | Animal and vegetable protein and acrylonitrile grafting copolymerization fiber and its manufacturing method |
Non-Patent Citations (3)
| Title |
|---|
| JP平3-193947A 1991.08.23 |
| JP特开2001-64879A 2001.03.13 |
| JP特开平5-106106A 1993.04.27 |
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