CN1203965A - Method for manufacturing pupa protein viscose filament rayon - Google Patents
Method for manufacturing pupa protein viscose filament rayon Download PDFInfo
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- CN1203965A CN1203965A CN 97107800 CN97107800A CN1203965A CN 1203965 A CN1203965 A CN 1203965A CN 97107800 CN97107800 CN 97107800 CN 97107800 A CN97107800 A CN 97107800A CN 1203965 A CN1203965 A CN 1203965A
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Abstract
The present invention relates to a textile material-pupa protein viscose filament rayon and its manufacturing method. Said invention uses pupa protein spinning solution and cellulose xanthate solution, and adopts the procedures of static mixing and solution injection to make spinning to obtain the pupa protein viscose filament rayon with real silk property. Its main raw materials are pulp, pupa protein, sulfuric acid, caustic soda, carbon bisulfide, formaldehyde and acrylamide. Said invented product is soft and possesses gold-yellow colour.
Description
The present invention relates to a kind of material manufacturing method of textile industry.
Silk fabrics is merrily and lightheartedly soft, gloss is quiet and tastefully laid out, good hygroscopicity, comfortable and easy to wear, be subjected to domestic and international consumer's welcome deeply, but owing to produce the raw material-silk shortage of silk fabrics, can not satisfy the needs of people life, people then seek a kind of raw material that replaces silk once developed regenerated protein abroad, with milk casein, soybean protein, peanut protein and zein raw material, all eliminated by other fibers because of wet strength is too low.China has a large amount of silkworm chrysalises, and as the waste material of silk weaving, great majority are used for feed and fertilizer.And contain a large amount of available native proteins in the silkworm chrysalis, people utilize silkworm chrysalis to extract pupa protein production food, tonic beverage, compound amino acid in the prior art.
Patent Office of the People's Republic of China discloses the invention that application number is 95111328.3 " silkworm chrysalis albumen composite long fibre and manufacture method thereof " on March 20th, 1996, the present inventor finds that this prior art has defective on the implementation, at first, application number be in claims of 95111328.3 invention the 2nd described: " ... it is characterized in that proportioning is pupa albumen 30%-35%; viscose glue 55%-65%, acryloyl ammonium 10%-15%." as in this ratio; can't realize the purpose that it reels off raw silk from cocoons in force, and described with self the 3rd (1) of claims: " ... pupa albumen: acrylamide is 1: 0.1-0.15...... " and (2) described " ... pupa albumen: viscose glue is 1: 2-2.5...... " are contradictory at all.So at application number is the root problem that 95111328.3 " silkworm chrysalis albumen composite long fibre and manufacture method thereof " do not solve this technology.
The object of the present invention is to provide a kind of utilize silkworm chrysalis albumen spinning solution and the spinning of cellulose xanthate solution blending, make the manufacture method of pupa albumen viscose filament yarn with real silk performance.
Main raw material of the present invention is pupa albumen, sulfuric acid, caustic soda, carbon disulfide, formaldehyde, acrylamide, the cotton pulp dregs of rice, carbon disulfide.
A kind of method for manufacturing pupa protein viscose filament rayon: get certain proportion pupa albumen and NaOH by the solid weight ratio, it is 45-50 ℃ that pupa albumen is dissolved in temperature, concentration is in the sodium hydrate aqueous solution of 1.2-2%, obtain pupa albumen solution after filtration, after the hydrogen peroxide of adding 0.5-1 ‰ causes in the pupa albumen solution of uniform temperature, get pupa albumen by the solid weight ratio again: acrylamide is 1: 0.1-0.15 adds acrylamide, carries out obtaining silkworm chrysalis albumen spinning solution after filtration behind the carbamyl ethylation reaction; Silkworm chrysalis albumen spinning solution and rayon spinning liquid carried out static mixing after the deaeration respectively by a certain percentage and spin before injection carry out spinning, through contains sodium sulfate 250-360g/L, sulfuric acid 80-130g/L, zinc sulfate 10-50g/L, proportion is 1.25-1.32, temperature is behind 45-55 ℃ the coagulating bath coagulation forming, to obtain fiber; The spinning cake of spinning is used by containing formaldehyde 25-50g/L, sulfuric acid 7-25g/L, the hydroformylation liquid of sodium sulphate 130-230g/L carries out hydroformylation to be handled 1-3 hour, and above-mentioned fiber is again through overpickling, desulfurization, washing, pickling, obtain pupa protein viscose filament rayon after washing, oil, dewater, drying.
The pupa albumen long filament of making, fiber number are 131-136dtex, and dried fracture strength is 1.3-1.8CN/dtex, dried elongation at break 15-25%, wet breaking strength 0.6-0.9CN/dtex, dyeing uniformity 2.5-4.0 level, regain 10-15%, the strand softness, it is golden yellow that color and luster is.
Pupa albumen long filament of the present invention integrates the advantage of real silk and viscose filament yarn, and its hygroscopicity, dyeability are better than real silk, and COLOR FASTNESS, the straightforward real silk that is better than that dangles, and is soft, is easy to processing.
Pupa albumen viscose filament yarn manufacture method provided by the invention turns waste into wealth silkworm chrysalis, has made full use of China's protein resource, has promoted COMPREHENSIVE UTILIZATION OF SILKWORM CHRYSALIS, for cheap and good-quality field of new has been opened up in textile industry.
Below with embodiment the present invention is further described:
Embodiment 1:
5kg NaOH is dissolved in 250 liters of soft water, makes 2% sodium hydroxide solution, this solution is heated to 45 ℃, get the 60kg pupa albumen and put into 45 ℃ of soft water rinsings, albumen powder 122kg must wet after filter is done.The albumen powder that will wet drops into above-mentioned sodium hydroxide solution, the limit edged is stirred to dissolving fully, make pupa albumen liquid, again by solid weight than pupa albumen: acrylamide is to add the 8kg acrylamide at 1: 0.13, add the 500ml hydrogen peroxide simultaneously and make initator, carry out the carbamyl ethylation reaction, control reaction temperature is 45 ℃, reaction time is 5 hours, is that 1.054 solid contents are 15.4% silkworm chrysalis albumen spinning solution with making proportion behind the solution process filtration free from admixture.Above-mentioned albumen spinning solution is after deaeration, in albumen: cellulose is that 1: 2 ratio is carried out direct fabrics after the static mixing with albumen spinning solution and viscose glue.Cellulosic making by the cotton pulp dregs of rice at 50 ± 1 ℃, the maceration extract of the dense 240 ± 0.8g/l of alkali floods after squeeze, pulverize, the experienced alkali cellulose of making, the latter and carbon disulfide reaction generate cellulose xanthate, make cellulose xanthate solution with the sig water dissolving, the step of going forward side by side is carried out maturation, filters, deaeration, spraying silk with the PN12-30-0.08 shower nozzle, spin 67 meters/minute of speed, coagulation bath temperature is 48 ℃, and proportion is 1.30, sulfuric acid 100g/l, sodium sulphate 310g/l, zinc sulfate 30g/l, the spinning cake of making carry out acetalation again to be handled 2 hours, hydroformylation liquid consists of formaldehyde 30g/l, sulfuric acid 10g/l, sodium sulphate 180g/l, temperature is 30 ℃, spinning cake after hydroformylation is handled is again through desulfurization, washing, pickling, washing, oil, pupa protein viscose filament rayon is made in oven dry, and it is light yellow that color and luster is.
Embodiment 2:
5kg NaOH is dissolved in 230 liters of soft water, is heated to 45 ℃, with the rinsing in 40 ℃ of soft water of 70kg pupa albumen, albumen powder 141kg must wet after filter is done.Put in the above-mentioned sodium hydroxide solution, the limit edged stirs, and heating-up temperature rises to 60 ℃, after two hours, albumen is dissolved in sodium hydroxide solution fully, after be cooled to 48 ℃, add the 250ml hydrogen peroxide and cause, simultaneously by solid weight than pupa albumen: acrylamide is 1: 0.13 adding 9KG acrylamide, carried out the carbamyl ethylation reaction 5 hours, behind the multiple times of filtration free from admixture, making proportion is 1.066, and solid content is 19.1% silkworm chrysalis albumen spinning solution.This albumen spinning solution is after deaeration, in albumen: cellulose is that 1: 2.2 ratio and viscose glue carries out carrying out spinning after the static mixing.Cellulosic making as described in the embodiment 1.With PN12-30-0.08 shower nozzle spray silk, spin 67 meters/minute of speed again, coagulation bath temperature is 51 ℃, proportion is 1.28, sulfuric acid 90g/l, sodium sulphate 285g/l, zinc sulfate 20g/l, the spinning cake of making carries out acetalation again to be handled 2 hours, and hydroformylation liquid consists of formaldehyde 34g/l, sulfuric acid 10g/l, sodium sulphate 200g/l, temperature is 35 ℃, the spinning cake after hydroformylation is handled again through desulfurization, washing, pickling, wash, oil, dry and make pupa protein viscose filament rayon, it is light yellow that color and luster is.
Embodiment 3:
4.5kg NaOH is dissolved in 220 liters of soft water, is heated to 40 ℃, get the rinsing in 50 ℃ of soft water of 65kg pupa albumen, albumen powder 130kg must wet after filter is done.It is put in the above-mentioned sodium hydroxide solution, stir while throwing, be heated to 60 ℃ simultaneously, after two hours, albumen is dissolved in the sodium hydroxide solution fully, the protein liquid temperature is reduced to 45 ℃, add 500ml hydrogen peroxide, 6.5kg acrylamide, carry out the carbamyl ethylation reaction, filter after 3 hours, making proportion is 1.055, and solid content is 16.7% albumen spinning solution.This protein liquid after deaeration under the 600mmHg vacuum, after the deaeration by albumen: cellulose is to carry out spinning after 1: 2.1 the mixed.Cellulosic making as described in the embodiment 1.Again with PN12-30-0.08 shower nozzle spray silk, coagulation bath composition: sulfuric acid 95g/l, sodium sulphate 285g/l, zinc sulfate 25g/l, 50 ℃ of temperature, proportion 1.28; The spinning cake that makes carries out acetalation again to be handled 2 hours, and hydroformylation liquid consists of formaldehyde 35g/l, sulfuric acid 8g/l, sodium sulphate 160g/l, again through desulfurization, pickling, oil, dry and make pupa protein viscose filament rayon, it is light yellow that color and luster is.
Claims (1)
1, a kind of method for manufacturing pupa protein viscose filament rayon: get certain proportion pupa albumen and NaOH by the solid weight ratio, it is 45-50 ℃ that pupa albumen is dissolved in temperature, concentration is in the sodium hydrate aqueous solution of 1.2-2%, obtain pupa albumen solution after filtration, after the hydrogen peroxide of adding 0.5-1 ‰ causes in the pupa albumen solution of uniform temperature, get pupa albumen by the solid weight ratio again: acrylamide is 1: 0.1-0.15 adds acrylamide, carries out obtaining silkworm chrysalis albumen spinning solution after filtration behind the carbamyl ethylation reaction; Silkworm chrysalis albumen spinning solution and rayon spinning liquid carried out static mixing after the deaeration respectively by a certain percentage and spin before injection carry out spinning, through contains sodium sulfate 250-360g/L, sulfuric acid 80-130g/L, zinc sulfate 10-50g/L, proportion is 1.25-1.32, temperature is behind 45-55 ℃ the coagulating bath coagulation forming, to obtain fiber; The spinning cake of spinning is used by containing formaldehyde 25-50g/L, sulfuric acid 7-25g/L, the hydroformylation liquid of sodium sulphate 130-230g/L carries out hydroformylation to be handled 1-3 hour, and above-mentioned fiber is again through overpickling, desulfurization, washing, pickling, obtain pupa protein viscose filament rayon after washing, oil, dewater, drying.It is characterized in that:
A, pupa albumen and NaOH ratio are 1: 0.06-0.15;
B, carbamyl ethylation reaction temperature are 40-55 ℃;
C, in albumen: cellulose is that 1: 2～2.2 ratio is mixed albumen spinning solution with viscose glue; The solid content of silkworm chrysalis albumen spinning solution is 15.4%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97107800A CN1061107C (en) | 1997-12-01 | 1997-12-01 | Method for manufacturing pupa protein viscose filament rayon |
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| CN97107800A CN1061107C (en) | 1997-12-01 | 1997-12-01 | Method for manufacturing pupa protein viscose filament rayon |
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| CN1203965A true CN1203965A (en) | 1999-01-06 |
| CN1061107C CN1061107C (en) | 2001-01-24 |
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| CN101962822A (en) * | 2010-11-05 | 2011-02-02 | 四川省宜宾惠美线业有限责任公司 | Method for manufacturing wood pupa protein viscose filament yarns |
| CN101974800A (en) * | 2010-11-05 | 2011-02-16 | 四川省宜宾惠美线业有限责任公司 | Method for manufacturing wood-pupa protein viscose staple fibers |
| CN102304782A (en) * | 2011-09-26 | 2012-01-04 | 四川省宜宾惠美线业有限责任公司 | Pupal protein viscose staple fiber and manufacturing method thereof |
| CN102383219A (en) * | 2011-09-26 | 2012-03-21 | 四川省宜宾惠美线业有限责任公司 | Pupal protein-viscose filament and manufacturing method thereof |
| CN101718007B (en) * | 2009-11-26 | 2012-05-02 | 郭筱洁 | Production method of regenerated fibroin fiber |
| CN102851787A (en) * | 2012-08-24 | 2013-01-02 | 宜宾丝丽雅股份有限公司 | Preparation method of pupa protein cellulose composite viscose staple fiber spinning solution |
| CN103266406A (en) * | 2012-05-24 | 2013-08-28 | 浙江真爱时尚家居有限公司 | Manufacturing technique of pupa protein silk fiber Raschel blanket |
| CN104005114A (en) * | 2014-05-05 | 2014-08-27 | 江苏金太阳布业有限公司 | Preparation method for wool keratin regenerated cellulose fiber |
| CN104963015A (en) * | 2015-06-09 | 2015-10-07 | 苏州威尔德工贸有限公司 | Sandwiched molybdenum disulfide/ silkworm pupa protein fiber |
| CN105821518A (en) * | 2016-05-13 | 2016-08-03 | 东莞市联洲知识产权运营管理有限公司 | Silkworm pupa protein/lotus cellulose composite fibers and preparing method thereof |
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Families Citing this family (2)
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| CN100554536C (en) * | 2006-08-04 | 2009-10-28 | 宜宾丝丽雅股份有限公司 | A kind of bamboo pupa protein fiber long, short silk and preparation method thereof |
| CN101298708B (en) * | 2008-06-25 | 2010-06-02 | 宜宾丝丽雅集团有限公司 | Protein cellulose viscose and preparing method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6059175A (en) * | 1983-09-02 | 1985-04-05 | 三菱レイヨン株式会社 | Silk modifying method |
| JPH0711576A (en) * | 1993-06-21 | 1995-01-13 | Toyobo Co Ltd | Yarn degradable in soil |
| CN1118820A (en) * | 1995-04-24 | 1996-03-20 | 四川三线经济技术联合发展总公司 | Silkworm chrysalis albumen composite long fibre and its production method |
| CN1044627C (en) * | 1995-04-25 | 1999-08-11 | 谯续俊 | Pupa albumen for spinning and its producing method |
| CN1040558C (en) * | 1995-05-16 | 1998-11-04 | 四川三线经济技术联合发展总公司 | Silkworm chrysalis albumen spinning solution and making method thereof |
-
1997
- 1997-12-01 CN CN97107800A patent/CN1061107C/en not_active Expired - Lifetime
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| CN101718007B (en) * | 2009-11-26 | 2012-05-02 | 郭筱洁 | Production method of regenerated fibroin fiber |
| CN101974800A (en) * | 2010-11-05 | 2011-02-16 | 四川省宜宾惠美线业有限责任公司 | Method for manufacturing wood-pupa protein viscose staple fibers |
| CN101962822B (en) * | 2010-11-05 | 2011-12-07 | 四川省宜宾惠美线业有限责任公司 | Method for manufacturing wood pupa protein viscose filament yarns |
| CN101962822A (en) * | 2010-11-05 | 2011-02-02 | 四川省宜宾惠美线业有限责任公司 | Method for manufacturing wood pupa protein viscose filament yarns |
| CN102304782A (en) * | 2011-09-26 | 2012-01-04 | 四川省宜宾惠美线业有限责任公司 | Pupal protein viscose staple fiber and manufacturing method thereof |
| CN102383219A (en) * | 2011-09-26 | 2012-03-21 | 四川省宜宾惠美线业有限责任公司 | Pupal protein-viscose filament and manufacturing method thereof |
| CN103266406A (en) * | 2012-05-24 | 2013-08-28 | 浙江真爱时尚家居有限公司 | Manufacturing technique of pupa protein silk fiber Raschel blanket |
| CN102851787A (en) * | 2012-08-24 | 2013-01-02 | 宜宾丝丽雅股份有限公司 | Preparation method of pupa protein cellulose composite viscose staple fiber spinning solution |
| CN102851787B (en) * | 2012-08-24 | 2014-05-14 | 宜宾丝丽雅股份有限公司 | Preparation method of pupa protein cellulose composite viscose staple fiber spinning solution |
| CN104005114A (en) * | 2014-05-05 | 2014-08-27 | 江苏金太阳布业有限公司 | Preparation method for wool keratin regenerated cellulose fiber |
| CN104963015A (en) * | 2015-06-09 | 2015-10-07 | 苏州威尔德工贸有限公司 | Sandwiched molybdenum disulfide/ silkworm pupa protein fiber |
| CN104963015B (en) * | 2015-06-09 | 2017-03-29 | 东莞市联洲知识产权运营管理有限公司 | A kind of molybdenum bisuphide/silkworm protein fiber of sandwich formats |
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| CN106835344A (en) * | 2017-02-20 | 2017-06-13 | 海安县兄弟合成纤维有限公司 | A kind of heat-resistant fireproof fibers material |
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