CN103074700A - Method for preparing filaments and staple fibers by using straw cellulose - Google Patents
Method for preparing filaments and staple fibers by using straw cellulose Download PDFInfo
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- CN103074700A CN103074700A CN2013100477529A CN201310047752A CN103074700A CN 103074700 A CN103074700 A CN 103074700A CN 2013100477529 A CN2013100477529 A CN 2013100477529A CN 201310047752 A CN201310047752 A CN 201310047752A CN 103074700 A CN103074700 A CN 103074700A
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Abstract
The invention discloses a method for preparing filaments and staple fibers by using straw cellulose. The method comprises the steps of: mixing straw cellulose pulp, paraformaldehyde and dimethyl sulfoxide at a certain proportion, stirring for 1-2h at a temperature of 40-70 DEG C, raising the temperature to 120-150 DEG C, continuously stirring for 2-4h until a primrose uniform spinning solution is generated, standing and deaerating for 12-24h; adding the spinning solution in a spinning kettle, metering the spinning solution through a metering pump and spraying out of a spinneret plate, coagulating in a coagulating bath into cellosilk, drawing and then washing residual solvent, winding, dewatering, oiling and drying into filaments; or dewatering, cutting off, oiling and drying into staple fibers. The filaments and the staple fibers which are prepared from the straw cellulose are smooth in surface, good in glossiness and high in breaking strength, and have a complete circular section and a proper elongation, and good moisture absorption, dyeing property and weaving property; and a fabric prepared from the filaments and the staple fibers has better size stability, tear resistance and crease resistance, and has a wide application prospect in fields such as clothing, industrial textiles and functional fibers.
Description
One, technical field:
The present invention relates to a kind of new method for preparing long filament and short silk with stalk cellulose, the stalk cellulose long filament and the short silk that are prepared by this spining technology can be widely used in the fields such as clothes, industrial textiles and functional fibre.
Two, background technology:
Contemporary society, biomass resource has obtained paying close attention to widely as a class renewable resource.Agricultural crop straw is a kind of reproducible biomass resource, and the output of the annual agricultural crop straw of China can reach 700,000,000 tons, and corn, wheat, paddy rice are as the cereal crops of mainly sowing in the world, and the stalk of its generation is but for a long time as offal treatment.Yet along with the continuous progress of science and technology, agricultural crop straw has become one of the abundantest in the world biomass resource.Agricultural crop straw three major polymers: cellulose, hemicellulose and lignin and some other organic substance form, wherein content of cellulose is about 30～50%, the stalk cellulose that will extract from agricultural crop straw can carry out long filament and the short silk that wet spinning prepares stalk cellulose as raw material, for the recycling of stalk cellulose provides wide application prospect.
At present, the system as cellulose solvent comprises N-methylmorpholine oxide water solution, lithium chloride/dimethylacetylamide, thiocyanic acid amine/liquefied ammonia, NaOH/urea, ionic liquid etc.Patent CN1336451A has introduced the preparation method with N-methylmorpholine oxide water solution dissolving cellulos; Patent CN101177792A has introduced with the cellulosic preparation method of ion liquid dissolving; Patent CN1594680A has introduced the preparation method with NaOH/urea dissolving cellulos; Patent CN101550614A has introduced the preparation method with lithium chloride/dimethylacetylamide dissolving cellulos.And the present invention adopts paraformaldehyde/dmso solution system, have that dissolution time is short, the advantages such as degraded do not occur cellulose in course of dissolution, the solvent that can be used as dissolving stalk cellulose prepares spinning solution step of going forward side by side and carries out spinning, is being a revolutionary approach aspect preparation stalk cellulose long filament and the short silk.
Three, summary of the invention:
Technical problem to be solved by this invention is: a kind of method for preparing long filament and short silk with stalk cellulose is provided, and the stalk cellulose long filament and the short silk that are prepared by this spinning process can be widely used in the fields such as clothes, industrial textiles and functional fibre.
The present invention is that the technical scheme that the technical solution problem is taked is:
A kind of method for preparing long filament and short silk with stalk cellulose, its concrete operation step is as follows:
⑴, be that 400～800 straw cellulose pulp is manual or be ground into the granule pulp with pulverizer with the degree of polymerization, with these granule pulps with vacuum drying oven 70 ℃ lower dry 24 hours, make its constant weight;
⑵, straw cellulose pulp, paraformaldehyde and dimethyl sulfoxide (DMSO) are mixed with certain proportion, under 40～70 ℃ temperature conditions, stirred 1～2 hour, then temperature to the 120～150 ℃ continuation that raises was stirred 2～4 hours, until generate flaxen even spinning solution, standing and defoaming 12～24 hours;
⑶, the spinning solution after will leaving standstill carry out wet spinning: spinning solution is joined in the spinning still, and spinning solution measures through measuring pump, from the spinnerets ejection, enters solidificating fiber silk in the coagulating bath;
⑷, above-mentioned filament carry out spinneret draft through winding apparatus, are further to stretch in the first water bath of 20～60 ℃ through excess temperature again, and its draw ratio is controlled at 0.98～1.6; Filament is the remaining solvent of flush away in the second water bath of 30～80 ℃ through excess temperature again;
⑸ the filament of, flush away solvent is namely made stalk cellulose long filament finished product by reeling, dewater, oil, drying; Perhaps the filament of flush away solvent is namely made the short silk of stalk cellulose finished product by dewatering, cut off, oil, drying.
In step ⑴, the content of alpha-cellulose is 80～95% in the described stalk cellulose.
In step ⑵, the weight ratio of described straw cellulose pulp, paraformaldehyde, dimethyl sulfoxide (DMSO) is 6～9:6～9:82～88.
In step ⑶, the temperature of described spinning still is controlled at 30～80 ℃; The specification of described spinnerets is: bore dia 0.1～0.3mm, hole count is 50～500 holes/plate.
In step ⑸, oil at filament, in the drying course, oil bath concentration is 0.1～0.45g/L, and bake out temperature is room temperature～100 ℃, and drying time is 10～24 hours.
Raw materials used all agricultural crop straws such as maize straw, Wheat Straw, straw, bagasse, kaoliang stalk, reed that comprise of stalk cellulose of the present invention.
The prepared stalk cellulose long filament of the present invention and short silk, smooth surface, good luster, fracture strength is high, and (detect according to authoritative testing agency: doing is by force 1.8-2.5cN/dtex, wet is by force 0.8-1.5 cN/dtex), have complete circular section and suitable percentage elongation, hygroscopicity, dyeability and weavability are good, its fabric has good DIMENSIONAL STABILITY, tear resistance, anti-crease property, is with a wide range of applications in fields such as clothes, industrial textiles and functional fibres.Simultaneously, make cellulosic filaments and short silk with stalk, belong to refuse reclamation, turn waste into wealth, production cost is low, and economic benefit, social benefit and obvious environment benefit are the good approach that agricultural wastes effectively utilize.
Four, the specific embodiment:
Below in conjunction with the concrete operations example the present invention is made further explanation and description: these operational instances only are not used in for explanation the present invention and limit the scope of the invention; After having read the content that the present invention narrates, those skilled in the art can do change and modification on the various forms to the present invention, and these equivalent form of values fall within the protection domain that claims of the present invention limit equally.
Embodiment 1:
A kind of method for preparing long filament and short silk with stalk cellulose, its concrete operation step is as follows:
(1), be that 400～800 straw cellulose pulp is manual or be ground into the granule pulp with pulverizer with the degree of polymerization (DP), these granule pulps with vacuum drying ovens under 70 ℃ of temperature conditions dry 24 hours, are made its constant weight.
, by following constituent content batching: be that straw cellulose pulp, paraformaldehyde, the dimethyl sulfoxide (DMSO) of 6:6:88 mixes with weight ratio, and under 40 ℃ temperature conditions, stirred 2 hours, then the temperature to 120 that raises a ℃ continuation was stirred 4 hours, until generate flaxen even spinning solution, standing and defoaming 12 hours;
⑶, above-mentioned spinning solution is carried out wet spinning: spinning solution is joined in the spinning still, and spinning solution measures through measuring pump, sprays from spinnerets, enter solidificating fiber silk in the coagulating bath, wherein, the temperature of spinning still is controlled at 30 ℃, the spinnerets specification is: bore dia 0.1mm, and hole count is 50 holes/plate;
⑷, above-mentioned filament carry out spinneret draft through winding apparatus, are further to stretch in the first water bath of 20 ℃ through excess temperature again, and its draw ratio is controlled at 1.0; Filament is the remaining solvent of flush away in the second water bath of 30 ℃ through excess temperature again;
⑸ the filament of, flush away solvent is namely made stalk cellulose long filament finished product by reeling, dewater, oil, drying; Perhaps the filament of flush away solvent is namely made the short silk of stalk cellulose finished product by dewatering, cut off, oil, drying; Oil at filament, in the drying course, oil bath concentration is 0.25g/L, bake out temperature is 60 ℃, drying time is 18 hours.
Embodiment 2:
A kind of method for preparing long filament and short silk with stalk cellulose, its concrete operation step is as follows:
(1), be that 400～800 straw cellulose pulp is manual or be ground into the granule pulp with pulverizer with the degree of polymerization (DP), these granule pulps with vacuum drying ovens under 70 ℃ of temperature conditions dry 24 hours, are made its constant weight.
, by following constituent content batching: be that straw cellulose pulp, paraformaldehyde, the dimethyl sulfoxide (DMSO) of 7:7:86 mixes with weight ratio, and under 50 ℃ temperature conditions, stirred 1.5 hours, then the temperature to 130 that raises a ℃ continuation was stirred 3 hours, until generate flaxen even spinning solution, standing and defoaming 18 hours;
⑶, above-mentioned spinning solution is carried out wet spinning: spinning solution is joined in the spinning still, spinning solution measures through measuring pump, spray from spinnerets, enter solidificating fiber silk in the coagulating bath, wherein, the temperature of spinning still is controlled at 40 ℃, and the spinnerets specification is: bore dia 0.2mm, and hole count is 250 holes/plate;
⑷, above-mentioned filament carry out spinneret draft through winding apparatus, are further to stretch in the first water bath of 40 ℃ through excess temperature again, and its draw ratio is controlled at 1.3; Filament is the remaining solvent of flush away in the second water bath of 50 ℃ through excess temperature again;
⑸ the filament of, flush away solvent is namely made stalk cellulose long filament finished product by reeling, dewater, oil, drying; Perhaps the filament of flush away solvent is namely made the short silk of stalk cellulose finished product by dewatering, cut off, oil, drying; Oil at filament, in the drying course, oil bath concentration is 0.35g/L, bake out temperature is 80 ℃, drying time is 15 hours.
Embodiment 3:
A kind of method for preparing long filament and short silk with stalk cellulose, its concrete operation step is as follows:
(1), be that 400～800 straw cellulose pulp is manual or be ground into the granule pulp with pulverizer with the degree of polymerization (DP), these granule pulps with vacuum drying ovens under 70 ℃ of temperature conditions dry 24 hours, are made its constant weight.
, by following constituent content batching: be that straw cellulose pulp, paraformaldehyde, the dimethyl sulfoxide (DMSO) of 9:9:82 mixes with weight ratio, and under 70 ℃ temperature conditions, stirred 1.0 hours, then the temperature to 150 that raises a ℃ continuation was stirred 2 hours, until generate flaxen even spinning solution, standing and defoaming 24 hours;
⑶, above-mentioned spinning solution is carried out wet spinning: spinning solution is joined in the spinning still, spinning solution measures through measuring pump, spray from spinnerets, enter solidificating fiber silk in the coagulating bath, wherein, the temperature of spinning still is controlled at 80 ℃, and the spinnerets specification is: bore dia 0.3mm, and hole count is 500 holes/plate;
⑷, above-mentioned filament carry out spinneret draft through winding apparatus, are further to stretch in the first water bath of 60 ℃ through excess temperature again, and its draw ratio is controlled at 1.6; Filament is the remaining solvent of flush away in the second water bath of 80 ℃ through excess temperature again;
⑸ the filament of, flush away solvent is namely made stalk cellulose long filament finished product by reeling, dewater, oil, drying; Perhaps the filament of flush away solvent is namely made the short silk of stalk cellulose finished product by dewatering, cut off, oil, drying; Oil at filament, in the drying course, oil bath concentration is 0.30g/L, bake out temperature is 70 ℃, drying time is 20 hours.
Claims (5)
1. method for preparing long filament and short silk with stalk cellulose, its concrete operation step is as follows:
⑴, be that 400～800 straw cellulose pulp is manual or be ground into the granule pulp with pulverizer with the degree of polymerization, with these granule pulps with vacuum drying oven 70 ℃ lower dry 24 hours, make its constant weight;
⑵, straw cellulose pulp, paraformaldehyde and dimethyl sulfoxide (DMSO) are mixed with certain proportion, under 40～70 ℃ temperature conditions, stirred 1～2 hour, then temperature to the 120～150 ℃ continuation that raises was stirred 2～4 hours, until generate flaxen even spinning solution, standing and defoaming 12～24 hours;
⑶, the spinning solution after will leaving standstill carry out wet spinning: spinning solution is joined in the spinning still, and spinning solution measures through measuring pump, from the spinnerets ejection, enters solidificating fiber silk in the coagulating bath;
⑷, above-mentioned filament carry out spinneret draft through winding apparatus, are further to stretch in the first water bath of 20～60 ℃ through excess temperature again, and its draw ratio is controlled at 0.98～1.6; Filament is the remaining solvent of flush away in the second water bath of 30～80 ℃ through excess temperature again;
⑸ the filament of, flush away solvent is namely made stalk cellulose long filament finished product by reeling, dewater, oil, drying; Perhaps the filament of flush away solvent is namely made the short silk of stalk cellulose finished product by dewatering, cut off, oil, drying.
2. a kind of method for preparing long filament and short silk with stalk cellulose according to claim 1, it is characterized in that: in step ⑴, the content of alpha-cellulose is 80～95% in the described stalk cellulose.
3. a kind of method for preparing long filament and short silk with stalk cellulose according to claim 1, it is characterized in that: in step ⑵, the weight ratio of described straw cellulose pulp, paraformaldehyde, dimethyl sulfoxide (DMSO) is 6～9:6～9:82～88.
4. a kind of method for preparing long filament and short silk with stalk cellulose according to claim 1, it is characterized in that: in step ⑶, the temperature of described spinning still is controlled at 30～80 ℃; The specification of described spinnerets is: bore dia 0.1～0.3mm, hole count is 50～500 holes/plate.
5. a kind of method for preparing long filament and short silk with stalk cellulose according to claim 1, it is characterized in that: in step ⑸, oil at filament, in the drying course, oil bath concentration is 0.1～0.45g/L, bake out temperature is room temperature～100 ℃, and drying time is 10～24 hours.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103806116A (en) * | 2014-02-20 | 2014-05-21 | 胡宏伟 | Viscose staple fiber spinning after-treatment method |
| CN104451949A (en) * | 2014-12-04 | 2015-03-25 | 江苏苏博特新材料股份有限公司 | Method for preparing nanometer cellulose whisker reinforcing polyoxymethylene fibers |
| CN105133134A (en) * | 2015-07-31 | 2015-12-09 | 爱谱诗（苏州）服装有限公司 | Manufacturing technology for wheat straw fiber fabric |
| CN106283267A (en) * | 2016-08-17 | 2017-01-04 | 江苏鸿顺合纤科技有限公司 | A kind of preparation method of the composite fibre for tearing woven fabric conveniently |
| CN108330557A (en) * | 2018-02-07 | 2018-07-27 | 湖州科博信息科技有限公司 | A kind of degradable biological base environment-protection fiber and its preparation process |
| CN109505018A (en) * | 2018-11-29 | 2019-03-22 | 山传雷 | A kind of antibiosis anti-acarien day tea fiber and preparation method thereof |
| CN109576808A (en) * | 2018-11-29 | 2019-04-05 | 山传雷 | A kind of inorganic fire-retarded intelligent temperature adjusting fiber cellulose fiber and preparation method thereof |
| CN110791878A (en) * | 2019-11-06 | 2020-02-14 | 江南大学 | Preparation method of high-adsorbability artificial fiber membrane |
| CN113802202A (en) * | 2021-11-03 | 2021-12-17 | 嘉兴桃原化纤股份有限公司 | Preparation process of environment-friendly regenerated fiber |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103806116A (en) * | 2014-02-20 | 2014-05-21 | 胡宏伟 | Viscose staple fiber spinning after-treatment method |
| CN103806116B (en) * | 2014-02-20 | 2014-12-10 | 胡宏伟 | Viscose staple fiber spinning after-treatment method |
| CN104451949A (en) * | 2014-12-04 | 2015-03-25 | 江苏苏博特新材料股份有限公司 | Method for preparing nanometer cellulose whisker reinforcing polyoxymethylene fibers |
| CN105133134A (en) * | 2015-07-31 | 2015-12-09 | 爱谱诗（苏州）服装有限公司 | Manufacturing technology for wheat straw fiber fabric |
| CN106283267A (en) * | 2016-08-17 | 2017-01-04 | 江苏鸿顺合纤科技有限公司 | A kind of preparation method of the composite fibre for tearing woven fabric conveniently |
| CN108330557A (en) * | 2018-02-07 | 2018-07-27 | 湖州科博信息科技有限公司 | A kind of degradable biological base environment-protection fiber and its preparation process |
| CN109505018A (en) * | 2018-11-29 | 2019-03-22 | 山传雷 | A kind of antibiosis anti-acarien day tea fiber and preparation method thereof |
| CN109576808A (en) * | 2018-11-29 | 2019-04-05 | 山传雷 | A kind of inorganic fire-retarded intelligent temperature adjusting fiber cellulose fiber and preparation method thereof |
| CN109505018B (en) * | 2018-11-29 | 2021-07-16 | 青岛邦特生态纺织科技有限公司 | Antibacterial and anti-mite Tiancha fiber and preparation method thereof |
| CN109576808B (en) * | 2018-11-29 | 2021-08-24 | 青岛邦特生态纺织科技有限公司 | Inorganic flame-retardant intelligent temperature-adjusting cellulose fiber and preparation method thereof |
| CN110791878A (en) * | 2019-11-06 | 2020-02-14 | 江南大学 | Preparation method of high-adsorbability artificial fiber membrane |
| CN110791878B (en) * | 2019-11-06 | 2021-06-22 | 江南大学 | Preparation method of high-adsorbability artificial fiber membrane |
| CN113802202A (en) * | 2021-11-03 | 2021-12-17 | 嘉兴桃原化纤股份有限公司 | Preparation process of environment-friendly regenerated fiber |
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