CN102912475A - Method for preparing high-strength chitosan fiber from multi-component coagulated bath lotion - Google Patents
Method for preparing high-strength chitosan fiber from multi-component coagulated bath lotion Download PDFInfo
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- CN102912475A CN102912475A CN2011102220835A CN201110222083A CN102912475A CN 102912475 A CN102912475 A CN 102912475A CN 2011102220835 A CN2011102220835 A CN 2011102220835A CN 201110222083 A CN201110222083 A CN 201110222083A CN 102912475 A CN102912475 A CN 102912475A
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Abstract
The invention relates to a preparation method for chitosan fiber. The method comprises the following steps: adding solvents such as a diluent and a plasticizer in the preparation process of coagulated bath lotion so as to overcome the defect that the fiber is quick in coagulation, loose in structure, low in strength, unstable in quality in the conventional preparation process; preparing a homogenous transparent chitosan spinning solution with the concentration of 3 to 30 percent by using 2 to 4 percent glacial acetic acid as a solvent; spinning by using a spinning machine; allowing silk extruded by a metering pump to enter a coagulation bath; regulating and controlling a swelling, dispersion, neutralization, salt precipitation and plasticizing reaction process and the fiber forming molecule orientation of the spinning solution in the coagulation bath by using the coagulated bath lotion which adopts sodium hydroxide as a basic neutralizing agent and adding sodium sulfate, ethanol and dibutyl phthalate (DBP) according to a certain ratio to serve as a salting-out agent, a diluent and a plasticizer respectively; and stretching, washing with water, washing with alcohol and drying to obtain the high-strength chitosan fiber.
Description
Technical field
The invention belongs to biological fiber material preparation technical field, be specifically related to a kind of preparation method of chitin fiber, particularly a kind of about use the preparation method of Chitosan Fiber With High Tenacity with multicomponent coagulation bath production weaving
Background technology
Chitin fiber is take shitosan powder or cotton-shaped tablet as main raw material, adopts suitable solvent, prepares suitable spinning solution, through the spray silk, solidify, stretch, wash, the operation such as drying makes.Because fiber itself has good physiological hygiene and antibiotic and sterilizing function, begin in recent years to be applied in high-end functionality textiles development aspect, domestic some university, scientific research institutions and relevant enterprise have been done many research and development and pilot scale successively, obtained many achievements, its technology of preparing is study hotspot and the forward position of current new material technology field.Chinese patent CN94116666.X, CN95119358.9, CN96103888.8, CN01131634.9, CN200810015053.5 etc. are the patents about chitin fiber and preparation method thereof.In these inventions, all relate to the operations such as chitosan solution preparation, spray silk, coagulating bath, stretching, washing, but all clearly propose preparation high strength, be fit to the chitin fiber needs multicomponent coagulation bath of weaving usefulness, do not mention that also each component of coagulation bath is in the effect of fiber process of setting and on the impact of fibre strength.Yet this is problem needing to overcome in the industrialization production, when body lotion prepares, add the functional components such as a certain proportion of sustained release agent, salting-out agents, plasticizer and can effectively control spinning solution swelling, diffusion in coagulating tank, the course of reaction that neutralizes, saltouts, plastifies and fibroblast molecularly oriented, make the chitin fiber of high strength, suitable weaving usefulness.
The basic components of solidification liquid is about 5% NaOH solution, and the neutralization of the acid in itself and the spinning solution thread causes fiber to separate out and solidify, and common coagulation bath only has NaOH, thus solidify very fast, loosely organized, intensity difference.
Slowly-releasing: add the medicament with diluting effect in the coagulation bath, such as ethanol do not participate in chemical reaction in coagulating bath, only play diluting effect, affect chitosan molecule swelling, diffusion process, the delayed coagulation time, be conducive to form finer and closely woven fibre structure.
Saltout: add the medicament with the function of saltouing in the coagulating bath, such as Na2SO4, a kind of strong electrolyte, it can make the large molecule in the stoste thread solidify because of desolventizing, and freezing action is slower.When Na2SO4 adds when an amount of, salting out strengthens, make curing condition become comparatively gentle, prolong hardening time, during stretching, though gel strand solvation, but completion of cure not yet, have larger stretching plastic, in drawing process, can obtain better molecularly oriented, the mechanical property of fiber is improved.
Plasticising: add the medicament with plasticising function in the coagulating bath, such as DBP, its molecule is inserted between the polymer molecular chain, weakened the stress of polymer molecule interchain, increase the mobility of polymer molecular chain, reduced the degree of crystallinity of polymer molecular chain, changed chemical constitution and the physical arrangement of polymer, thereby the plasticity of polymer is increased, and namely TENSILE STRENGTH improves.
Summary of the invention
For the problem that exists in the actual production process, the present invention proposes a kind of preparation method of chitin fiber, use the method can effectively control spinning solution swelling, diffusion in coagulating tank, the course of reaction that neutralizes, saltouts, plastifies and fibroblast molecularly oriented, make the chitin fiber of high strength, suitable weaving usefulness.。Implementation step comprises: preparation of spinning solution, dissolving, filtration, deaeration, measuring pump metering, spray silk, be frozen into silk, stretching, washing, alcohol wash, oil, drying.Implementation is as follows:
The first step, the dissolving of chitosan solution, in the spinning material of chitin fiber, high-purity chitosan powder (or flocculus material) accounts for percentage by weight 3-30%, solvent glacial acetic acid aqueous solution weight is 2-4%, solubilizer, thinner, defoamer are an amount of, and raw material drops in the deionized water successively, start mixer, mixing speed 40-200 rev/min, stirred 1-8 hour.
Second step, middle press filtration, reactor pressure is controlled at below the 1MPa, double-filtration, filter stainless steel 400-800 order.
The 3rd step, the vacuum stirring deaeration, vacuum tank vacuum 95%, mixing speed 40-200 rev/min, a spinning solution high position enters tank, 2-8 hour deaeration time.
The 4th step, metering spray silk, with measuring pump control spray silk speed and initial titre, spray silk liquid immerses coagulating tank.
The 5th step, solidify, spinning solution is coagulating bath in-tank-solidification and preliminary the stretching.
Step after the 6th step reached, the treatment process such as the stretching of the wet spinning that employing is ripe, washing, drying can make Chitosan Fiber With High Tenacity.
The present invention compared with prior art has the following advantages:
1, the interlinkage degree is high between chitosan molecule, fibre strength is large, and single fiber is done fracture strength and is higher than 2.5cn.
2, fiber is even, high conformity, and the line density deviation ratio is less than 6%.
3, fiber plasticity improves good springiness, and elongation at break is greater than 20%.
Embodiment
Embodiment 1
Get the 600KG deionized water and add reactor, start and stir, drop into 20KG shitosan powder, drop into successively an amount of glacial acetic acid, urea, zinc acetate, silicone oil, stirred 4 hours at 20 ℃, namely get the uniform shitosan spinning solution of dissolving; Utilize filter pressure filtration, pressure is controlled at below the 1MPa, filter stainless steel 600 orders.Filtrate enters the vacuum defoamation tank from tank deck, and vacuum tank vacuum 95% stirs 4 hours deaeration time; Slurries after the deaeration are pumped to spinning head with metering, spinning head 4000 holes, coagulating bath is the aqueous solution of NaOH, sodium sulphate and ethanol, the content of NaOH is 4%, the content of sodium sulphate is 2%, and the content of ethanol is that 4%, DBP content is about 5/10000ths, coagulation bath temperature is 20 ℃, the stretching ratio 1.5 of fiber is after the stretching, at normal temperatures, carry out successively deionization washing, alcohol wash, oil, drying, namely make chitin fiber, fibre number 1.8dtex, intensity＞2.5CN/dtex,, can be used for spinning, nonwoven fabric etc.
Embodiment 2
Get the 300KG deionized water and add reactor, start and stir, drop into successively 30KG shitosan tablet, drop into successively an amount of glacial acetic acid, urea, zinc acetate, silicone oil, stirred 4 hours at 20 ℃, namely get the uniform shitosan spinning solution of dissolving; Utilize filter pressure filtration, pressure is controlled at below the 1MPa, filter stainless steel 800 orders.Filtrate enters the vacuum defoamation tank from tank deck, and vacuum tank vacuum 95% stirs 6 hours deaeration time; Slurries after the deaeration are pumped to spinning head with metering, spinning head 6000 holes, coagulating bath is the aqueous solution of NaOH, sodium sulphate and ethanol, the content of NaOH is 4%, the content of sodium sulphate is 3%, and the content of ethanol is that 4%, DBP content is about 5/10000ths, coagulation bath temperature is 20 ℃, the stretching ratio 1.6 of fiber is after the stretching, at normal temperatures, carry out successively deionization washing, alcohol wash, oil, drying, namely make chitin fiber, fibre number 2.2dtex, intensity＞2.5CN/dtex,, can be used for spinning, nonwoven fabric etc.
Claims (7)
1. the preparation method of a chitin fiber, add high-purity chitosan powder (or flocculus material) under the normal temperature and account for percentage by weight 3-30%, solvent glacial acetic acid aqueous solution weight is 2-4%, solubilizer, thinner, defoamer is an amount of, raw material drops in the deionized water successively, start mixer, mixing speed 40-200 rev/min, stirred 1-4 hour, with static pressure with twice of solution press filtration, send into vacuum tank and stir deaeration 2-4 hour, obtain the shitosan spinning solution that concentration is about the homogeneous phase transparent of 3-30%, adopt the spinning machine spinning, the silk that measuring pump is extruded enters coagulating tank, and coagulation bath is NaOH, the aqueous solution of sodium sulphate and ethanol, the content of NaOH are 4-8%, the content of sodium sulphate is 2-6%, the content of ethanol is 4-8%, DBP content is ten thousand/to 8/10000ths, by stretching, washing, alcohol wash, oil, drying obtains Chitosan Fiber With High Tenacity.
2. the preparation method of chitin fiber according to claim 1 is characterized in that, the molecular weight of described chitosan powder (or flocculus material) is greater than 800,000, and viscosity is at 20 ℃ of time＞500mpa.s of normal pressure, deacetylation＞85%, and purity is greater than 99%.
3. the preparation method of chitin fiber according to claim 1 is characterized in that, when dissolving chitosan powder (or flocculus material), adds a certain proportion of solubilizer, thinner, defoamer.
4. the preparation method of chitin fiber according to claim 1 is characterized in that, when filtering chitosan solution, is pressurized to 0.3-0.5Mpa with air compressor machine, makes solution with pressure by filter, filter 400-800 order.
5. the preparation method of chitin fiber according to claim 1 is characterized in that, the chitosan solution after the filtration enters the vacuum defoamation of negative pressure storage tank, tank internal pressure＜76mmHG.
6. the preparation method of chitin fiber according to claim 1, it is characterized in that, adopt the spinning machine spinning, the silk that measuring pump is extruded enters coagulating tank, coagulation bath is take NaOH as basic neutralizer, add a certain proportion of sodium sulphate, ethanol, DBP respectively as salting-out agents, diluent, plasticizer, swelling, the diffusion in coagulating tank of regulation and control spinning solution, the course of reaction that neutralizes, saltouts, plastifies and fibroblast molecularly oriented.
7. the preparation method of chitin fiber according to claim 1 is characterized in that, by stretching, washing, alcohol wash, oil, drying obtains Chitosan Fiber With High Tenacity.
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| CN2011102220835A CN102912475A (en) | 2011-08-04 | 2011-08-04 | Method for preparing high-strength chitosan fiber from multi-component coagulated bath lotion |
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| CN2011102220835A CN102912475A (en) | 2011-08-04 | 2011-08-04 | Method for preparing high-strength chitosan fiber from multi-component coagulated bath lotion |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104389050A (en) * | 2014-11-28 | 2015-03-04 | 湖北中烟工业有限责任公司 | Production method of chitosan fiber tobacco tow |
| CN104562293A (en) * | 2013-10-22 | 2015-04-29 | 成立萍 | Preparation method for water-locking chitosan fibers |
| CN109576803A (en) * | 2018-10-18 | 2019-04-05 | 青岛即发集团股份有限公司 | A kind of production method of chitin fiber |
| CN112952215A (en) * | 2021-01-31 | 2021-06-11 | 复旦大学 | Water-based fiber battery and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6059123A (en) * | 1983-09-12 | 1985-04-05 | Fuji Boseki Kk | Production of chitosan fiber |
| WO1996025538A1 (en) * | 1995-02-14 | 1996-08-22 | Chisso Corporation | Biodegradable fiber and nonwoven fabric |
| CN1261111A (en) * | 2000-01-14 | 2000-07-26 | 东华大学 | Antibacterial fibres containing chitin and its derivatives, and preparing process thereof |
| US6235816B1 (en) * | 1995-04-07 | 2001-05-22 | Biotec Biologische Naturverpackungen Gmbh | Compositions and methods for manufacturing thermoplastic starch blends |
| CN102002764A (en) * | 2010-12-28 | 2011-04-06 | 天津市东南恒生医用科技有限公司 | Spinning method and post-treating process of biodegradable aliphatic polyester medical fibre |
-
2011
- 2011-08-04 CN CN2011102220835A patent/CN102912475A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6059123A (en) * | 1983-09-12 | 1985-04-05 | Fuji Boseki Kk | Production of chitosan fiber |
| WO1996025538A1 (en) * | 1995-02-14 | 1996-08-22 | Chisso Corporation | Biodegradable fiber and nonwoven fabric |
| US6235816B1 (en) * | 1995-04-07 | 2001-05-22 | Biotec Biologische Naturverpackungen Gmbh | Compositions and methods for manufacturing thermoplastic starch blends |
| CN1261111A (en) * | 2000-01-14 | 2000-07-26 | 东华大学 | Antibacterial fibres containing chitin and its derivatives, and preparing process thereof |
| CN102002764A (en) * | 2010-12-28 | 2011-04-06 | 天津市东南恒生医用科技有限公司 | Spinning method and post-treating process of biodegradable aliphatic polyester medical fibre |
Non-Patent Citations (3)
| Title |
|---|
| 别亚琴等: "高强度壳聚糖纤维的制备和应用进展", 《化纤与纺织技术》 * |
| 李达: "壳聚糖纤维生产关键技术的研究", 《青岛大学硕士学位论文》 * |
| 贾继阳等: "壳聚糖纤维的制备、性能及在非织造材料中的应用", 《广西纺织科技》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104562293A (en) * | 2013-10-22 | 2015-04-29 | 成立萍 | Preparation method for water-locking chitosan fibers |
| CN104562293B (en) * | 2013-10-22 | 2017-05-17 | 成立萍 | Preparation method for water-locking chitosan fibers |
| CN104389050A (en) * | 2014-11-28 | 2015-03-04 | 湖北中烟工业有限责任公司 | Production method of chitosan fiber tobacco tow |
| CN109576803A (en) * | 2018-10-18 | 2019-04-05 | 青岛即发集团股份有限公司 | A kind of production method of chitin fiber |
| CN109576803B (en) * | 2018-10-18 | 2023-09-12 | 青岛即发集团股份有限公司 | Production method of chitosan fiber |
| CN112952215A (en) * | 2021-01-31 | 2021-06-11 | 复旦大学 | Water-based fiber battery and preparation method thereof |
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Application publication date: 20130206 |