CN102851790A - Preparation method of producing high-strength chitosan fiber by use of double-screw pump - Google Patents
Preparation method of producing high-strength chitosan fiber by use of double-screw pump Download PDFInfo
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- CN102851790A CN102851790A CN2011101840756A CN201110184075A CN102851790A CN 102851790 A CN102851790 A CN 102851790A CN 2011101840756 A CN2011101840756 A CN 2011101840756A CN 201110184075 A CN201110184075 A CN 201110184075A CN 102851790 A CN102851790 A CN 102851790A
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- preparation
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- spinning
- chitosan
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- 239000000835 fiber Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 18
- 238000009987 spinning Methods 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229960000583 acetic acid Drugs 0.000 claims abstract description 5
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 229920002101 Chitin Polymers 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 5
- 230000001112 coagulating effect Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000010009 beating Methods 0.000 claims 1
- 230000006196 deacetylation Effects 0.000 claims 1
- 238000003381 deacetylation reaction Methods 0.000 claims 1
- 238000001125 extrusion Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 239000012530 fluid Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000004090 dissolution Methods 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000013530 defoamer Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000011085 pressure filtration Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000009941 weaving Methods 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
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- Artificial Filaments (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a preparation method of chitosan fibers, overcomes the shortcomings, such as low solution concentration, long dissolving time, difficult filtering, long defoaming time, instable product quality and low fiber strength, of the chitosan fiber preparation process at present, and adopts 2-5% glacial acetic acid as solvent, where a chitosan tablet raw material is added at a room temperature and stirred for 15-30 min. A double-screw pump is adopted for cyclic delivery for 1 hr, to fully dissolve the preparation, and also used to press-filter the solution and feed it into a vacuum tank for deforming for 2-4 hr to obtain 0.5-30% homogenous-phase transparent chitosan spinning fluid. A spinning machine is adopted for spinning, the yarn extruded by a metering pump enters a condensation bath, and high-strength chitosan fibers are obtained by drawing, water washing, alcohol washing and drying.
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 Quimby pump 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, the operation such as stretching makes.Because it has obvious physiological hygiene and antibacterial action, caused attention at the high-end functionality piece market in recent years, 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 spinning solution dissolving, filtration, deaeration operation, but all clearly propose the high suitable weaving of preparation intensity and need use high concentration, high viscosity chitosan solution with chitin fiber, dissolution time length, the sad filter that runs into when also not mentioning this solution of preparation, the solution that is difficult for the knotty problems such as deaeration.Yet these all are the problems that large-scale production must solve emphatically, and introducing Quimby pump in production procedure can effectively address the above problem.
The operation principle of Quimby pump is: during screw pump work, just enter the seal cavity that screw thread and pump case enclose after liquid is inhaled into, when the active screw rod rotated, the screw pump sealed volume improved screw pump pressure under the extruding of thread, and mobile vertically.Because screw rod is constant speed rotation, also be uniform so liquid flows out flow.
The screw pump characteristics are: the screw pump loss is little, and economic performance is good.Pressure is high, and flow is even and even, and rotating speed is high, can with prime mover direct connection.
Screw pump is applicable to the transfer of highly viscous medium; transport viscosity can be up to 200000 centipoises; medium can contain particle or fiber simultaneously: particle diameter can reach 30mm (being no more than eccentricity of rotor), and fiber length can 350mm (pitch of suitable 0.4 rotor).Its content generally can reach 40% of medium, if when the solids in the medium is trickle powder shape, high-load can reach 60% or highlyer also can carry.
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, dissolution time length, sad filter when the method has overcome the preparation highly concentrated solution, be difficult for the difficult points such as deaeration.Implementation step comprises: spinning solution preparation, spinning solution dissolving, filtration, deaeration, measuring pump metering, spray silk, be frozen into silk, 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 0.5-30%, solvent glacial acetic acid aqueous solution weight is 2-5%, propyl alcohol is 0.5%, defoamer 0.1%, and raw material drops in the deionized water successively, starts mixer, mixing speed 40-200 rev/min, stirred 15-30 minute; Close Quimby pump outlet side strainer valve, open circulating valve, start Quimby pump, 750 rev/mins of rotating speeds, raw material is accelerate dissolution in squeezing broken course of conveying, circular flow 1 hour.
Second step is opened Quimby pump outlet side strainer valve, closes circulating valve, utilize screw pump pressure filtration, filtrate enters the vacuum defoamation tank from top, and pump discharge pressure is controlled at below the 5MPa, filter stainless steel 400-800 order, vacuum tank vacuum 95%, 2-4 hour static deaeration time.
The 3rd step and after step, adopt ripe wet spinning technology, through the spray silk, stretch, washing, the treatment process such as dry, can make Chitosan Fiber With High Tenacity.
The present invention compared with prior art has the following advantages:
1, dissolution time is short, the batching of same volume, and dissolution time only has the 1/6-1/10 of common stirring and dissolving time spent;
2, filtration time is short, the batching of same volume, and filtration time is less than 1/5 of the static pressure plate-type filtering;
3, can filter rapidly high viscosity solution, overcome the difficult point that the static pressure leaf filter can not filter high viscosity solution;
4, be easy to the solution deaeration, high pressing filtering liquid enters vacuum tank, than the easier deaeration of normal pressure solution;
5, save the energy, significantly reduce compressor, vavuum pump working time, save electric energy;
6, reduce water clock, reduce the wastage.
Description of drawings
Accompanying drawing is that dotted line encloses and partly is critical workflow of the present invention and equipment among the figure with the technological process of production schematic diagram of Quimby pump preparation weaving with Chitosan Fiber With High Tenacity, and all devices must be selected the acid and alkali-resistance material.
The specific embodiment
Embodiment 1
Get the 600KG deionized water and add reactor, start and stir, drop into successively 20KG chitosan raw material, 12KG glacial acetic acid, 7KG urea, 5KG glycerol, 7KG defoamer, stirred 15 minutes at 20 ℃, close strainer valve, open circulating valve, start screw pump, turned round 1 hour, and namely got the uniform shitosan spinning solution of dissolving; Open strainer valve, close circulating valve, utilize screw pump pressure filtration, filtrate directly enters the vacuum defoamation tank, and pump discharge pressure is controlled at below the 5MPa, filter stainless steel 600 orders, vacuum tank vacuum 95%, static deaeration time 2 h; Slurries after the deaeration are pumped to spinning head, spinning head aperture 0.04mm, 4000 holes with metering, coagulating bath is the aqueous solution of NaOH and ethanol, and the content of NaOH is 4%, and the content of ethanol is 5%, coagulation bath temperature is 20 ℃, and 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, dimension limit 2dtex, intensity＞2.0CN/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 20KG chitosan raw material, 12KG glacial acetic acid, 7KG urea, 2KG ethanol, 7KG defoamer, stirred 15 minutes at 10 ℃, close strainer valve, open circulating valve, start screw pump, turned round 0.5 hour, and namely got the uniform shitosan spinning solution of dissolving; Open strainer valve, close circulating valve, utilize screw pump pressure filtration, filtrate directly enters the vacuum defoamation tank, and pump discharge pressure is controlled at below the 5MPa, filter stainless steel 800 orders, vacuum tank vacuum 95%, 1 hour static deaeration time; Slurries after the deaeration are pumped to spinning head, spinning head aperture 0.04mm, 4000 holes with metering, coagulating bath is the aqueous solution of NaOH and ethanol, and the content of NaOH is 5%, and the content of ethanol is 5%, coagulation bath temperature is 20 ℃, and the stretching ratio 1.8 of fiber is after the stretching, at normal temperatures, carry out successively deionization washing, alcohol wash, oil, drying, namely make chitin fiber, fiber limit 2.4dtex, intensity＞2.0CN/dtex can be used for spinning, nonwoven fabric etc.
Claims (6)
1. the preparation method of a chitin fiber, adopt the glacial acetic acid solution of 2-5% to make solvent, add mass fraction 0.5-30% shitosan tablet material under the normal temperature, stirred first 15-30 minute, rear beating with Quimby pump circulated 1 hour, utilized screw rod to squeeze broken its quick dissolving that makes; With Quimby pump with the solution press filtration, send into vacuum tank and stir deaeration 2-4 hour, obtain the shitosan spinning solution of the homogeneous phase transparent of concentration 0.5-30%, adopt the spinning machine spinning, the silk that measuring pump is extruded enters coagulating tank, 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 shitosan tablet is greater than 200,000, and viscosity is at 20 ℃ of time＞500mpa.s of normal pressure, deacetylation＞80%.
3. the preparation method of chitin fiber according to claim 1, it is characterized in that, when dissolving shitosan tablet, suck at the bottom of the Quimby pump autoreaction still, output to the reactor top, in pump, utilize the compressional movement of twin-screw that not diffluent particle is squeezed broken dissolving, solution circulation is reciprocal, reactor pressure 0.3-0.5Mpa, pump discharge pressure＜5Mpa, 750 rev/mins of rotating speeds, inlet filter 10-50 order.
4. the preparation method of chitin fiber according to claim 1 is characterized in that, when filtering chitosan solution, with Quimby pump the solution high-pressure extrusion is passed through filter, pump inlet pressure 0.3-0.5Mpa, pump discharge pressure＜5Mpa, 750 rev/mins of rotating speeds, filter 400-800 order.
5. the preparation method of chitin fiber according to claim 1 is characterized in that, the spinning solution after the filtration enters the vacuum defoamation of negative pressure storage tank, tank internal pressure＜76mmHG from top.
6. the preparation method of chitin fiber according to claim 1 is characterized in that, adopts the spinning machine spinning, and the silk that measuring pump is extruded enters coagulating tank, by stretching, washing, alcohol wash, oil, drying obtains Chitosan Fiber With High Tenacity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110184075.6A CN102851790B (en) | 2011-07-01 | 2011-07-01 | Preparation method of producing high-strength chitosan fiber by use of double-screw pump |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110184075.6A CN102851790B (en) | 2011-07-01 | 2011-07-01 | Preparation method of producing high-strength chitosan fiber by use of double-screw pump |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102851790A true CN102851790A (en) | 2013-01-02 |
| CN102851790B CN102851790B (en) | 2014-08-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110184075.6A Expired - Fee Related CN102851790B (en) | 2011-07-01 | 2011-07-01 | Preparation method of producing high-strength chitosan fiber by use of double-screw pump |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3042706A4 (en) * | 2013-09-02 | 2016-09-21 | Hismer Bio Technology Co Ltd | Composite defoaming method for high-viscosity pure-chitosan spinning solution |
| KR101770658B1 (en) | 2013-09-02 | 2017-08-23 | 히스머 바이오-테크놀로지 컴퍼니, 리미티드 | Defoaming apparatus for high-viscosity pure-chitosan spinning solution |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0328050A2 (en) * | 1988-02-08 | 1989-08-16 | E.I. Du Pont De Nemours And Company | High strength chitosan fibers and fabrics thereof |
| US4932404A (en) * | 1980-10-29 | 1990-06-12 | Unitaka, Ltd. | Chitin fibers and process for the production of the same |
| CN101173048A (en) * | 2007-10-19 | 2008-05-07 | 东华大学 | Method for continuous preparation of polymer solution with ion liquid as solvent |
| CN101250759A (en) * | 2008-04-07 | 2008-08-27 | 宁阳华兴海慈新材料有限公司 | Medical chitosan fibre and preparation method thereof |
| CN201802619U (en) * | 2010-06-29 | 2011-04-20 | 江西凯峰泵业有限公司 | Double-screw pump suitable for conveying easily-dried and hardened chemical medium with high viscosity |
-
2011
- 2011-07-01 CN CN201110184075.6A patent/CN102851790B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4932404A (en) * | 1980-10-29 | 1990-06-12 | Unitaka, Ltd. | Chitin fibers and process for the production of the same |
| EP0328050A2 (en) * | 1988-02-08 | 1989-08-16 | E.I. Du Pont De Nemours And Company | High strength chitosan fibers and fabrics thereof |
| CN101173048A (en) * | 2007-10-19 | 2008-05-07 | 东华大学 | Method for continuous preparation of polymer solution with ion liquid as solvent |
| CN101250759A (en) * | 2008-04-07 | 2008-08-27 | 宁阳华兴海慈新材料有限公司 | Medical chitosan fibre and preparation method thereof |
| CN201802619U (en) * | 2010-06-29 | 2011-04-20 | 江西凯峰泵业有限公司 | Double-screw pump suitable for conveying easily-dried and hardened chemical medium with high viscosity |
Non-Patent Citations (2)
| Title |
|---|
| 《机床与液压》 19991231 杨凯等 "螺杆泵的应用及双螺杆泵的发展" 第14,15,61页 1-6 , 第4期 * |
| 杨凯等: ""螺杆泵的应用及双螺杆泵的发展"", 《机床与液压》, no. 4, 31 December 1999 (1999-12-31) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3042706A4 (en) * | 2013-09-02 | 2016-09-21 | Hismer Bio Technology Co Ltd | Composite defoaming method for high-viscosity pure-chitosan spinning solution |
| KR101770658B1 (en) | 2013-09-02 | 2017-08-23 | 히스머 바이오-테크놀로지 컴퍼니, 리미티드 | Defoaming apparatus for high-viscosity pure-chitosan spinning solution |
| KR101770659B1 (en) | 2013-09-02 | 2017-08-23 | 히스머 바이오-테크놀로지 컴퍼니, 리미티드 | Composite defoaming method for high-viscosity pure-chitosan spinning solution |
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| CN102851790B (en) | 2014-08-06 |
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Owner name: TIANJIN ZHONGSHENG BIOLOGY ENGINEERING CO., LTD. Free format text: FORMER OWNER: ZHOU XINMIN Effective date: 20150803 |
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Effective date of registration: 20150803 Address after: 300457, Tianjin economic and Technological Development Zone Taida small and medium-sized enterprise garden 5, building two, floor 206 workshop Patentee after: Tianjin Zhongsheng Biological Engineering Co.,Ltd. Address before: 300221 Golden Bay Garden, Dagu South Road, Tianjin, Hexi District, 6-1-201 Patentee before: Zhou Xinmin |
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