CN1986921A - Algae fiber gel spinning preparing process - Google Patents
Algae fiber gel spinning preparing process Download PDFInfo
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- CN1986921A CN1986921A CN 200510131145 CN200510131145A CN1986921A CN 1986921 A CN1986921 A CN 1986921A CN 200510131145 CN200510131145 CN 200510131145 CN 200510131145 A CN200510131145 A CN 200510131145A CN 1986921 A CN1986921 A CN 1986921A
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- sodium alginate
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- coagulating bath
- alginate
- lower alcohol
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Abstract
The present invention is process of spinning algae fiber. The production process includes the following steps: dissolving sodium alginate in water solution of sodium hydroxide to obtain 5-25 wt% concentration sodium alginate solution, adding certain amount of hypochloric acid or its salt, stirring at certain temperature, filtering and debubbling to obtain spinning gel; extruding the spinning gel with spinning screw into the first coagulating bath with water and lower alcohol, and drafting for 40-200 % to form the initially formed sodium alginate fiber; and ion exchanging and drafting in the second coagulating bath with lower alcohol, hydrogen chloride and water solution of calcium chloride to form the sodium alginate fiber product.
Description
Technical field:
The present invention relates to a kind of algae fiber gel spinning preparing process, adopt the gel spinning method with sodium alginate soln by spinning screw extrude metering, drawing-off prepares alginate fibre, realizes preparing fast high-strength alginate fibre, belongs to the macromolecule chemical material field.
Background technology:
Marine resources are abundant, and area is wide, take up an area of 71% of sphere area, are the material bases of human survival and development.Marine resources are of a great variety, and reserves are very abundant.Marine natural compound sodium alginate, shitosan, sweet mellow wine etc. are subjected to paying close attention to widely, are green recyclability resources, especially utilize the alginate fibre of preparation such as sodium alginate to can be used as the green fiber material and use.The goods of alginate fibre have good health care and medical function, can promote wound to produce sodium alginate, calcium alginate gel by calcium ion and body's sodium ion-exchange, this gel is hydrophilic, can suppress passing through of bacterium, thereby promote neoblastic growth, healing of wound.
The kind of marine alga is a lot, and alginic acid is the main composition of algin, and it is present in the stem and leaf of marine alga (be roughly equal to 10～20%, all the other are crude protein, crude fat, crude fibre, moisture and impurity etc.).Alginic acid is that marine alga is produced with soda ash solution processing, adds hydrochloric acid in the diffusate of soda ash, free alginic acid the white gels shape precipitation and separate out.Alginic acid has carboxyl-COOH on the 5th carbon atom, carboxyl is an organic acid group, and it is acid that the hydrogen atom H in the carboxyl is.When with in sodium carbonate (soda ash) or the NaOH (caustic soda) and the time, on the 5th carbon atom of alginic acid-hydrogen atom H in the COOH substituted by sodium atom Na, just generates sodium alginate.Sodium alginate through can be made into alginic acid acid calcium after the processing, has excellent biological compatibility as a kind of water soluble polymer.Contain sodium alginate and calcium alginate component fibers and nonwoven cloth material and can be used for hospital gauze, bandage etc.Sodium alginate is mixed with fiber and the existing research of nonwoven fabric both at home and abroad through spinning or with other composition, Wren David etc. has invented the fabric (WO9001954) of curing the wound such as the preparation that is beneficial to sodium alginate, David P.Tong has applied for alginate fibre aftertreatment technology (USP4562110), and Miao Jiuchang has applied for that shitosan, collagen and calcium alginate meet spongy biological dressing and preparation technology (ZL02111437.4) thereof or the like.The main methods such as solvent spinning or film forming that adopt prepare alginate fibre and composite in these patents, because sodium alginate wet spinning concentration ratio is lower, so the ability of spinning is also lower, and intensity is not high.
Summary of the invention:
Purpose of the present invention is low for overcoming alginate fibre spinning concentration, and the spinning ability is low, and the shortcoming that intensity is not high provides a kind of sodium alginate gel spinning preparation technology.Can prepare alginate fibre fast by this technology, and the intensity of fiber obtains certain raising.
For achieving the above object, preparation technology of the present invention comprises: dissolving, stirring, deaeration, drawing-off, ion exchange process specifically are that sodium alginate with certain viscosity is dissolved in that to obtain mass percent in the water that contains 0.5～8% NaOH be 5～25% sodium alginate soln.The viscosity of sodium alginate soln is 600～2000mPaS, and solution temperature is 40～90 ℃; Add 0.01～0.1% hypochlorous acid or hypochlorite again, keep uniform temperature to stir, filter deaeration with 150-250 order filter cloth; The sodium alginate soln for preparing is expressed in first coagulating bath by spinning screw, drawing-off-40～200%, wherein first coagulating bath is made up of water, lower alcohol, wherein the ratio of water and lower alcohol is 20: 80～80: 20, wherein lower alcohol is methyl alcohol, ethanol or mixture, and coagulation bath temperature is 5～60 ℃; Again the alginate fibre of first one-step forming is entered second coagulating bath and carry out ion-exchange, draw forming, second coagulating bath is made up of lower alcohol, hydrogen chloride and calcium chloride water, wherein pure content 1～8%, hydrogen chloride content 1～6%, calcium chloride content 1～8%, coagulation bath temperature is 30～90 ℃.Alginate fibre is in the second coagulating bath drawing-off, and drafting multiple is 10～300%.The present invention has improved the spinning speed of alginate fibre by gel spinning technology, has improved the intensity of fiber simultaneously.
Specific embodiments:
The present invention can be specifically described its preparation process and effect by following embodiment.
Embodiment 1:
Getting high viscosity sodium alginate 10 gram is dissolved in the aqueous solution that 90 grams contain NaOH 2.2% and obtains 10% sodium alginate soln, add a certain amount of aqueous sodium hypochlorite solution, make its content in sodium alginate soln reach 0.08%, 80 ℃ of following high-speed stirred, utilize 200 order filter cloths to filter, by spinning screw the sodium alginate soln gel is expressed in first coagulating bath again, first coagulating bath contains 80% ethanol, water and 0.2% cetyl chloride pyrroles, coagulation bath temperature is 20 ℃, drawing-off 100%, draw alginate fibre, then alginate fibre is entered by 6% ethanol, ion-exchange is carried out in second coagulating bath that 2% hydrochloride aqueous solution and 5% calcium chloride are formed, its coagulation bath temperature is 55 ℃, alginate fibre is 200% at the multiple of the second coagulating bath drawing-off, again with the alginate fibre process washing that obtains, processes such as drying obtain spinnable alginate fibre finished product.
Embodiment 2:
Getting high viscosity sodium alginate 60 gram is dissolved in the aqueous solution that 940 grams contain NaOH 1.2% and obtains 6% sodium alginate soln, add a certain amount of aqueous sodium hypochlorite solution, make clorox content in sodium alginate soln reach 0.1%, 60 ℃ of following high-speed stirred, filter with 200 order filter cloths, by spinning screw the sodium alginate soln gel is expressed in first coagulating bath again, first coagulating bath contains 60% ethanol, water and 0.1% cetyl chloride pyrroles, coagulation bath temperature is 20 ℃, drawing-off 60%, obtain alginate fibre, to enter second coagulating bath again through the alginate fibre of drawing-off and carry out ion-exchange, second coagulating bath is by 10% ethanol, 1% hydrochloride aqueous solution and 4% calcium chloride are formed, coagulation bath temperature is 45 ℃, alginate fibre is 150% at the multiple of second coagulating bath, and the alginate fibre that obtains is through washing, processes such as drying obtain spinnable alginate fibre finished product.
Alginate fibre to embodiment 1,2 gained carries out Mechanics Performance Testing, and the result shows that the dry state fracture strength of alginate fibre reaches 2.6 cN/dTex and 3.4 cN/dTex respectively, illustrates that technical scheme of the present invention has adaptability.
Claims (4)
1, algae fiber gel spinning preparing process, comprise dissolving, stirring, deaeration, drawing-off, ion exchange process, it is characterized in that: the sodium alginate of certain viscosity is dissolved in the aqueous solution that contains NaOH, clorox, keeps that uniform temperature stirs, filtration, deaeration; Sodium alginate soln is extruded in the coagulating bath by spinning screw, and the alginate fibre with first one-step forming carries out ion-exchange again, and drawing-off obtains spinning alginate fibre.
2, algae fiber gel spinning preparing process according to claim 1, it is characterized in that: the viscosity of Na-alginate solution is 600～2000mPaS, and the sodium alginate soln mass percent is 5～25%, sodium hydrate content is 0.5～8%, hypochlorous acid or hypochlorite content are 0.01～0.1%, solution temperature is 40～90 ℃, filter cloth with 150～250 orders.
3, algae fiber gel spinning preparing process according to claim 1, it is characterized in that: first coagulating bath is made up of water, lower alcohol, the ratio of water and lower alcohol is 20: 80～80: 20, wherein lower alcohol is methyl alcohol, ethanol or mixture, coagulation bath temperature is 5～60 ℃, and the first coagulating bath drafting multiple is-40～200%.
4, algae fiber gel spinning preparing process according to claim 1, it is characterized in that: second coagulating bath is made up of lower alcohol, hydrogen chloride and calcium chloride water, wherein: pure content 1～8%, hydrogen chloride content 1～6%, calcium chloride content 1～8%, coagulation bath temperature is 30～90 ℃, and drafting multiple is 10～300%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB2005101311456A CN100491612C (en) | 2005-12-21 | 2005-12-21 | Algae fiber gel spinning preparing process |
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| CNB2005101311456A CN100491612C (en) | 2005-12-21 | 2005-12-21 | Algae fiber gel spinning preparing process |
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| CN1986921A true CN1986921A (en) | 2007-06-27 |
| CN100491612C CN100491612C (en) | 2009-05-27 |
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| CN101994168A (en) * | 2010-11-07 | 2011-03-30 | 青岛大学 | Method for preparing high-strength carrageenin fibers |
| CN101768798B (en) * | 2010-01-22 | 2011-06-29 | 青岛大学 | Preparation method of sodium alga acid/ carbon nano tube composite fibre |
| CN101718010B (en) * | 2009-12-31 | 2011-08-17 | 中国纺织科学研究院 | Method for preparing seaweed fiber |
| CN102181961A (en) * | 2011-03-07 | 2011-09-14 | 青岛大学 | Method for preparing graphene functionalized alginate fibers |
| CN101445983B (en) * | 2007-11-26 | 2011-11-02 | 青岛喜盈门集团有限公司 | High-strength fireproof and radiation-proof healthcare face fabric |
| CN103556301A (en) * | 2013-10-18 | 2014-02-05 | 江南大学 | Method for coloring alginate fibers by nano pigment |
| WO2015036733A1 (en) * | 2013-09-13 | 2015-03-19 | Xiros Limited | Method of producing a swellable polymer fibre |
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| CN104947245A (en) * | 2015-07-13 | 2015-09-30 | 苏州华良化纤纺织有限公司 | Fabricating technique of alginate fiber cloth |
| CN105040158A (en) * | 2015-07-09 | 2015-11-11 | 厦门百美特生物材料科技有限公司 | Copper calcium alginate fiber and its preparation method and use |
| CN105200762A (en) * | 2015-09-10 | 2015-12-30 | 大连工业大学 | Washing and caring liquid and washing and caring finishing method for washing and caring seaweed simulation wig composite fibers |
| CN105544002A (en) * | 2015-12-18 | 2016-05-04 | 厦门百美特生物材料科技有限公司 | Superabsorbent composite fiber and preparation method thereof |
| CN105755578A (en) * | 2015-12-25 | 2016-07-13 | 青岛海之林生物科技开发有限公司 | Application and preparation method of water-soluble calcium alginate fibers |
| CN106012103A (en) * | 2016-07-04 | 2016-10-12 | 青岛大学 | Method for preparing high-strength alginate fiber |
| CN106283270A (en) * | 2015-05-18 | 2017-01-04 | 武汉纺织大学 | A kind of aquogel type alginate fibre and preparation method thereof |
| CN113106604A (en) * | 2021-03-16 | 2021-07-13 | 上海水星家用纺织品股份有限公司 | Preparation method of alginate fiber home textile fabric and prepared fabric |
| CN116536793A (en) * | 2023-04-27 | 2023-08-04 | 青岛大学 | Calcium alginate/polyester composite fiber and preparation method thereof |
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| CN102828285A (en) * | 2012-09-13 | 2012-12-19 | 青岛明月生物医用材料有限公司 | Alginate fiber as well as preparation method and application thereof |
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- 2005-12-21 CN CNB2005101311456A patent/CN100491612C/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445983B (en) * | 2007-11-26 | 2011-11-02 | 青岛喜盈门集团有限公司 | High-strength fireproof and radiation-proof healthcare face fabric |
| CN101718010B (en) * | 2009-12-31 | 2011-08-17 | 中国纺织科学研究院 | Method for preparing seaweed fiber |
| CN101768798B (en) * | 2010-01-22 | 2011-06-29 | 青岛大学 | Preparation method of sodium alga acid/ carbon nano tube composite fibre |
| CN101994168A (en) * | 2010-11-07 | 2011-03-30 | 青岛大学 | Method for preparing high-strength carrageenin fibers |
| CN102181961A (en) * | 2011-03-07 | 2011-09-14 | 青岛大学 | Method for preparing graphene functionalized alginate fibers |
| CN102181961B (en) * | 2011-03-07 | 2013-02-27 | 青岛大学 | Method for preparing graphene functionalized alginate fibers |
| CN103590124B (en) * | 2012-12-27 | 2015-07-15 | 青岛海芬海洋生物科技有限公司 | Preparation method of enteromorpha regenerated cellulose fibers |
| WO2015036733A1 (en) * | 2013-09-13 | 2015-03-19 | Xiros Limited | Method of producing a swellable polymer fibre |
| CN105683426B (en) * | 2013-09-13 | 2018-04-17 | 艾克希罗斯有限公司 | The method for preparing polymers capable of swelling fiber |
| US9869037B2 (en) | 2013-09-13 | 2018-01-16 | Xiros Limited | Method of producing a swellable polymer fibre |
| CN105683426A (en) * | 2013-09-13 | 2016-06-15 | 艾克希罗斯有限公司 | Method of producing a swellable polymer fibre |
| CN103556301B (en) * | 2013-10-18 | 2016-06-22 | 江南大学 | A kind of nano dye is to the painted method of alginate fibre |
| CN103556301A (en) * | 2013-10-18 | 2014-02-05 | 江南大学 | Method for coloring alginate fibers by nano pigment |
| CN106283270A (en) * | 2015-05-18 | 2017-01-04 | 武汉纺织大学 | A kind of aquogel type alginate fibre and preparation method thereof |
| CN105040158A (en) * | 2015-07-09 | 2015-11-11 | 厦门百美特生物材料科技有限公司 | Copper calcium alginate fiber and its preparation method and use |
| CN104947245A (en) * | 2015-07-13 | 2015-09-30 | 苏州华良化纤纺织有限公司 | Fabricating technique of alginate fiber cloth |
| CN105200762B (en) * | 2015-09-10 | 2017-06-16 | 大连工业大学 | For washing the wash and maintenance liquid of shield seaweeds emulation wig composite fibre and its washing shield method for sorting |
| CN105200762A (en) * | 2015-09-10 | 2015-12-30 | 大连工业大学 | Washing and caring liquid and washing and caring finishing method for washing and caring seaweed simulation wig composite fibers |
| CN105544002A (en) * | 2015-12-18 | 2016-05-04 | 厦门百美特生物材料科技有限公司 | Superabsorbent composite fiber and preparation method thereof |
| CN105755578A (en) * | 2015-12-25 | 2016-07-13 | 青岛海之林生物科技开发有限公司 | Application and preparation method of water-soluble calcium alginate fibers |
| CN106012103A (en) * | 2016-07-04 | 2016-10-12 | 青岛大学 | Method for preparing high-strength alginate fiber |
| CN113106604A (en) * | 2021-03-16 | 2021-07-13 | 上海水星家用纺织品股份有限公司 | Preparation method of alginate fiber home textile fabric and prepared fabric |
| CN113106604B (en) * | 2021-03-16 | 2022-08-26 | 上海水星家用纺织品股份有限公司 | Preparation method of alginate fiber home textile fabric and prepared fabric |
| CN116536793A (en) * | 2023-04-27 | 2023-08-04 | 青岛大学 | Calcium alginate/polyester composite fiber and preparation method thereof |
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| CN100491612C (en) | 2009-05-27 |
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Effective date of registration: 20180301 Address after: 266113 Shandong city of Qingdao Province in the Red Island Economic Zone Street Shao Road No. 67 Patentee after: Qingdao source sea new Mstar Technology Ltd Address before: 266071 Ningxia Road, Shandong,, No. 308, Qiingdao University Patentee before: Qingdao University |