CN101240468A - Polyacrylonitrile-chitin composite fiber and its production process - Google Patents
Polyacrylonitrile-chitin composite fiber and its production process Download PDFInfo
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- CN101240468A CN101240468A CNA2008100346733A CN200810034673A CN101240468A CN 101240468 A CN101240468 A CN 101240468A CN A2008100346733 A CNA2008100346733 A CN A2008100346733A CN 200810034673 A CN200810034673 A CN 200810034673A CN 101240468 A CN101240468 A CN 101240468A
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- polyacrylonitrile
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Abstract
The invention relates to a polyacrylonitrile-chitin composite fiber and a manufacturing method of the same, the composite fiber includes a chitin and a polyacrylonitrile, the solid content of chitin is 1-20%, the solid content of polyacrylonitrile is 80-90%; the manufacturing method includes: 1) the 3-45% PAN solution is solvated in the solution; 2) the chitin which addition is 1-20% of polyacrylonitrile dried weight is added to polyacrylonitrile forming the polyacrylonitrile-chitin spinning solution to standing and deairing; 3) the spinning solution is spun from the spinneret holes, after stretching, washing, drying and other common procedure forming conventional processes finished product. The invention can improve the human affinity to PAN fiber, improve the anti-bacterial and antipruritic fiber effects to fiber, and increase the antistatic property to PAN fiber.
Description
Technical field
The invention belongs to composite and method field of manufacturing thereof, particularly relate to a kind of polyacrylonitrile-chitin composite fiber and manufacture method thereof.
Background technology
Polyacrylonitrile fibre is commonly called as acrylic fibers, be a kind of synthetic fiber, good warmth retention property, excellent dyeability arranged and do not have moth erosion and mould sex change, can obtain after its dyeing than wool gay colours more, polyacrylonitrile is widely used in making the simulate wool goods, so polyacrylonitrile is known as artificial wool again.But polyacrylonitrile also has a lot of shortcomings: hydrophily is poor, causes at easy static electrification of dry weather and human body compatibility relatively poorly, and anti-microbial property is also not so good.
In order to improve the performance of these shortcomings of polyacrylonitrile, the researcher has done a large amount of work aspect modified polyacrylonitrile, as silk graft polypropylene nitrile, milk protein graft polypropylene nitrile fiber, but these all will just carry out very big change to existing equipment, technology at polymerization stage, can not obtain a large amount of popularizations.
Chitin and derivative thereof have anti-microbial property and certain hydrophily well.China's chitin aboundresources.Recently also the someone begins chitin and derivative thereof are used for the modification of chemical fibre, is the Chinese patent of 99120092 " cm-chitosan and alginic acid blend film or fiber preparation method and uses thereof " as application number.In chitin and derivative thereof, the cost of chitin is minimum, but the compatibility of chitin and the fibre-forming polymer that some are conventional is poor, particularly chitin both infusibility melt, water insoluble again, diluted acid, diluted alkaline, concentrated base and common organic solvents, therefore the application in the chemical fibre modification is restricted.
Summary of the invention
Technical problem to be solved by this invention provides a kind of polyacrylonitrile-chitin composite fiber and manufacture method thereof, to remedy the deficiencies in the prior art and defective, meets the demands of production and living.
The present invention utilizes chitin and polyacrylonitrile that polar group is arranged, compatibility is good, particularly chitin can be dissolved in the partial solvent (sodium sulfocyanate, the potassium rhodanide aqueous solution) of polyacrylonitrile, therefore make chitin and polyacrylonitrile in spinning solution even mix and disperse after, prepare polyacrylonitrile-chitin composite fiber by the original spinning technique of polyacrylonitrile fibre, with the hydrophily of improving polyacrylonitrile fibre, antistatic behaviour, with the affine antibiotic property of human body.
A kind of polyacrylonitrile-chitin composite fiber of the present invention is made up of chitin and polyacrylonitrile, and chitin accounts for 1～20% of composite fibre solid content, and polyacrylonitrile accounts for 80～99% of fiber solid content.
Described polyacrylonitrile is acrylonitrile homopolymer or copolymer, and viscosity average molecular weigh is that 50000～170000 conventional molecular weight or viscosity average molecular weigh are 500000～2000000 super high molecular weight;
Described chitin is industrial chitin goods or directly from extracting from the cell membrane of the wing that saves sufficient animal (Araneae, shell-fish) or shell and fungi and algae;
The preparation method of a kind of polyacrylonitrile-chitin composite fiber of the present invention comprises the steps:
(1) polyacrylonitrile is dissolved in the solvent, is made into mass fraction and is 3～45% polyacrylonitrile solution;
(2) the chitin powder is dissolved in the solvent of polyacrylonitrile or after making superfine powder and adds in the polyacrylonitrile solution, addition is 1～20% of a polyacrylonitrile dry weight, is made into the polyacrylonitrile-chitin spinning solution, standing and defoaming;
(3) spinning solution that step (2) is obtained is through spinneret orifice ejection back curing molding, stretched again, washing, curls, makes finished product after these several roads routine operations such as typing, drying.
Solvent in the described step (1) is that mass percent is that 30%～75% zinc chloride, sodium sulfocyanate, potassium rhodanide, the aqueous solution of nitric acid, mass percent are one or more in 5%～80% ethylene carbonate sodium thiocyanate solution, dimethyl formamide, dimethylacetylamide, the dimethyl sulfoxide (DMSO).
Superfine powder particle size range in the described step (2) is at 100nm-1000nm.
Curing molding in the described step (3) is to finish through wet spinning, dry spinning, dry-wet spinning or gel spinning technology.
Described wet spinning technology is spinning, stretching, washing, drying or washing, stretching, drying, specifically to be spinning solution enter after the spinning head ejection is solidified into silk the spinning bath, coagulating bath is 0～30% the aqueous solution for solvent quality concentration, and temperature is 0～70 ℃, and it stretches and divides multistage carrying out, it is 1～3 grade, hot bath or saturated vapor are done drawing medium, and the temperature of stretching is 65～140 ℃, and total draw ratio is 1～10 times; Drying can be undertaken by radiation, Contact Heating, and temperature is 80～170 ℃.
Described dry-spinning process is spinning, stretching, drying, promptly being heated to 130～140 ℃ spinning solution enters spinning shaft after the special-purpose spinning head ejection of spinning doughnut and is solidified into silk, long 6～the 10m of spinning shaft, medium is air, nitrogen or saturated vapor, is heated to 280～400 ℃; Be stretched as 1～3 grade and carry out, hot bath or saturated vapor are done drawing medium, and temperature is 65～140 ℃, and total draw ratio is 1～10 times; Drying can be undertaken by radiation, Contact Heating, and temperature is 80～170 ℃.
Described dry-wet spinning moulding process is spinning, stretching, washing, drying or spinning, washing, stretching, drying, wherein spinning solution passes through one section air gap earlier from spinning head ejection back, enter then and be solidified into silk in the spinning bath, the medium of air gap is air or nitrogen, air gap length is 1～10cm, coagulating bath is 0～30% the aqueous solution for solvent quality concentration, and temperature is 0～70 ℃; Describedly be stretched as 1～3 grade, hot bath or saturated vapor are done drawing medium, and the temperature of stretching is 65～140 ℃, and total draw ratio is 1～10 times; Described drying is undertaken by radiation, Contact Heating, and temperature is 80～170 ℃.
Described gel spinning technology is spinning, washing, extraction, stretching, dry, specifically be to be heated to 130～180 ℃ spinning solution after the special-purpose spinning head ejection of spinning doughnut, to enter to introduce and freeze to form the gel state strand the cold coagulating bath through air gap, the medium of air gap is air or other gas nitrogen, air gap length is 1～10cm, coagulating bath is that solvent quality concentration is 75%～85% the aqueous solution, and temperature is 0～10 ℃; Described extraction is that the gel state strand that will come out from coagulating bath imports earlier the good solvent of volatility, and the solvent that described volatility is good has ethanol, ethylene glycol or glycerol; Describedly be stretched as 2～3 grades, bathe or saturated vapor is done drawing medium with hot bath, hot alcohols, the temperature of stretching is 65～140 ℃, 10～30 times of total draw ratios; Described drying can be undertaken by radiation, Contact Heating or gas medium, and temperature is 80～170 ℃.
Beneficial effect of the present invention:
Improve the human body compatibility of polyacrylonitrile fibre, in addition give the fiber anti-bacterial, anti-itching special efficacy, increase the antistatic behaviour of polyacrylonitrile fibre.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
A kind of polyacrylonitrile-chitin composite fiber, described composite fibre is made up of chitin and polyacrylonitrile, and chitin accounts for 1% of composite fibre solid content, and polyacrylonitrile accounts for 99% of fiber solid content.
Be that 90000 polyacrylonitrile and chitin powder be dissolved in 51.3% sodium thiocyanate water solution together, make concentration with viscosity average molecular weigh be 11% spinning solution, polyacrylonitrile and chitin weight ratio are 100: 1, leave standstill 12h after stirring, deaeration.
Spinning solution enters the spinneret orifice ejection through measuring pump.Enter first coagulating bath, the content of sodium sulfocyanate is 9% in the coagulating bath, and temperature is 10 ℃.Enter second coagulating bath again, carry out predraft, coagulating bath is 3% sodium thiocyanate water solution, and bathing temperature is that 50 ℃ of stretching ratios are 1.5 times.Stretch through saturated vapor, draft temperature is 100 ℃ again, and stretching ratio is 10 times, with after washing, oils, and is dry under the condition of 100 ℃ of temperature.Dry fiber curls at 80 ℃, and the back oils once more 130 ℃ of temperature HEAT SETTING, obtains polyacrylonitrile/chitin composite fiber finished product 80 ℃ of dryings.
Embodiment 2
A kind of polyacrylonitrile-chitin composite fiber, described composite fibre is made up of chitin and polyacrylonitrile, and chitin accounts for 10% of composite fibre solid content, and polyacrylonitrile accounts for 90% of fiber solid content.
With viscosity average molecular weigh is the solder(ing)acid that 120000 polyacrylonitrile is dissolved in 65% weight, makes concentration and be 12% spinning solution, with the chitin superfine powder of the 500nm mixed by 9: 1, leaves standstill 12h after stirring, deaeration then.
Spinning solution enters the spinneret orifice ejection through measuring pump.Enter first coagulating bath, the content of calcium chloride is 12% in the coagulating bath, and temperature is 30 ℃.Through second coagulating bath, carry out predraft again, coagulating bath is the 4% calcium chloride acid sodium aqueous solution aqueous solution, and temperature is 50 ℃, and stretching ratio is 3 times.Through steam stretching, draft temperature is 70 ℃ again, and stretching ratio is 5 times, with after washing, oils, and is dry under the condition of 110 ℃ of temperature.Dry fiber curls at 70 ℃, and the back oils once more 80 ℃ of temperature HEAT SETTING, obtains polyacrylonitrile/chitin composite fiber finished product 90 ℃ of dryings.
Embodiment 3
A kind of polyacrylonitrile-chitin composite fiber is characterized in that: described composite fibre is made up of chitin and polyacrylonitrile, and chitin accounts for 20% of composite fibre solid content, and polyacrylonitrile accounts for 80% of fiber solid content.
Polyacrylonitrile is dissolved in dimethyl sulfoxide (DMSO), and to make concentration be 25% spinning solution, with the chitin superfine powder of the 700nm mixed by 8: 2, leaves standstill 12h after stirring, deaeration then.
Spinning solution enters the spinneret orifice ejection through measuring pump.Enter first coagulating bath, the content of dimethyl sulfoxide (DMSO) is 20% in the coagulating bath, and temperature is 20 ℃.Through second coagulating bath, carry out predraft again, coagulating bath is 9% dimethyl sulfoxide (DMSO), and temperature is 50 ℃, and stretching ratio is 3 times.Through steam stretching, draft temperature is 35 ℃ again, and stretching ratio is 5 times, with after washing, oils, and is dry under the condition of 110 ℃ of temperature.Dry fiber curls at 50 ℃, and the back oils once more 120 ℃ of temperature HEAT SETTING, obtains polyacrylonitrile/chitin composite fiber finished product 110 ℃ of dryings.
Claims (11)
1. polyacrylonitrile-chitin composite fiber, it is characterized in that: this fiber is made up of chitin and polyacrylonitrile, and chitin accounts for 1～20% of composite fibre solid content, and polyacrylonitrile accounts for 80～99% of fiber solid content.
2. polyacrylonitrile-chitin composite fiber according to claim 1, it is characterized in that: described polyacrylonitrile is acrylonitrile homopolymer or copolymer, and viscosity average molecular weigh is that 50000～170000 conventional molecular weight or viscosity average molecular weigh are 500000～2000000 super high molecular weight.
3. polyacrylonitrile-chitin composite fiber according to claim 1 is characterized in that: described chitin is industrial chitin goods or directly from extracting from the cell membrane that saves sufficient animal Araneae, crustacean wing or shell and fungi and algae.
4. the preparation method of a polyacrylonitrile-chitin composite fiber comprises the steps:
(1) polyacrylonitrile is dissolved in the solvent, is made into mass fraction and is 3～45% polyacrylonitrile solution;
(2) the chitin powder is dissolved in the solvent of polyacrylonitrile or after making superfine powder and adds in the polyacrylonitrile solution, addition is 1～20% of a polyacrylonitrile dry weight, is made into the polyacrylonitrile-chitin spinning solution, standing and defoaming;
(3) spinning solution that step (2) is obtained is through spinneret orifice ejection back curing molding, stretched again, washing, curls, makes finished product after the typing, dry this several roads routine operation.
5. the preparation method of polyacrylonitrile-chitin composite fiber according to claim 1 is characterized in that: the solvent in the described step (1) is that mass percent is that 30%～75% zinc chloride, sodium sulfocyanate, potassium rhodanide, the aqueous solution of nitric acid, mass percent are one or more in 5%～80% ethylene carbonate sodium thiocyanate solution, dimethyl formamide, dimethylacetylamide, the dimethyl sulfoxide (DMSO).
6. the preparation method of polyacrylonitrile-chitin composite fiber according to claim 1, it is characterized in that: the superfine powder particle size range in the described step (2) is at 100nm-1000nm.
7. the preparation method of polyacrylonitrile-chitin composite fiber according to claim 1, it is characterized in that: the curing molding in the described step (3) is to finish through wet spinning, dry spinning, dry-wet spinning or gel spinning technology.
8. the preparation method of polyacrylonitrile-chitin composite fiber according to claim 7, it is characterized in that: described wet spinning technology is spinning, stretching, washing, drying or washing, stretching, drying, specifically to be spinning solution enter after the spinning head ejection is solidified into silk the spinning bath, coagulating bath is 0～30% the aqueous solution for solvent quality concentration, temperature is 0～70 ℃, it stretches and divides multistage carrying out, it is 1～3 grade, hot bath or saturated vapor are done drawing medium, the temperature that stretches is 65～140 ℃, and total draw ratio is 1～10 times; Drying is to be undertaken by radiation, Contact Heating, and temperature is 80～170 ℃.
9. the preparation method of polyacrylonitrile-chitin composite fiber according to claim 7, it is characterized in that: described dry-spinning process is spinning, stretching, drying, specifically be to be heated to 130～140 ℃ spinning solution to enter spinning shaft after the special-purpose spinning head ejection of spinning doughnut and be solidified into silk, long 6～the 10m of spinning shaft, medium is air, nitrogen or saturated vapor, is heated to 280～400 ℃; Be stretched as 1～3 grade and carry out, hot bath or saturated vapor are done drawing medium, and temperature is 65～140 ℃, and total draw ratio is 1～10 times; Drying is to be undertaken by radiation, Contact Heating, Contact Heating, and temperature is 80～170 ℃.
10. the preparation method of polyacrylonitrile-chitin composite fiber according to claim 7, it is characterized in that: described dry-wet spinning moulding process is spinning, stretching, washing, drying or spinning, washing, stretching, drying, wherein spinning solution passes through one section air gap earlier from spinning head ejection back, enter then and be solidified into silk in the spinning bath, the medium of air gap is air or nitrogen, air gap length is 1～10cm, coagulating bath is 0～30% the aqueous solution for solvent quality concentration, and temperature is 0～70 ℃; Be stretched as 1～3 grade, hot bath or saturated vapor are done drawing medium, and the temperature of stretching is 65～140 ℃, and total draw ratio is 1～10 times; Drying be by radiation,, Contact Heating carries out, temperature is 80～170 ℃.
11. the preparation method of polyacrylonitrile-chitin composite fiber according to claim 7, it is characterized in that: described gel spinning technology is spinning, washing, extraction, stretching, dry, specifically be to be heated to 130～180 ℃ spinning solution after the special-purpose spinning head ejection of spinning doughnut, to enter to introduce and freeze to form the gel state strand the cold coagulating bath through air gap, the medium of air gap is air or nitrogen, air gap length is 1～10cm, coagulating bath is that solvent quality concentration is 75%～85% the aqueous solution, and temperature is 0～10 ℃; Extraction is that the gel state strand that will come out from coagulating bath imports earlier the good solvent of volatility, and the solvent that described volatility is good has ethanol, ethylene glycol or glycerol; Be stretched as 2～3 grades, do drawing medium with hot bath, the bath of hot alcohols or saturated vapor, the temperature of stretching is 65～140 ℃, 10～30 times of total draw ratios; Drying is to be undertaken by radiation, Contact Heating or gas medium, and temperature is 80～170 ℃.
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| CN101845676A (en) * | 2010-05-18 | 2010-09-29 | 北京航空航天大学 | Multifunctional composite fiber and preparation method thereof |
| CN102268753A (en) * | 2010-06-04 | 2011-12-07 | 康力得生技股份有限公司 | Manufacture method for high-molecular fiber and wound dressing, and obtained wound dressing |
| CN103061040A (en) * | 2013-01-06 | 2013-04-24 | 浙江理工大学 | Electrostatic spinning preparation method of silk fibroin/polyacrylonitrile based antibacterial ultraviolet-resistant nanofiber membrane |
| CN103173893A (en) * | 2010-06-04 | 2013-06-26 | 康力得生技股份有限公司 | Polymer fiber and preparation method thereof |
| CN103752179A (en) * | 2014-01-09 | 2014-04-30 | 天津工业大学 | Preparation method of hydrophobic hollow fiber membrane |
| CN103757735A (en) * | 2013-12-26 | 2014-04-30 | 江苏神泰科技发展有限公司 | Preparation method of high modulus polyethylene fiber |
| CN105821509A (en) * | 2016-04-28 | 2016-08-03 | 东华大学 | Antibacterial anti-static polyacrylonitrile fibers and manufacture method thereof |
| WO2016127465A1 (en) * | 2015-02-09 | 2016-08-18 | 上海史墨希新材料科技有限公司 | Preparation method for high-strength polyacrylonitrile nano composite fibres |
| CN106978643A (en) * | 2017-02-26 | 2017-07-25 | 浙江峰赫纺织有限公司 | A kind of durability antibacterial polyacrylonitrile fiber |
| CN107502993A (en) * | 2017-08-11 | 2017-12-22 | 广东富琳健康产业有限公司 | A kind of far IR fibre for physiotherapy cushion for travelling and preparation method thereof |
| CN107988707A (en) * | 2017-12-25 | 2018-05-04 | 合肥洁诺无纺布制品有限公司 | A kind of non-woven fabrics neonate blanket of fluffy antibacterial and preparation method thereof |
| CN110592713A (en) * | 2019-05-24 | 2019-12-20 | 苏州峰佳达化纤纺织有限公司 | Preparation method of antibacterial polyacrylonitrile fiber |
| CN116837481A (en) * | 2023-05-25 | 2023-10-03 | 青岛狮印海洋生物科技有限公司 | Chitin-based antibacterial composite fiber and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101845676B (en) * | 2010-05-18 | 2012-05-23 | 北京航空航天大学 | Multifunctional composite fiber and preparation method thereof |
| CN101845676A (en) * | 2010-05-18 | 2010-09-29 | 北京航空航天大学 | Multifunctional composite fiber and preparation method thereof |
| CN103173893B (en) * | 2010-06-04 | 2015-04-22 | 康力得生技股份有限公司 | Polymer fiber and preparation method thereof |
| CN103173893A (en) * | 2010-06-04 | 2013-06-26 | 康力得生技股份有限公司 | Polymer fiber and preparation method thereof |
| CN102268753B (en) * | 2010-06-04 | 2014-03-12 | 康力得生技股份有限公司 | Manufacture method for wound dressing, and obtained wound dressing |
| CN102268753A (en) * | 2010-06-04 | 2011-12-07 | 康力得生技股份有限公司 | Manufacture method for high-molecular fiber and wound dressing, and obtained wound dressing |
| CN103061040B (en) * | 2013-01-06 | 2015-10-28 | 浙江理工大学 | The electrostatic spinning preparation method of fibroin/polyacrylonitrile-radical antibacterial ultraviolet-resistannanofiber nanofiber membrane |
| CN103061040A (en) * | 2013-01-06 | 2013-04-24 | 浙江理工大学 | Electrostatic spinning preparation method of silk fibroin/polyacrylonitrile based antibacterial ultraviolet-resistant nanofiber membrane |
| CN103757735A (en) * | 2013-12-26 | 2014-04-30 | 江苏神泰科技发展有限公司 | Preparation method of high modulus polyethylene fiber |
| CN103752179A (en) * | 2014-01-09 | 2014-04-30 | 天津工业大学 | Preparation method of hydrophobic hollow fiber membrane |
| WO2016127465A1 (en) * | 2015-02-09 | 2016-08-18 | 上海史墨希新材料科技有限公司 | Preparation method for high-strength polyacrylonitrile nano composite fibres |
| CN105821509A (en) * | 2016-04-28 | 2016-08-03 | 东华大学 | Antibacterial anti-static polyacrylonitrile fibers and manufacture method thereof |
| CN106978643A (en) * | 2017-02-26 | 2017-07-25 | 浙江峰赫纺织有限公司 | A kind of durability antibacterial polyacrylonitrile fiber |
| CN107502993A (en) * | 2017-08-11 | 2017-12-22 | 广东富琳健康产业有限公司 | A kind of far IR fibre for physiotherapy cushion for travelling and preparation method thereof |
| CN107988707A (en) * | 2017-12-25 | 2018-05-04 | 合肥洁诺无纺布制品有限公司 | A kind of non-woven fabrics neonate blanket of fluffy antibacterial and preparation method thereof |
| CN110592713A (en) * | 2019-05-24 | 2019-12-20 | 苏州峰佳达化纤纺织有限公司 | Preparation method of antibacterial polyacrylonitrile fiber |
| CN116837481A (en) * | 2023-05-25 | 2023-10-03 | 青岛狮印海洋生物科技有限公司 | Chitin-based antibacterial composite fiber and preparation method and application thereof |
| CN116837481B (en) * | 2023-05-25 | 2024-03-12 | 青岛狮印海洋生物科技有限公司 | Chitin-based antibacterial composite fiber and preparation method and application thereof |
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Application publication date: 20080813 |