CN102373514A - Glucomannan fiber and preparation method thereof - Google Patents
Glucomannan fiber and preparation method thereof Download PDFInfo
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- CN102373514A CN102373514A CN2011103094350A CN201110309435A CN102373514A CN 102373514 A CN102373514 A CN 102373514A CN 2011103094350 A CN2011103094350 A CN 2011103094350A CN 201110309435 A CN201110309435 A CN 201110309435A CN 102373514 A CN102373514 A CN 102373514A
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Abstract
The invention discloses a glucomannan fiber and a preparation method thereof. The preparation method comprises the following steps: carrying out stirring and swelling on 10-30 parts of purified glucomannan and 100-200 parts of 50% ethanol by weight for 1h in a reaction kettle under normal temperature, then raising the temperature to 50 DEG C, adding 0.01-2.0 parts of initiator to react for 10-30min and then adding 1-10.0 parts of grafting monomer to react for 0.5-6h at 30-90 DEG C under the protection of N2; adding 1-10% of sodium hydroxide solution, stirring the mixture uniformly and adjusting the pH value to be neutral, thus obtaining spinning solution; and after filtering and defoaming the spinning solution, spraying the spinning solution into an ethanol coagulating bath by adopting a spinneret with diameter being 0.1-0.5mm to coagulate and form the spinning solution, and after eluting the coagulated and formed product with water, drying the product for 0.5-1h at 50-70 DEG C, thus obtaining the glucomannan fiber. The glucomannan fiber belongs to a functional fiber modified by natural polysaccharide, has high fineness, light specific weight, high tensile strength, strong acid and alkali resistance and good moisture absorption and conductivity and is an ideal raw material of apparel textiles, health care products, medical and environmental products and the like.
Description
Technical field
The present invention relates to a kind of Glucomannan fiber and preparation method thereof, belong to the technical field of compositions that contains the Glucomannan material.
Background technology
At present the world per capita the fiber consumption figure be 8kg, will increase from now on, according to the up-to-date prediction of the United Nations, to the year two thousand fifty world population will reach 9,000,000,000, the fiber aggregate demand will reach about 0.9～100,000,000 ton.The big fast development that promotes fiber industry of fiber consumption; And along with science and technology development and human living standard's raising, people have proposed requirement comfortable and easy to wear, attractive in appearance, health care to clothes, thereby all kinds of tencel and textiles thereof continue to bring out; Like milk fibre, soybean fiber, bamboo fibre, chitin fiber etc.; Their each tool advantage and characteristics, good serviceability quite receives the consumer to like that market prospects are inestimable.
Glucomannan is a kind of from plant konjaku, jerusalem artichoke, any of several broadleaf plants lotus root, and the natural macromolecule amylose that extracts in the microbial bacterial, molecular weight are 200; 000～2, between 000,000; Its main chain passes through β-1 by glucose and mannose, and the 4-glycosidic bond is formed by connecting, at the mannose C of main chain
3Exist through β-1 on the position, the branched structure that the 3-glycosidic bond combines has 3 side chains on per 32 saccharide residues, on per 19 saccharide residues 1 acetyl group is arranged.The size of Glucomannan molecular weight and its solubility, dissolved adhesiveness are closely related, and the content of acetyl group is being controlled the size of macromolecule water-solubility.Glucomannan has multifrequency nature such as gelation, thickening property, film forming, antibiotic property and physiological function that some are special, as improve glycometabolism, regulate lipid-metabolism, cleaning intestine, anticancer, delay cell senescence, improve heart and brain and vascular function etc.Sufficient, biodegradable as a kind of renewable natural resources source, have chemical modifiable functional group, can be widely used in environmental protection, food, medicine, chemical industry and biological field.Utilize the fiber of Glucomannan production to have excellent biological compatibility; Its fracture strength and modulus are moderate; Elongation is big, and the spinning weaving performance is good, has both had the good characteristic of natural silk; The physical and chemical performance that has synthetic fiber again can be widely used in the industries such as textile clothing, health care product, medical treatment and environmental supplies.
Summary of the invention
Goal of the inventionThe purpose of this invention is to provide a kind of is the method for raw material production Glucomannan fiber with natural Glucomannan, is the service that large-scale develops and utilizes of renewable resource Glucomannan.
Technical schemeTechnical scheme of the present invention is: a kind of Glucomannan fiber is characterized in that the weight proportion of its component and each component is: 10～30 parts of purifying Glucomannans, 0.01～2.0 part of initator, 1～10.0 part of grafted monomers, 100～200 parts of 50% ethanol; It is by weight getting 10～30 parts of purifying Glucomannans, and 100～200 parts of 50% ethanol normal temperature in agitated reactor stirs swelling 1h down, is warming up to 50 ℃ then; Add 0.01～2.0 part of initator, reaction 10～30min adds 1～10.0 part of grafted monomers then; At 30～90 ℃, and at N
2Protective condition is reaction 0.5～6h down; Add 1%～10% sodium hydroxide solution and stir, transfer pH, promptly obtain spinning solution to neutral; With spinning solution filter, after the deaeration, adopting diameter is that the spinning head of 0.1～0.5mm sprays into alcohol solidification and makes its coagulation forming in bathing, and behind water wash, obtains at 50～70 ℃ of down dry 0.5～1h.
Described Glucomannan is from plant konjaku, jerusalem artichoke, any of several broadleaf plants lotus root, the Glucomannan that extracts in the bacterium, and average grain diameter is 1～200 um.
The Glucomannan content of purifying Glucomannan is more than 90%, got through Ethanol Treatment, purification by common coarse powder of glucomannan.It is that common coarse powder of glucomannan is swollen in the ethanol of concentration 50% lixiviate 2 times, with distilled water wash 3 times, and centrifugal dehydration; Be settled out the purifying head product with absolute ethyl alcohol again; Head product earlier with 95% washing with alcohol, is used absolute ethanol washing at last, and the product after the washing obtains through drying.
Initator is selected one or more the combination in any in ammonium ceric nitrate, potassium permanganate, potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate, hydrogen peroxide, benzoyl peroxide, the lauroyl peroxide for use.
Grafted monomers is selected one or more the combination in any in acrylonitrile, acrylic acid, styrene, acrylamide, methyl acrylate, butyl acrylate, the vinyl acetate for use.
Prepare the method for Glucomannan fiber, the steps include:
The first step, by weight getting 10～30 parts of purifying Glucomannans, 50% ethanol stirs swelling 1h for 100～200 parts under the normal temperature in agitated reactor; Be warming up to 50 ℃ then; Add 0.01～2.0 part of initator, reaction 10～30min adds 1～10.0 part of grafted monomers then; At 30～90 ℃, and under the N2 protective condition, react 0.5～6h;
Second step added 1%～10% sodium hydroxide solution and stirs, and transferred pH to neutral, promptly obtained spinning solution;
The 3rd step, with spinning solution filter, after the deaeration, adopting diameter is that the spinning head of 0.1～0.5mm sprays into alcohol solidification and makes its coagulation forming in bathing, and behind water wash, at 50～70 ℃ of down dry 0.5～1h, promptly obtains the Glucomannan fiber.
Beneficial effectThe present invention is a raw material with reproducible natural macromolecule amylose-Glucomannan, processes novel Glucomannan fiber.The main raw material Glucomannan of forming this fiber contain polyhydroxy, half compliance molecular chain structure and self with faintly acid make that its fibre is soft, smooth, quality is frivolous, moisture absorption, wet transmitting performance are superior.This fiber is pure white and has the gloss as the real silk that dyeability is good, is the desirable feedstock of making top-grade fashion.This fibre composition Glucomannan has excellent biological compatibility, can not produce any toxicity to Skin Cell, has the effect of health care, nutrition skin.As the tencel raw material because its excellent processing characteristics and serviceability can be widely used in manufacture fields such as textile clothing, health care product, medical treatment and environmental supplies.
The specific embodiment
The present invention is realized that by following practical implementation measure wherein said raw material umber is parts by weight except that specified otherwise.Below in conjunction with embodiment the present invention is done into-goes on foot detailed description.
Glucomannan purifying: common coarse powder of glucomannan is swollen in the ethanol of concentration 50% lixiviate 2 times; With distilled water wash 3 times; Centrifugal dehydration is settled out the purifying head product with absolute ethyl alcohol again, and head product is earlier with 95% washing with alcohol; Use absolute ethanol washing at last, the product after the washing can obtain the purifying Glucomannan through drying.Glucomannan content is more than 90%.
Embodiment 1: by weight getting 10 parts of purifying Glucomannans, 50% ethanol stirs swelling 1h for 100 parts under the normal temperature in agitated reactor, be warming up to 50 ℃ then, adds 0.01 part of ammonium ceric nitrate, and reaction 10min adds 1 part of acrylonitrile then, at 30 ℃, and at N
2Protective condition is reaction 6h down; Add 1% sodium hydroxide solution and stir, transfer pH, promptly obtain spinning solution to neutral; With spinning solution filter, after the deaeration, adopting diameter is that the spinning head of 0.1mm sprays into alcohol solidification and makes its coagulation forming in bathing, and behind water wash, at 50 ℃ of dry 0.51h down, promptly obtains the Glucomannan fiber.
Embodiment 2: by weight getting 30 parts of purifying Glucomannans, 50% ethanol stirs swelling 1h for 200 parts under the normal temperature in agitated reactor, be warming up to 50 ℃ then, adds 2.0 parts in initator potassium permanganate, and reaction 30min adds 10.0 parts of methyl acrylates then, at 90 ℃, and at N
2Protective condition is reaction 0.5h down; Add 10% sodium hydroxide solution and stir, transfer pH, promptly obtain spinning solution to neutral; With spinning solution filter, after the deaeration, adopting diameter is that the spinning head of 0.5mm sprays into alcohol solidification and makes its coagulation forming in bathing, and behind water wash, at 70 ℃ of dry 1h down, promptly obtains the Glucomannan fiber.
Embodiment 3: by weight getting 20 parts of purifying Glucomannans, 50% ethanol stirs swelling 1h for 160 parts under the normal temperature in agitated reactor, be warming up to 50 ℃ then; Add 1 part of potassium peroxydisulfate, 0.5 part of benzoyl peroxide, reaction 20min adds 5 parts in acrylic acid, 3 parts of methyl acrylates then; Under 70 ℃, and at N
2Protective condition is reaction 3h down; Add 6% sodium hydroxide solution and stir, transfer pH, promptly obtain spinning solution to neutral; With spinning solution filter, after the deaeration, adopting diameter is that the spinning head of 0.3mm sprays into alcohol solidification and makes its coagulation forming in bathing, and behind water wash, at 60 ℃ of dry 0.6h down, promptly obtains the Glucomannan fiber.
Embodiment 4: by weight getting 15 parts of purifying Glucomannans, 50% ethanol stirs swelling 1h for 150 parts under the normal temperature in agitated reactor, be warming up to 50 ℃ then; Add 0.1 part of sodium peroxydisulfate, 1 part of ammonium persulfate, reaction 25min adds 2 parts of styrene, 3 parts of acrylamides then; Under 60 ℃, and at N
2Protective condition is reaction 4h down; Add 8% sodium hydroxide solution and stir, transfer pH, promptly obtain spinning solution to neutral; With spinning solution filter, after the deaeration, adopting diameter is that the spinning head of 0.4mm sprays into alcohol solidification and makes its coagulation forming in bathing, and behind water wash, at 55 ℃ of dry 1h down, promptly obtains the Glucomannan fiber.
Embodiment 5: by weight getting 18 parts of purifying Glucomannans; 50% ethanol stirs swelling 1h for 130 parts under the normal temperature in agitated reactor, be warming up to 50 ℃ then, adds 1 part of hydrogen peroxide, 0.5 part of lauroyl peroxide; Reaction 15min; Add 3 parts of butyl acrylates, 4 parts of vinyl acetates then, under 45 ℃, and at N
2Protective condition is reaction 5h down; Add 4% sodium hydroxide solution and stir, transfer pH, promptly obtain spinning solution to neutral; With spinning solution filter, after the deaeration, adopting diameter is that the spinning head of 0.2mm sprays into alcohol solidification and makes its coagulation forming in bathing, and behind water wash, at 60 ℃ of dry 0.6h down, promptly obtains the Glucomannan fiber.
Claims (6)
1. a Glucomannan fiber is characterized in that, the weight proportion of its component and each component is: 10～30 parts of purifying Glucomannans, 0.01～2.0 part of initator, 1～10.0 part of grafted monomers, 100～200 parts of 50% ethanol; It is by weight getting 10～30 parts of purifying Glucomannans, and 100～200 parts of 50% ethanol normal temperature in agitated reactor stirs swelling 1h down, is warming up to 50 ℃ then; Add 0.01～2.0 part of initator, reaction 10～30min adds 1～10.0 part of grafted monomers then; At 30～90 ℃, and at N
2Protective condition is reaction 0.5～6h down; Add 1%～10% sodium hydroxide solution and stir, transfer pH, promptly obtain spinning solution to neutral; With spinning solution filter, after the deaeration, adopting diameter is that the spinning head of 0.1～0.5mm sprays into alcohol solidification and makes its coagulation forming in bathing, and behind water wash, obtains at 50～70 ℃ of down dry 0.5～1h.
2. Glucomannan fiber according to claim 1 is characterized in that, described Glucomannan is the Glucomannan that from plant konjaku, jerusalem artichoke, any of several broadleaf plants lotus root, bacterium, extracts, and average grain diameter is 1～200 um.
3. Glucomannan fiber according to claim 1 is characterized in that, described purifying Glucomannan is that common coarse powder of glucomannan is swollen in the ethanol of concentration 50% lixiviate 2 times; With distilled water wash 3 times; Centrifugal dehydration is settled out the purifying head product with absolute ethyl alcohol again, and head product is earlier with 95% washing with alcohol; Use absolute ethanol washing at last, the product after the washing obtains through dry.
4. Glucomannan fiber according to claim 1; It is characterized in that described initator is selected one or more the combination in any in ammonium ceric nitrate, potassium permanganate, potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate, hydrogen peroxide, benzoyl peroxide, the lauroyl peroxide for use.
5. Glucomannan fiber according to claim 1; It is characterized in that described grafted monomers is selected one or more the combination in any in acrylonitrile, acrylic acid, styrene, acrylamide, methyl acrylate, butyl acrylate, the vinyl acetate for use.
6. prepare the method for the described Glucomannan fiber of claim 1, the steps include:
The first step, by weight getting 10～30 parts of purifying Glucomannans, 50% ethanol stirs swelling 1h for 100～200 parts under the normal temperature in agitated reactor; Be warming up to 50 ℃ then; Add 0.01～2.0 part of initator, reaction 10～30min adds 1～10.0 part of grafted monomers then; At 30～90 ℃, and under the N2 protective condition, react 0.5～6h;
Second step added 1%～10% sodium hydroxide solution and stirs, and transferred pH to neutral, promptly obtained spinning solution;
The 3rd step, with spinning solution filter, after the deaeration, adopting diameter is that the spinning head of 0.1～0.5mm sprays into alcohol solidification and makes its coagulation forming in bathing, and behind water wash, at 50～70 ℃ of down dry 0.5～1h, promptly obtains the Glucomannan fiber.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102926016A (en) * | 2012-10-31 | 2013-02-13 | 西南科技大学 | Method for preparing modified konjac glucomannan fiber by electrostatic spinning |
| CN102926027A (en) * | 2012-10-31 | 2013-02-13 | 西南科技大学 | Method for preparing modified konjac glucomannan/biodegradation polyester polyblend fibers through electrostatic spinning |
| CN103263696A (en) * | 2013-06-08 | 2013-08-28 | 武汉纺织大学 | Novel catgut implantation at acupoint and preparation method thereof |
| CN105849326A (en) * | 2013-11-07 | 2016-08-10 | 纳幕尔杜邦公司 | Composition for preparing polysaccharide fibers |
| CN106215819A (en) * | 2016-08-03 | 2016-12-14 | 西南科技大学 | The preparation method of konjak portuguese gansu polyose gel microsphere |
| CN107326538A (en) * | 2017-06-22 | 2017-11-07 | 仲恺农业工程学院 | A kind of antibacterial water absorption cushion fresh-keeping for cold fresh meat and preparation method thereof |
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| CN101497678A (en) * | 2008-01-28 | 2009-08-05 | 西南科技大学 | Thermoplastic glucomannan and preparation thereof |
| CN101824166A (en) * | 2009-03-06 | 2010-09-08 | 西南科技大学 | Thermoplastic glucomannan/plant fiber blending material and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102926016A (en) * | 2012-10-31 | 2013-02-13 | 西南科技大学 | Method for preparing modified konjac glucomannan fiber by electrostatic spinning |
| CN102926027A (en) * | 2012-10-31 | 2013-02-13 | 西南科技大学 | Method for preparing modified konjac glucomannan/biodegradation polyester polyblend fibers through electrostatic spinning |
| CN102926016B (en) * | 2012-10-31 | 2014-12-03 | 西南科技大学 | Method for preparing modified konjac glucomannan fiber by electrostatic spinning |
| CN102926027B (en) * | 2012-10-31 | 2014-12-03 | 西南科技大学 | Method for preparing modified konjac glucomannan/biodegradation polyester polyblend fibers through electrostatic spinning |
| CN103263696A (en) * | 2013-06-08 | 2013-08-28 | 武汉纺织大学 | Novel catgut implantation at acupoint and preparation method thereof |
| CN103263696B (en) * | 2013-06-08 | 2015-01-21 | 武汉纺织大学 | Novel catgut implantation at acupoint and preparation method thereof |
| CN105849326A (en) * | 2013-11-07 | 2016-08-10 | 纳幕尔杜邦公司 | Composition for preparing polysaccharide fibers |
| CN106215819A (en) * | 2016-08-03 | 2016-12-14 | 西南科技大学 | The preparation method of konjak portuguese gansu polyose gel microsphere |
| CN106215819B (en) * | 2016-08-03 | 2019-01-22 | 西南科技大学 | The preparation method of konjak portuguese gansu polyose gel microsphere |
| CN107326538A (en) * | 2017-06-22 | 2017-11-07 | 仲恺农业工程学院 | A kind of antibacterial water absorption cushion fresh-keeping for cold fresh meat and preparation method thereof |
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Application publication date: 20120314 |