CN100585064C - Functional fiber preparation method - Google Patents

Functional fiber preparation method Download PDF

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Publication number
CN100585064C
CN100585064C CN200710164712A CN200710164712A CN100585064C CN 100585064 C CN100585064 C CN 100585064C CN 200710164712 A CN200710164712 A CN 200710164712A CN 200710164712 A CN200710164712 A CN 200710164712A CN 100585064 C CN100585064 C CN 100585064C
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China
Prior art keywords
cyclodextrin
weight
chitin fiber
list aldehyde
acetone
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CN200710164712A
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CN101187162A (en
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胡智文
温会涛
万军民
陈文兴
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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Abstract

The invention relates to a process for preparing functional fabric, which grafts cyclodextrin into the chitose fabric and includes Levofloxacin Hydrochloride to prepare the antibiotic and anti-infection functional fabric product with slow release property. The process can be used for preparing functional fabric and dressing for treatment of skin bacterial infection, genital system and gynaecologic infection, such as antibiotic and anti-infection sanitary towel.

Description

A kind of preparation method of functional fibre
Technical field
That the present invention relates to is a kind of preparation method who utilizes chitin fiber and derivative thereof to make functional fibre, belongs to the textile fabric preparing technical field.
Background technology
Chitin fiber is to extract from marine organisms, is a kind of tencel that forms with the chitin solution of deacetylation spinning.Because there is active-NH in a large number in it 2,-OH, nontoxic, easily degrade, thereby obtained extensive use at aspects such as biological medicine, Industrial Wastewater Treatment, heavy metal ion recovery.
Cyclodextrin (be called for short CD) is the cyclic oligomer sugar compounds that is linked to each other with α-1,4 type glycosidic linkage by six above glucopyranose units, according to glucose unit number (6,7,8) can be divided into α-, β-, γ-CD etc.Its notable attribute is that to have a ring outer hydrophilic, and is hydrophobic and the three-dimensional chirality cavity microenvironment of certain size arranged in the ring, can the suitable organic molecule of envelope size, so it can form the Subjective and Objective super molecular compounds with a lot of organic matters.
Lavo-ofloxacin (Levofloxacn, LVLX, commodity are called Cravit) be Ofloxacin (Ofloxacin, OFLX) laevoisomer, have another name called ofloxacin, be complete synthetic the 3rd generation quinolones broad-spectrum high efficacy antimicrobial, have characteristics such as has a broad antifungal spectrum, antibacterial action is strong, bad reaction is little, its external preparation can be used for treating that the skin bacterium sexuality is dyed, reproductive system and gynecological infection.
Announce that in " Zhejiang Polytechnical University's journal " the 2nd phase in 2004 " the levofloxacin slow release microballoon preparation that shitosan is matrix " literary composition is arranged, disclose the technology such as sustained-release micro-spheres of utilizing the Chitosan Preparation lavo-ofloxacin in the literary composition.
Summary of the invention
The object of the present invention is to provide a kind of by in chitin fiber by grafting introduce cyclodextrin, and with its inclusion lavo-ofloxacin, make have sustained release performance the preparation method of a kind of antibiotic and anti-infectious functional fibre.This method is: A) be 1: 8~10 to put into dimethyl sulfoxide (DMSO) and dissolve by weight with cyclodextrin; Be 1: 1~1.6 adding neighbour-iodoxy benzoic acid by cyclodextrin and the benzoic mol ratio of neighbour-iodoxy then, reacted 20~28 hours down at 20~30 ℃, stir, the elimination insoluble matter adds proper amount of acetone, separates out white solid, filter, with the white solid that obtains acetone washes clean, after freeze drying, obtain cyclodextrin list aldehyde;
B) be 1: 1~23 to put into 0.1% sodium carbonate liquor swelling 0.5~5 hour by weight with chitin fiber; Be washed with distilled water to neutrality, dry;
C) being that 1: 30~50 to put into the pH value be in 5~7 the aqueous solution by weight with the chitin fiber after the swelling, is 1: 0.8~1.4 to add cyclodextrin list aldehyde by the weight ratio of chitin fiber and cyclodextrin list aldehyde, and vibration is 20~30 ℃ of reactions 1~3 hour down;
D) be in 1: 1~3 input reactant liquors with the reductant sodium cyanoborohydride by cyclodextrin list aldehyde and sodium cyanoborohydride mol ratio, keep other reaction conditions constant, reacted 6~8 days, question response finishes the back and regulates pH to alkaline, respectively with distilled water and acetone washing;
E) will handle through the product drying that obtains after the above-mentioned reaction after, be that 1: 10~100 lavo-ofloxacin solution of putting into 5~50mg/L were handled 6-12 hour by weight, pull product out drying and handle, obtain functional fibre.
It can be beta-schardinger dextrin-or gamma-cyclodextrin that benzene is invented described cyclodextrin.
Functional fibre of the present invention can be used for the treatment of that the skin bacterium sexuality is dyed, functional fibre, the dressing of reproductive system and gynecological infection, as antibiotic, anti-infective sanitary napkin etc.
The present invention compared with prior art has following outstanding advantage: 1) utilize the three-dimensional chirality hydrophobic cavity of cyclodextrin to the inclusion of lavo-ofloxacin and slow-release function can controlled pharmacy thing release, further bring into play its drug effect, reduce side effect; 2) can improve availability to medicine; 3) fiber can be made different shape by braiding, cutting, and is easy to use.
The specific embodiment
Embodiment 1:A) be to put into dimethyl sulfoxide (DMSO) at 1: 8 to dissolve by weight with beta-schardinger dextrin-; Be 1: 1 adding neighbour-iodoxy benzoic acid by cyclodextrin and the benzoic mol ratio of neighbour-iodoxy then, reacted 20 hours down at 20 ℃, stir, the elimination insoluble matter adds proper amount of acetone, separates out white solid, filter, with the white solid that obtains acetone washes clean, after freeze drying, obtain cyclodextrin list aldehyde;
B) be to put into 0.1% sodium carbonate liquor swelling at 1: 1 0.5 hour by weight with chitin fiber; Be washed with distilled water to neutrality, dry;
C) being that to put into the pH value at 1: 30 be in 5 the aqueous solution by weight with the chitin fiber after the swelling, is to add cyclodextrin list aldehyde at 1: 0.8 by the weight ratio of chitin fiber and cyclodextrin list aldehyde, and vibration is 20 ℃ of reactions 1 hour down;
D) be to drop in reactant liquor at 1: 1 the reductant sodium cyanoborohydride by cyclodextrin list aldehyde and sodium cyanoborohydride mol ratio, keep other reaction conditions constant, react 6 days, question response finishes the back and regulates pH to alkalescence, washs with distilled water and acetone respectively;
E) will handle through the product drying that obtains after the above-mentioned reaction after, be that the lavo-ofloxacin solution of putting into 5mg/L at 1: 10 was handled 6 hours by weight, pull product out drying and handle, obtain functional fibre.
Embodiment 2, A) with gamma-cyclodextrin are by weight to put into dimethyl sulfoxide (DMSO) at 1: 10 to dissolve; Be 1: 1.6 adding neighbour-iodoxy benzoic acid by cyclodextrin and the benzoic mol ratio of neighbour-iodoxy then, reacted 28 hours down at 30 ℃, stir, the elimination insoluble matter adds proper amount of acetone, separates out white solid, filter, with the white solid that obtains acetone washes clean, after freeze drying, obtain cyclodextrin list aldehyde;
B) be to put into 0.1% sodium carbonate liquor swelling at 1: 23 5 hours by weight with chitin fiber; Be washed with distilled water to neutrality, dry;
C) being that to put into the pH value at 1: 50 be in 7 the aqueous solution by weight with the chitin fiber after the swelling, is to add cyclodextrin list aldehyde at 1: 1.4 by the weight ratio of chitin fiber and cyclodextrin list aldehyde, and vibration is 30 ℃ of reactions 3 hours down;
D) be to drop in reactant liquor at 1: 3 the reductant sodium cyanoborohydride by cyclodextrin list aldehyde and sodium cyanoborohydride mol ratio, keep other reaction conditions constant, react 8 days, question response finishes the back and regulates pH to alkalescence, washs with distilled water and acetone respectively;
E) will handle through the product drying that obtains after the above-mentioned reaction after, be that the lavo-ofloxacin solution of putting into 50mg/L at 1: 100 was handled 12 hours by weight, pull product out drying and handle, obtain functional fibre.
Embodiment 3, A) with cyclodextrin are by weight to put into dimethyl sulfoxide (DMSO) at 1: 8.8 to dissolve; Be 1: 1.3 adding neighbour-iodoxy benzoic acid by cyclodextrin and the benzoic mol ratio of neighbour-iodoxy then, reacted 24 hours down at 25 ℃, stir, the elimination insoluble matter adds proper amount of acetone, separates out white solid, filter, with the white solid that obtains acetone washes clean, after freeze drying, obtain cyclodextrin list aldehyde;
B) be to put into 0.1% sodium carbonate liquor swelling at 1: 12 2 hours by weight with chitin fiber; Be washed with distilled water to neutrality, dry;
C) being that to put into the pH value at 1: 40 be in 6 the aqueous solution by weight with the chitin fiber after the swelling, is to add cyclodextrin list aldehyde at 1: 1.1 by the weight ratio of chitin fiber and cyclodextrin list aldehyde, and vibration is 25 ℃ of reactions 2 hours down;
D) be to drop in reactant liquor at 1: 2 the reductant sodium cyanoborohydride by cyclodextrin list aldehyde and sodium cyanoborohydride mol ratio, keep other reaction conditions constant, react 7 days, question response finishes the back and regulates pH to alkalescence, washs with distilled water and acetone respectively;
E) will handle through the product drying that obtains after the above-mentioned reaction after, be that the lavo-ofloxacin solution of putting into 30mg/L at 1: 50 was handled 8 hours by weight, pull product out drying and handle, obtain functional fibre.

Claims (2)

1, a kind of preparation method of functional fibre, this method is: A) be 1: 8~10 to put into dimethyl sulfoxide (DMSO) and dissolve by weight with cyclodextrin; Be 1: 1~1.6 adding neighbour-iodoxy benzoic acid by cyclodextrin and the benzoic mol ratio of neighbour-iodoxy then, reacted 20~28 hours down at 20~30 ℃, stir, the elimination insoluble matter adds proper amount of acetone, separates out white solid, filter, with the white solid that obtains acetone washes clean, after freeze drying, obtain cyclodextrin list aldehyde;
B) be 1: 1~23 to put into 0.1% sodium carbonate liquor swelling 0.5~5 hour by weight with chitin fiber; Be washed with distilled water to neutrality, dry;
C) being that 1: 30~50 to put into the pH value be in 5~7 the aqueous solution by weight with the chitin fiber after the swelling, is 1: 0.8~1.4 to add cyclodextrin list aldehyde by the weight ratio of chitin fiber and cyclodextrin list aldehyde, and vibration is 20~30 ℃ of reactions 1~3 hour down;
D) be in 1: 1~3 input reactant liquors with the reductant sodium cyanoborohydride by cyclodextrin list aldehyde and sodium cyanoborohydride mol ratio, keep other reaction conditions constant, reacted 6~8 days, question response finishes the back and regulates pH to alkaline, respectively with distilled water and acetone washing;
E) will handle through the product drying that obtains after the above-mentioned reaction after, be that 1: 10~100 lavo-ofloxacin solution of putting into 5~50mg/L were handled 6-12 hour by weight, pull product out drying and handle, obtain functional fibre.
2, the preparation method of functional fibre according to claim 1 is characterized in that described cyclodextrin is a kind of in beta-schardinger dextrin-and the gamma-cyclodextrin.
CN200710164712A 2007-12-06 2007-12-06 Functional fiber preparation method Expired - Fee Related CN100585064C (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102505470A (en) * 2011-10-31 2012-06-20 中国人民解放军军事医学科学院卫生装备研究所 Preparation method of antibacterial function fiber
CN111840632A (en) * 2019-04-25 2020-10-30 广东泰宝医疗科技股份有限公司 Liquid dressing containing hemostatic microcapsule and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1490349A (en) * 2002-10-15 2004-04-21 浙江大学 Preparation of chitin-beta-cyclodextrin resin
JP2005264392A (en) * 2004-03-19 2005-09-29 Ishikawa Pref Gov Treating agent for synthetic fiber fabric, method for producing functional synthetic fiber fabric using the treating agent for synthetic fiber fabric, and functional synthetic fiber fabric

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1490349A (en) * 2002-10-15 2004-04-21 浙江大学 Preparation of chitin-beta-cyclodextrin resin
JP2005264392A (en) * 2004-03-19 2005-09-29 Ishikawa Pref Gov Treating agent for synthetic fiber fabric, method for producing functional synthetic fiber fabric using the treating agent for synthetic fiber fabric, and functional synthetic fiber fabric

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