CN102605672B - High-porosity chitosan/macromolecule blending thin film felt and preparation method thereof - Google Patents

High-porosity chitosan/macromolecule blending thin film felt and preparation method thereof Download PDF

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CN102605672B
CN102605672B CN201210109417.2A CN201210109417A CN102605672B CN 102605672 B CN102605672 B CN 102605672B CN 201210109417 A CN201210109417 A CN 201210109417A CN 102605672 B CN102605672 B CN 102605672B
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shitosan
wadding
cotton
quilt
fine
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CN102605672A (en
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杨庆
郯志清
沈新元
吉亚丽
吴文华
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Donghua University
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Donghua University
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Abstract

The invention relates to a high-porosity chitosan/macromolecule blending thin film felt and a preparation method thereof. The blending thin film felt is a film structure formed by stacking various flocculent fibers in a mixed manner. The preparation method comprises the following steps of: (1) putting chitosan into an acetic acid water solution so as to prepare chitosan pulp; (2) dissolving sodium hydroxide, urea and zinc acetate in water to be used as chitosan coagulating liquid; (3) spraying the chitosan pulp to the coagulating liquid at a high-speed stirring condition, so as to the coagulating liquid to coagulate to be chitosan flocculent fibers, and diffusing the chitosan flocculent fibers in deionized water after filtering and water washing so as to form chitosan flocculent fiber suspension supernatant; (4) carrying out the steps (1)-(3) to prepare corresponding macromolecule flocculent fiber suspension supernatant by using a certain macromolecule raw material; (5) mixing the chitosan flocculent fiber suspension supernatant with the macromolecule flocculent fiber suspension supernatant at a proper ratio, and then picking obtained blending thin film felt out by using a filter screen; and (6) deeply freezing and sublimating the thin film felt after water on the surface of the thin film felt is drained, so as to obtain the high-porosity chitosan/macromolecule blending thin film felt. The material has good solution adsorbability and is suitable for being used as wound dressing.

Description

A kind of high porosity shitosan/polymer blended film felt and preparation method thereof
Technical field
The present invention relates to a kind of high porosity shitosan/polymer blended film felt and preparation method thereof.
Background technology
Shitosan is the product of chitin N-deacetylation, and its chemical name is β-(1 → 4)-2-amino-2-deoxy-D-Glucose.Pure chitosan is translucent, the tasteless odorless avirulence of a kind of white, slightly nacreous powdery solid; can be hydrolyzed under given conditions, the chemical reaction such as alkylation, acyl group, carboxy methylation, sulfonation, nitrated, halogenation, oxidation, reduction, condensation and complexing; can generate the chitosan derivatives with different performance, expand the range of application of shitosan.
Shitosan has good physiologically active, energy Antibacterial activity, activating machine system, absorption and excretion heavy metal, maintenance immune effect and dissolubility etc.Shitosan also has other special purpose, shitosan as special in cosmetics, the special shitosan of flocculant, agriculture feed and the special shitosan of bait, the special shitosan of tobacco smoked sheet etc.Shitosan also has extensive use aspect food, as antiseptic, fruit and vegetable fresh-keeping agent, antioxidant, food supplement, clarification of water agent, enzyme immobilization agent etc.The application of shitosan aspect medical science mainly contains: styptic, Wound filling, bactericidal agent, Wound-healing agent, medicinal slow release agent, dental filling, artificial blood vessel, wound ulcer dressing, operation suture thread etc.
In shitosan application, one of modal form is fiber and fabric nonwoven cloth.The spinning of chitin fiber has various ways, the most generally wet spinning.The people such as Hu Qiaoling are dissolved shitosan as spinning solution taking basic solvent, shitosan macromolecular chain is existed with height solvent swelling state, macromolecular chain is arranged tightr, overcome shitosan unsure state in acid solution, guarantee that shitosan macromolecular chain is not hydrolyzed and glycosidic bond does not rupture, the mechanical property of chitin fiber is improved [Hu Qiaoling etc., a kind of preparation method (201110099174.4) of chitin fiber].Medical chitosan fibre is prepared with wet spinning process by Zhou Jia villages etc., chitosan powder is placed in to glacial acetic acid aqueous solution temp-controlling and time-controlling under stirring condition slowly to be dissolved, shitosan content > 99.9%[Zhou Jia village in the chitin fiber of making etc., medical chitosan fibre and preparation method thereof (200810015053.5)].The people such as Yu Shitao adopt ionic liquid aqueous solution as solvent, slowly add shitosan powder, after stirring, filtration, deaeration, obtain concentration and be 3～7.5% homogeneous phase transparent spinning solution, adopt subsequently conventional wet spinning process to obtain chitin fiber [Yu Shitao etc., a kind of preparation method (200910138811.7) of chitin fiber].
In recent years, method of electrostatic spinning is used to spin chitosan ultrafine fiber.The people such as Xu Xiongli are taking formic acid as solvent, after being mixed according to a certain percentage with shitosan slurries, gelatin solution adds silver nitrate, gelatin/chitosan/the liquor argenti nitratis ophthalmicus of gained is carried out to electrostatic spinning, prepared composite nanometer fiber felt containing nano silver gelatin/chitosan can be used as medical dressing [Xu Xiongli etc., for medical dressing composite nanometer fiber felt containing nano silver gelatin/chitosan and preparation (200710171324.1)].The people such as Huang little Jun are dissolved in shitosan and polyvinyl alcohol in the mixed solvent of glacial acetic acid and water and form clear solution, make chitosan nano fiber composite membrane by method of electrostatic spinning, and carrier using it as enzyme immobilization, [Huang little Jun etc., a kind of preparation method (200610154566.5) of chitosan nano fiber composite film immobilized enzyme].The people such as Wu great Yong prepare chitosan nano fiber membrane with method of electrostatic spinning, this tunica fibrosa is soaked, is cleaned in alkaline solution and dry processing after obtain chitosan nano fibrous membrane adsorbing material, the heavy metal ion [Wu great Yong etc., chitosan nano fibrous membrane adsorbing material and preparation method thereof (201110146164.1)] such as this material can efficient adsorption Cu (II), Hg (II), Cd (II) and Pb (II).
The wet spinning process of chitin fiber be use the most extensively, be also the most traditional spinning process, whole spinning technique route is too tediously long, production cost is very high; Although method of electrostatic spinning can obtain superfine fibre, output is extremely low.It is simple that copy paper method of the present invention is prepared the method technological process of shitosan and shitosan/polymer blended film felt thereof, equipment investment is few, and due to copy paper film felt has been adopted to freeze drying, the copy paper film felt obtaining is high porosity structure, water absorbing properties is extremely strong, is suitable for surface of a wound auxiliary material.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of high porosity shitosan/polymer blended film felt and preparation method thereof, and this blend film felt has good solution adsorptivity, biocidal property and strength and elongation, can be for the treatment of human body surface wound; And preparation method is simple, be suitable for suitability for industrialized production.
A kind of high porosity shitosan of the present invention/polymer blended film felt, described high porosity shitosan/polymer blended film felt is the high voidage membrane structure that shitosan wadding is fine and the fine accumulation of macromolecule wadding forms; Its mass ratio is that shitosan wadding is fine: macromolecule wadding fibre=99.9: 0.1～50: 50; Described wadding fibre refers to cotton-shaped short fiber, and described cotton-shaped short fiber refers to little and loose short fiber coagula; The voidage of described high porosity shitosan/polymer blended film felt is 30～80 (V/V) %.
As preferred technical scheme:
A kind of high porosity shitosan as above/polymer blended film felt, described macromolecule is one or more mixing in polycaprolactone, polyethylene glycol, polytetramethylene carbonate diol, PLA and cellulose.
A kind of high porosity shitosan as above/polymer blended film felt, described cotton-shaped short fiber sprays solidification forming by slurries to the coagulating bath under high-speed stirred and obtains; Described high voidage membrane structure adopts freeze-drying to make.
The present invention also provides the preparation method of a kind of high porosity shitosan/polymer blended film felt, comprises the following steps:
(1) shitosan slurries preparation: it is to dissolve and make shitosan slurries in 2～8 (V/V) % acetic acid that shitosan powder is invested in to concentration, and the shitosan content in described shitosan slurries is 0.5～5.0 (W/W) %;
(2) shitosan solidification liquid preparation: NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; In described shitosan solidification liquid, naoh concentration is 4～12 (W/W) %, and urea concentration is 0.5～1.0 (W/W) %, and zinc acetate concentration is 0.1～0.5 (W/W) %;
(3) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton under high-speed stirred; The described shitosan fine suspension of wadding a quilt with cotton is made up of cotton-shaped shitosan short fiber and suspension, and described cotton-shaped shitosan short fiber is suspended in suspension; Described cotton-shaped shitosan short fiber refers to little and loose shitosan short fiber coagula; The shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtaining cotton-shaped shitosan short fiber is that shitosan wadding is fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1～5 (W/W) %;
(4) macromolecule raw material of appropriate ratio is invested in corresponding solvent and makes Polymer Solution; Allocate the solidification liquid of corresponding Polymer Solution;
(5) under high-speed stirred, spray Polymer Solution to solidification liquid, make it be frozen into the macromolecule fine suspension of wadding a quilt with cotton;
(6) the fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtaining cotton-shaped polymeric staple fiber is that macromolecule wadding is fine;
(7) fibre of again macromolecule being wadded a quilt with cotton is dispersed in and in deionized water, forms the macromolecule fine suspension clear liquid of wadding a quilt with cotton, and its concentration is 0.1～5 (W/W) %;
(8) shitosan is wadded a quilt with cotton fine suspension clear liquid and macromolecule wadded a quilt with cotton fine suspension clear liquid with 1～9: 9～1 weight ratio mixing and stirring, with filter screen, the mixing wadding fibre in suspension is taken up, and obtain one deck by mixing the fine blend film felt forming of wadding;
(9) after the dry surface moisture of film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain high porosity shitosan/polymer blended film felt.
The preparation method of a kind of high porosity shitosan/polymer blended film felt as above, described macromolecule raw material is polycaprolactone, polyethylene glycol, polytetramethylene carbonate diol, PLA or cellulose; Described coordinative solvent and the mass concentration of making Polymer Solution are: for polycaprolactone, solvent is oxolane, and concentration is 3～30% (W/W) %; For polyethylene glycol, molecular weight is 2000～20000, and solvent is 75 ± 5 DEG C of hot water, and concentration is 3～30% (W/W) %; For polytetramethylene carbonate diol, solvent is dimethyl formamide, and concentration is 3～30 (W/W) %; For PLA, solvent is carrene, and concentration is 3～30 (W/W) %; For cellulose, solvent is 4-methyl morpholine-N-oxide, and concentration is 1～10 (W/W) %.
The preparation method of a kind of high porosity shitosan/polymer blended film felt as above, described solidification liquid is allocated as: for polycaprolactone/tetrahydrofuran solution, solidification liquid is 25 ± 2 DEG C of deionized waters; For the polyethylene glycol/75 ± 5 DEG C aqueous solution, solidification liquid is 25 ± 2 DEG C of deionized waters; For polytetramethylene carbonate diol/dimethyl formamide solution, solidification liquid is 25 ± 2 DEG C of deionized waters; For PLA/dichloromethane solution, solidification liquid is 25 ± 2 DEG C of deionized waters; For cellulose/4-methyl morpholine-N-oxide solution, solidification liquid is 25 ± 2 DEG C of deionized waters.
The preparation method of a kind of high porosity shitosan/polymer blended film felt as above, it is 100～1000rpm that described high-speed stirred refers to speed of agitator interval; Described injection refers to: Polymer Solution is packed in the charging basket of Electronic spraying machine, open electric air pump Polymer Solution is sprayed into solidification liquid with the speed of 0.2～0.3l/min with vaporific form.
The preparation method of a kind of high porosity shitosan/polymer blended film felt as above, described filter operation is: first the Buchner funnel of having laid filter paper is inserted in to Bu Shi flask upper opening and by sealing joint, then pour fine the wadding that sprays solidification forming suspension into Buchner funnel, suspension is drawn into beaker under suction function, and the fine solid of wadding a quilt with cotton is stayed in Buchner funnel; Described dispersion is that fine the wadding through filtering solid is put into beaker, adds the deionized water fibre that makes to wad a quilt with cotton to be again dispersed in water; Can wash away the coagulating agent in original solution through filtration and dispersion repeatedly, fine suspension clear liquid obtains wadding a quilt with cotton.
The preparation method of a kind of high porosity shitosan/polymer blended film felt as above, described filter screen is the diddle-net that a kind of copy paper is used, and filter screen material is stainless steel, and mesh size is 200～400 orders; Described cryogenic refrigeration refers to and sample is refrigerated to-40～-50 DEG C, and the moisture content containing has become ice cube; Described distillation is freezing to be carried out in vacuum freeze drier, and distillation refrigerating process is: freeze-drying time is 48 ± 2 hours, freeze-drying pressure 80 ± 5Pa, 60 ± 2 DEG C of temperature of heating plate.
The present invention provides again the preparation method of a kind of high porosity shitosan/polymer blended film felt, by two or more the macromolecule making by above-mentioned steps (4)～(7) the fine suspension clear liquid blend of wadding a quilt with cotton, then obtain the polymer blended film felt of high porosity shitosan/multicomponent by step (7)～(8) operation.
Traditional chitosan short fiber film felt production process route is very long, conventionally will experience: shitosan dissolves, and------spray silk--solidify-slubbing stretching-drawing and setting--washing-coiling long fiber-cut-out-staple fibre--shredding-lapping-chitosan short fiber film felt is measured-refiltered to stoste--in filtration.Long process route causes cost to improve, and invests greatly, makes basic material come from the chitin fiber market price of discarded shrimp shell, crab shell high.The preparation of polymeric staple fiber dimension film felt and nonwoven fabric will be experienced tediously long technical process equally, and technological process is conventionally: macromolecule raw material-wet spinning (or melt spinning)--long fiber-cut-out-staple fibre--shredding-lapping-polymeric staple fiber dimension film felt.Though Static Spinning also can be used for preparing tunica fibrosa, also one step forming just from stoste to tunica fibrosa, and also fibre fineness reaches micron order, and its output is minimum, is difficult to substitute the market demand of conventional staple fibre film felt (nonwoven fabric).
The present invention has adopted a kind of new forming polymer method--spray-up method, has obtained the cotton-shaped shape short fiber that floats on a liquid, has produced after the film felt of high moisture percentage by copy paper method, adopts freezing and sublimation mode to remove moisture and retains the space in structure simultaneously.The advantage of this new material is to have very high porosity and good solution adsorptivity, is well suited for as wound dressing.In addition its preparation method is simple, and process route shortens greatly, and its typical process flow is: the fine fine cleaning-copy paper shaping-freeze drying-wadding fibrous film felt that is shaped-wads a quilt with cotton of slurries preparation-wadding.
Beneficial effect:
(1) shitosan of the present invention/polymer blended film felt is the high-voidage membrane structure forming with wadding fibrous accumulation, has good strength and elongation, and maximum feature is that voidage is high, and absorbency is good, is well suited for as wound dressing.Its preparation method is simple, and cost is low, environmentally friendly, and economic benefit is high.
(2) one of key of the present invention: shitosan and high molecular slurries are to enter coagulating bath under high-speed stirred and solidified forming by spray regime.
(3) two of key of the present invention: adopt copy paper method to prepare blend film felt, prepare tunica fibrosa with conventional wet spinning process compared with, its technological process is shortened greatly.
(4) three of key of the present invention: nascent blend film felt is carried out to freeze drying, and the final products of gained have high porosity and pick up.
Detailed description of the invention
Below in conjunction with detailed description of the invention, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and polycaprolactone, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 2 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 0.5 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 4 (W/W) %, and urea concentration is 0.5 (W/W) %, and zinc acetate concentration is 0.1 (W/W) %; Under stirring, the rotating speed of 100rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(2) the polycaprolactone fine suspension clear liquid preparation of wadding a quilt with cotton: polycaprolactone is invested in and makes the polycaprolactone solution that concentration is 3% (W/W) % in oxolane; Solidification liquid is 23 DEG C of deionized waters; Under the rotating speed of 100rpm stirs, spray polycaprolactone slurries to polycaprolactone solidification liquid, make it be frozen into the polycaprolactone fine suspension of wadding a quilt with cotton; This polycaprolactone fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polycaprolactone wadding fine; The fibre of again polycaprolactone being wadded a quilt with cotton is dispersed in and in deionized water, forms the polycaprolactone fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and polycaprolactone wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 2: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polycaprolactone.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/polycaprolactone.
Embodiment 2
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and polycaprolactone, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 8 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 5.0 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 12 (W/W) %, and urea concentration is 1.0 (W/W) %, and zinc acetate concentration is 0.5 (W/W) %; Under stirring, the rotating speed of 1000rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(2) the polycaprolactone fine suspension clear liquid preparation of wadding a quilt with cotton: polycaprolactone is invested in and makes the polycaprolactone solution that concentration is 30% (W/W) % in oxolane; Solidification liquid is 27 DEG C of deionized waters; Under the rotating speed of 1000rpm stirs, spray polycaprolactone slurries to polycaprolactone solidification liquid, make it be frozen into the polycaprolactone fine suspension of wadding a quilt with cotton; This polycaprolactone fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polycaprolactone wadding fine; The fibre of again polycaprolactone being wadded a quilt with cotton is dispersed in and in deionized water, forms the polycaprolactone fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and polycaprolactone wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 3: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polycaprolactone.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/polycaprolactone.
Embodiment 3
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and polycaprolactone, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 5 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 3 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 8 (W/W) %, and urea concentration is 0.7 (W/W) %, and zinc acetate concentration is 0.3 (W/W) %; Under stirring, the rotating speed of 500rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(2) the polycaprolactone fine suspension clear liquid preparation of wadding a quilt with cotton: polycaprolactone is invested in and makes the polycaprolactone solution that concentration is 15% (W/W) % in oxolane; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray polycaprolactone slurries to polycaprolactone solidification liquid, make it be frozen into the polycaprolactone fine suspension of wadding a quilt with cotton; This polycaprolactone fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polycaprolactone wadding fine; The fibre of again polycaprolactone being wadded a quilt with cotton is dispersed in and in deionized water, forms the polycaprolactone fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and polycaprolactone wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 2.5: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polycaprolactone.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/polycaprolactone.
Embodiment 4
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and polyethylene glycol, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 2 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 0.5 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 4 (W/W) %, and urea concentration is 0.5 (W/W) %, and zinc acetate concentration is 0.1 (W/W) %; Under stirring, the rotating speed of 100rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(2) the polyethylene glycol fine suspension clear liquid preparation of wadding a quilt with cotton: the polyethylene glycol that is 10000 by molecular weight is invested in and makes the polyglycol solution that concentration is 3% (W/W) % in 70 DEG C of hot water; Solidification liquid is 23 DEG C of deionized waters; Under the rotating speed of 100rpm stirs, spray polyethylene glycol slurries to polyethylene glycol solidification liquid, make it be frozen into the polyethylene glycol fine suspension of wadding a quilt with cotton; This polyethylene glycol fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polyethylene glycol wadding fine; The fibre of again polyethylene glycol being wadded a quilt with cotton is dispersed in and in deionized water, forms the polyethylene glycol fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and polyethylene glycol wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 2: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polyethylene glycol.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/polyethylene glycol.
Embodiment 5
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and polyethylene glycol, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 8 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 5.0 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 12 (W/W) %, and urea concentration is 1.0 (W/W) %, and zinc acetate concentration is 0.5 (W/W) %; Under stirring, the rotating speed of 1000rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(2) the polyethylene glycol fine suspension clear liquid preparation of wadding a quilt with cotton: the polyethylene glycol that is 10000 by molecular weight is invested in and makes the polyglycol solution that concentration is 30% (W/W) % in 80 DEG C of hot water; Solidification liquid is 27 DEG C of deionized waters; Under the rotating speed of 1000rpm stirs, spray polyethylene glycol slurries to polyethylene glycol solidification liquid, make it be frozen into the polyethylene glycol fine suspension of wadding a quilt with cotton; This polyethylene glycol fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polyethylene glycol wadding fine; The fibre of again polyethylene glycol being wadded a quilt with cotton is dispersed in and in deionized water, forms the polyethylene glycol fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and polyethylene glycol wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 3: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polyethylene glycol.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/polyethylene glycol.
Embodiment 6
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and polyethylene glycol, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 5 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 3 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 8 (W/W) %, and urea concentration is 0.7 (W/W) %, and zinc acetate concentration is 0.3 (W/W) %; Under stirring, the rotating speed of 500rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(2) the polyethylene glycol fine suspension clear liquid preparation of wadding a quilt with cotton: the polyethylene glycol that is 10000 by molecular weight is invested in and makes the polyglycol solution that concentration is 15% (W/W) % in 75 DEG C of hot water; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray polyethylene glycol slurries to polyethylene glycol solidification liquid, make it be frozen into the polyethylene glycol fine suspension of wadding a quilt with cotton; This polyethylene glycol fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polyethylene glycol wadding fine; The fibre of again polyethylene glycol being wadded a quilt with cotton is dispersed in and in deionized water, forms the polyethylene glycol fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and polyethylene glycol wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 2.5: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polyethylene glycol.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/polyethylene glycol.
Embodiment 7
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and polytetramethylene carbonate diol, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 2 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 0.5 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 4 (W/W) %, and urea concentration is 0.5 (W/W) %, and zinc acetate concentration is 0.1 (W/W) %; Under stirring, the rotating speed of 100rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(2) the polytetramethylene carbonate diol fine suspension clear liquid preparation of wadding a quilt with cotton: polytetramethylene carbonate diol is invested in and makes the polytetramethylene carbonate diol solution that concentration is 3% (W/W) % in dimethyl formamide; Solidification liquid is 23 DEG C of deionized waters; Under the rotating speed of 100rpm stirs, spray polytetramethylene carbonate diol slurries to polytetramethylene carbonate diol solidification liquid, make it be frozen into the polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton; This polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polytetramethylene carbonate diol wadding fine; The fibre of again polytetramethylene carbonate diol being wadded a quilt with cotton is dispersed in and in deionized water, forms the polytetramethylene carbonate diol fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and polytetramethylene carbonate diol wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 2: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polytetramethylene carbonate diol.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/polytetramethylene carbonate diol.
Embodiment 8
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and polytetramethylene carbonate diol, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 8 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 5.0 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 12 (W/W) %, and urea concentration is 1.0 (W/W) %, and zinc acetate concentration is 0.5 (W/W) %; Under stirring, the rotating speed of 1000rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(2) the polytetramethylene carbonate diol fine suspension clear liquid preparation of wadding a quilt with cotton: polytetramethylene carbonate diol is invested in and makes the polytetramethylene carbonate diol solution that concentration is 30% (W/W) % in dimethyl formamide; Solidification liquid is 27 DEG C of deionized waters; Under the rotating speed of 1000rpm stirs, spray polytetramethylene carbonate diol slurries to polytetramethylene carbonate diol solidification liquid, make it be frozen into the polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton; This polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polytetramethylene carbonate diol wadding fine; The fibre of again polytetramethylene carbonate diol being wadded a quilt with cotton is dispersed in and in deionized water, forms the polytetramethylene carbonate diol fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and polytetramethylene carbonate diol wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 3: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polytetramethylene carbonate diol.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/polytetramethylene carbonate diol.
Embodiment 9
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and polytetramethylene carbonate diol, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 5 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 3 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 8 (W/W) %, and urea concentration is 0.7 (W/W) %, and zinc acetate concentration is 0.3 (W/W) %; Under stirring, the rotating speed of 500rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(2) the polytetramethylene carbonate diol fine suspension clear liquid preparation of wadding a quilt with cotton: polytetramethylene carbonate diol is invested in and makes the polytetramethylene carbonate diol solution that concentration is 15% (W/W) % in dimethyl formamide; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray polytetramethylene carbonate diol slurries to polytetramethylene carbonate diol solidification liquid, make it be frozen into the polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton; This polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polytetramethylene carbonate diol wadding fine; The fibre of again polytetramethylene carbonate diol being wadded a quilt with cotton is dispersed in and in deionized water, forms the polytetramethylene carbonate diol fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and polytetramethylene carbonate diol wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 2.5: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polytetramethylene carbonate diol.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/polytetramethylene carbonate diol.
Embodiment 10
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and PLA, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 2 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 0.5 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 4 (W/W) %, and urea concentration is 0.5 (W/W) %, and zinc acetate concentration is 0.1 (W/W) %; Under stirring, the rotating speed of 100rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(2) the PLA fine suspension clear liquid preparation of wadding a quilt with cotton: PLA is invested in and makes the PLA solution that concentration is 3% (W/W) % in carrene; Solidification liquid is 23 DEG C of deionized waters; Under the rotating speed of 100rpm stirs, spray PLA slurries to PLA solidification liquid, make it be frozen into the PLA fine suspension of wadding a quilt with cotton; This PLA fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain PLA wadding fine; The fibre of again PLA being wadded a quilt with cotton is dispersed in and in deionized water, forms the PLA fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and PLA wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 2: 1, with filter screen, the mixing wadding fibre in suspension taken up, and obtains one deck and mixes the fine blend film felt forming of wadding by shitosan/PLA.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/PLA.
Embodiment 11
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and PLA, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 8 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 5.0 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 12 (W/W) %, and urea concentration is 1.0 (W/W) %, and zinc acetate concentration is 0.5 (W/W) %; Under stirring, the rotating speed of 1000rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(2) the PLA fine suspension clear liquid preparation of wadding a quilt with cotton: PLA is invested in and makes the PLA solution that concentration is 30% (W/W) % in carrene; Solidification liquid is 27 DEG C of deionized waters; Under the rotating speed of 1000rpm stirs, spray PLA slurries to PLA solidification liquid, make it be frozen into the PLA fine suspension of wadding a quilt with cotton; This PLA fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain PLA wadding fine; The fibre of again PLA being wadded a quilt with cotton is dispersed in and in deionized water, forms the PLA fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and PLA wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 3: 1, with filter screen, the mixing wadding fibre in suspension taken up, and obtains one deck and mixes the fine blend film felt forming of wadding by shitosan/PLA.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/PLA.
Embodiment 12
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and PLA, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 5 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 3 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 8 (W/W) %, and urea concentration is 0.7 (W/W) %, and zinc acetate concentration is 0.3 (W/W) %; Under stirring, the rotating speed of 500rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(2) the PLA fine suspension clear liquid preparation of wadding a quilt with cotton: PLA is invested in and makes the PLA solution that concentration is 15% (W/W) % in carrene; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray PLA slurries to PLA solidification liquid, make it be frozen into the PLA fine suspension of wadding a quilt with cotton; This PLA fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain PLA wadding fine; The fibre of again PLA being wadded a quilt with cotton is dispersed in and in deionized water, forms the PLA fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(3) shitosan is wadded a quilt with cotton fine suspension clear liquid and PLA wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 2.5: 1, with filter screen, the mixing wadding fibre in suspension taken up, and obtains one deck and mixes the fine blend film felt forming of wadding by shitosan/PLA.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity shitosan/PLA.
Embodiment 13
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and cellulose, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 2 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 0.5 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 4 (W/W) %, and urea concentration is 0.5 (W/W) %, and zinc acetate concentration is 0.1 (W/W) %; Under stirring, the rotating speed of 100rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(2) the fine suspension clear liquid preparation of cellulose wadding: cellulose is invested in and makes the cellulose solution that concentration is 3% (W/W) % in 4-methyl morpholine-N-oxide; Solidification liquid is 23 DEG C of deionized waters; Under stirring, the rotating speed of 100rpm to cellulose gel solid-liquid jet fiber element slurries, makes the fine suspension of its solidificating fiber element wadding; The fine suspension of this cellulose wadding is filtered, clean with deionized water, obtain cellulose wadding fibre; Cellulose wadding fibre is dispersed in deionized water again and forms the fine suspension clear liquid of cellulose wadding, its fine concentration of wadding a quilt with cotton is 0.1 (W/W) %.
(3) shitosan is wadded a quilt with cotton to the fine suspension clear liquid of fine suspension clear liquid and cellulose wadding with the weight ratio mixing and stirring of 2: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtain one deck and mix the fine blend film felt forming of wadding by Chitosan/Cellulose.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity Chitosan/Cellulose.
Embodiment 14
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and cellulose, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 8 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 5.0 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 12 (W/W) %, and urea concentration is 1.0 (W/W) %, and zinc acetate concentration is 0.5 (W/W) %; Under stirring, the rotating speed of 1000rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(2) the fine suspension clear liquid preparation of cellulose wadding: cellulose is invested in and makes the cellulose solution that concentration is 30% (W/W) % in 4-methyl morpholine-N-oxide; Solidification liquid is 27 DEG C of deionized waters; Under stirring, the rotating speed of 1000rpm to cellulose gel solid-liquid jet fiber element slurries, makes the fine suspension of its solidificating fiber element wadding; The fine suspension of this cellulose wadding is filtered, clean with deionized water, obtain cellulose wadding fibre; Cellulose wadding fibre is dispersed in deionized water again and forms the fine suspension clear liquid of cellulose wadding, its fine concentration of wadding a quilt with cotton is 0.2 (W/W) %.
(3) shitosan is wadded a quilt with cotton to the fine suspension clear liquid of fine suspension clear liquid and cellulose wadding with the weight ratio mixing and stirring of 3: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtain one deck and mix the fine blend film felt forming of wadding by Chitosan/Cellulose.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity Chitosan/Cellulose.
Embodiment 15
The two component blend film felt Preparation Methods of a kind of high porosity shitosan and cellulose, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 5 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 3 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 8 (W/W) %, and urea concentration is 0.7 (W/W) %, and zinc acetate concentration is 0.3 (W/W) %; Under stirring, the rotating speed of 500rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(2) the fine suspension clear liquid preparation of cellulose wadding: cellulose is invested in and makes the cellulose solution that concentration is 15% (W/W) % in 4-methyl morpholine-N-oxide; Solidification liquid is 25 DEG C of deionized waters; Under stirring, the rotating speed of 500rpm to cellulose gel solid-liquid jet fiber element slurries, makes the fine suspension of its solidificating fiber element wadding; The fine suspension of this cellulose wadding is filtered, clean with deionized water, obtain cellulose wadding fibre; Cellulose wadding fibre is dispersed in deionized water again and forms the fine suspension clear liquid of cellulose wadding, its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(3) shitosan is wadded a quilt with cotton to the fine suspension clear liquid of fine suspension clear liquid and cellulose wadding with the weight ratio mixing and stirring of 2.5: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtain one deck and mix the fine blend film felt forming of wadding by Chitosan/Cellulose.
(4) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain the two component blend film felts of high porosity Chitosan/Cellulose.
Embodiment 16
A kind of high porosity shitosan, polycaprolactone and polyethylene glycol three-component blend film felt Preparation Method, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 4 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 3.0 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 8 (W/W) %, and urea concentration is 0.7 (W/W) %, and zinc acetate concentration is 0.3 (W/W) %; Under stirring, the rotating speed of 500rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(2) the polycaprolactone fine suspension clear liquid preparation of wadding a quilt with cotton: polycaprolactone is invested in and makes the polycaprolactone solution that concentration is 15% (W/W) % in oxolane; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray polycaprolactone slurries to polycaprolactone solidification liquid, make it be frozen into the polycaprolactone fine suspension of wadding a quilt with cotton; This polycaprolactone fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polycaprolactone wadding fine; The fibre of again polycaprolactone being wadded a quilt with cotton is dispersed in and in deionized water, forms the polycaprolactone fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(3) the polyethylene glycol fine suspension clear liquid preparation of wadding a quilt with cotton: the polyethylene glycol that is 20000 by molecular weight is invested in and makes the polyglycol solution that concentration is 15% (W/W) % in 80 DEG C of hot water; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray polyethylene glycol slurries to polyethylene glycol solidification liquid, make it be frozen into the polyethylene glycol fine suspension of wadding a quilt with cotton; This polyethylene glycol fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polyethylene glycol wadding fine; The fibre of again polyethylene glycol being wadded a quilt with cotton is dispersed in and in deionized water, forms the polyethylene glycol fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(4) shitosan is wadded a quilt with cotton wad a quilt with cotton fine suspension clear liquid and polyethylene glycol of fine suspension clear liquid, polycaprolactone wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 3: 2: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polycaprolactone/polyethyleneglycol.
(5) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain high porosity shitosan/polycaprolactone/polyethyleneglycol three component blend film felts.
Embodiment 17
A kind of high porosity shitosan, polytetramethylene carbonate diol and PLA three-component blend film felt Preparation Method, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 5 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 3 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 8 (W/W) %, and urea concentration is 0.7 (W/W) %, and zinc acetate concentration is 0.3 (W/W) %; Under stirring, the rotating speed of 500rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(2) the polytetramethylene carbonate diol fine suspension clear liquid preparation of wadding a quilt with cotton: polytetramethylene carbonate diol is invested in and makes the polytetramethylene carbonate diol solution that concentration is 15% (W/W) % in dimethyl formamide; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray polytetramethylene carbonate diol slurries to polytetramethylene carbonate diol solidification liquid, make it be frozen into the polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton; This polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polytetramethylene carbonate diol wadding fine; The fibre of again polytetramethylene carbonate diol being wadded a quilt with cotton is dispersed in and in deionized water, forms the polytetramethylene carbonate diol fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(3) the PLA fine suspension clear liquid preparation of wadding a quilt with cotton: PLA is invested in and makes the PLA solution that concentration is 15% (W/W) % in carrene; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray PLA slurries to PLA solidification liquid, make it be frozen into the PLA fine suspension of wadding a quilt with cotton; This PLA fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain PLA wadding fine; The fibre of again PLA being wadded a quilt with cotton is dispersed in and in deionized water, forms the PLA fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(4) shitosan is wadded a quilt with cotton wad a quilt with cotton fine suspension clear liquid and PLA of fine suspension clear liquid, polytetramethylene carbonate diol wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 3: 2: 1, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine blend film felt forming of wadding by shitosan/polytetramethylene carbonate diol/PLA.
(5) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain high porosity shitosan/polytetramethylene carbonate diol/PLA three component blend film felts.
Embodiment 18
A kind of high porosity shitosan, polycaprolactone, polytetramethylene carbonate diol and cellulose four component blend film felt Preparation Methods, comprise the following steps:
(1) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: it is to dissolve and make shitosan slurries in 5 (V/V) % acetic acid that shitosan powder is invested in to concentration, and shitosan content is 3 (W/W) %; NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; Naoh concentration is 8 (W/W) %, and urea concentration is 0.7 (W/W) %, and zinc acetate concentration is 0.3 (W/W) %; Under stirring, the rotating speed of 500rpm to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton; This shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain shitosan wadding fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(2) the polycaprolactone fine suspension clear liquid preparation of wadding a quilt with cotton: polycaprolactone is invested in and makes the polycaprolactone solution that concentration is 15% (W/W) % in oxolane; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray polycaprolactone slurries to polycaprolactone solidification liquid, make it be frozen into the polycaprolactone fine suspension of wadding a quilt with cotton; This polycaprolactone fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polycaprolactone wadding fine; The fibre of again polycaprolactone being wadded a quilt with cotton is dispersed in and in deionized water, forms the polycaprolactone fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(3) the polytetramethylene carbonate diol fine suspension clear liquid preparation of wadding a quilt with cotton: polytetramethylene carbonate diol is invested in and makes the polytetramethylene carbonate diol solution that concentration is 15% (W/W) % in dimethyl formamide; Solidification liquid is 25 DEG C of deionized waters; Under the rotating speed of 500rpm stirs, spray polytetramethylene carbonate diol slurries to polytetramethylene carbonate diol solidification liquid, make it be frozen into the polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton; This polytetramethylene carbonate diol fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtain polytetramethylene carbonate diol wadding fine; The fibre of again polytetramethylene carbonate diol being wadded a quilt with cotton is dispersed in and in deionized water, forms the polytetramethylene carbonate diol fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(4) the fine suspension clear liquid preparation of cellulose wadding: cellulose is invested in and makes the cellulose solution that concentration is 5% (W/W) % in 4-methyl morpholine-N-oxide; Solidification liquid is 25 DEG C of deionized waters; Under stirring, the rotating speed of 500rpm to cellulose gel solid-liquid jet fiber element slurries, makes the fine suspension of its solidificating fiber element wadding; The fine suspension of this cellulose wadding is filtered, clean with deionized water, obtain cellulose wadding fibre; Cellulose wadding fibre is dispersed in deionized water again and forms the fine suspension clear liquid of cellulose wadding, its fine concentration of wadding a quilt with cotton is 0.15 (W/W) %.
(5) shitosan is wadded a quilt with cotton wad a quilt with cotton fine suspension clear liquid, polytetramethylene carbonate diol of fine suspension clear liquid, polycaprolactone wadded a quilt with cotton fine suspension clear liquid and the fine suspension clear liquid of cellulose wadding with 3: 2: 2: 1 weight ratio mixing and stirring, with filter screen, the mixing wadding fibre in suspension is taken up, obtained one deck and mix the fine four component blend film felts that form of wadding by shitosan/polycaprolactone/polytetramethylene carbonate diol/cellulose.
(6) after the dry surface moisture of blend film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain high porosity shitosan/polycaprolactone/polytetramethylene carbonate diol/cellulose four component blend film felts.

Claims (4)

1. a preparation method for high porosity shitosan/polymer blended film felt, is characterized in that comprising the following steps:
(1) shitosan slurries preparation: it is to dissolve and make shitosan slurries in 2～8 (V/V) % acetic acid that shitosan powder is invested in to concentration, and the shitosan content in described shitosan slurries is 0.5～5.0 (W/W) %;
(2) shitosan solidification liquid preparation: NaOH, urea and zinc acetate are invested in deionized water and stir and make shitosan solidification liquid; In described shitosan solidification liquid, naoh concentration is 4～12 (W/W) %, and urea concentration is 0.5～1.0 (W/W) %, and zinc acetate concentration is 0.1～0.5 (W/W) %;
(3) the shitosan fine suspension clear liquid preparation of wadding a quilt with cotton: to shitosan solidification liquid jetski glycan slurries, make it be frozen into the shitosan fine suspension of wadding a quilt with cotton under high-speed stirred; The described shitosan fine suspension of wadding a quilt with cotton is made up of cotton-shaped shitosan short fiber and suspension, and described cotton-shaped shitosan short fiber is suspended in suspension; Described cotton-shaped shitosan short fiber refers to little and loose shitosan short fiber coagula; The shitosan fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtaining cotton-shaped shitosan short fiber is that shitosan wadding is fine; The fibre of again shitosan being wadded a quilt with cotton is dispersed in and in deionized water, forms the shitosan fine suspension clear liquid of wadding a quilt with cotton, and its fine concentration of wadding a quilt with cotton is 0.1～5 (W/W) %;
(4) macromolecule raw material of appropriate ratio is invested in corresponding solvent and makes Polymer Solution; Allocate the solidification liquid of corresponding Polymer Solution;
(5) under high-speed stirred, spray Polymer Solution to solidification liquid, make it be frozen into the macromolecule fine suspension of wadding a quilt with cotton; It is 100～1000rpm that described high-speed stirred refers to speed of agitator interval;
(6) the fine suspension of wadding a quilt with cotton is filtered, clean with deionized water, obtaining cotton-shaped polymeric staple fiber is that macromolecule wadding is fine;
(7) fibre of again macromolecule being wadded a quilt with cotton is dispersed in and in deionized water, forms the macromolecule fine suspension clear liquid of wadding a quilt with cotton, and its concentration is 0.1～5 (W/W) %;
(8) shitosan is wadded a quilt with cotton fine suspension clear liquid and macromolecule wadded a quilt with cotton fine suspension clear liquid with the weight ratio mixing and stirring of 1～9:9～1, with filter screen, the mixing wadding fibre in suspension taken up, and obtains one deck by mixing the fine blend film felt forming of wadding;
(9) after the dry surface moisture of film felt filter of taking up, carry out cryogenic refrigeration, then it is distilled freezing, obtain high porosity shitosan/polymer blended film felt; Described high porosity shitosan/polymer blended film felt is the high voidage membrane structure that shitosan wadding is fine and the fine accumulation of macromolecule wadding forms; Its mass ratio is that shitosan wadding is fine: macromolecule wadding fibre=99.9:0.1～50:50; Described wadding fibre refers to cotton-shaped short fiber, and described cotton-shaped short fiber refers to little and loose short fiber coagula; The voidage of described high porosity shitosan/polymer blended film felt is 30～80 (V/V) %;
Described macromolecule raw material is polycaprolactone, polyethylene glycol, polytetramethylene carbonate diol, PLA or cellulose; Described coordinative solvent and the mass concentration of making Polymer Solution are: for polycaprolactone, solvent is oxolane, and concentration is 3～30% (W/W) %; For polyethylene glycol, molecular weight is 2000～20000, and solvent is 75 ± 5 DEG C of hot water, and concentration is 3～30% (W/W) %; For polytetramethylene carbonate diol, solvent is dimethyl formamide, and concentration is 3～30 (W/W) %; For PLA, solvent is carrene, and concentration is 3～30 (W/W) %; For cellulose, solvent is 4-methyl morpholine-N-oxide, and concentration is 1～10 (W/W) %;
Described solidification liquid is allocated as: for polycaprolactone/tetrahydrofuran solution, solidification liquid is 25 ± 2 DEG C of deionized waters; For the polyethylene glycol/75 ± 5 DEG C aqueous solution, solidification liquid is 25 ± 2 DEG C of deionized waters; For polytetramethylene carbonate diol/dimethyl formamide solution, solidification liquid is 25 ± 2 DEG C of deionized waters; For PLA/dichloromethane solution, solidification liquid is 25 ± 2 DEG C of deionized waters; For cellulose/4-methyl morpholine-N-oxide solution, solidification liquid is 25 ± 2 DEG C of deionized waters;
Described filter screen is the diddle-net that a kind of copy paper is used, and filter screen material is stainless steel, and mesh size is 200～400 orders; Described cryogenic refrigeration refers to and sample is refrigerated to-40～-50 DEG C, and the moisture content containing has become ice cube; Described distillation is freezing to be carried out in vacuum freeze drier, and distillation refrigerating process is: freeze-drying time is 48 ± 2 hours, freeze-drying pressure 80 ± 5Pa, 60 ± 2 DEG C of temperature of heating plate.
2. the preparation method of a kind of high porosity shitosan/polymer blended film felt according to claim 1, it is characterized in that, described injection refers to: Polymer Solution is packed in the charging basket of Electronic spraying machine, open electric air pump Polymer Solution is sprayed into solidification liquid with the speed of 0.2～0.3l/min with vaporific form.
3. the preparation method of a kind of high porosity shitosan/polymer blended film felt according to claim 1, it is characterized in that, described filter operation is: first the Buchner funnel of having laid filter paper is inserted in to Bu Shi flask upper opening and by sealing joint, then pour fine the wadding that sprays solidification forming suspension into Buchner funnel, suspension is drawn into beaker under suction function, and the fine solid of wadding a quilt with cotton is stayed in Buchner funnel; Described dispersion is that fine the wadding through filtering solid is put into beaker, adds the deionized water fibre that makes to wad a quilt with cotton to be again dispersed in water; Can wash away the coagulating agent in original solution through filtration and dispersion repeatedly, fine suspension clear liquid obtains wadding a quilt with cotton.
4. the preparation method of a kind of high porosity shitosan/polymer blended film felt as claimed in claim 1, it is characterized in that: by two or more the macromolecule making by step (4)～(7) the fine suspension clear liquid blend of wadding a quilt with cotton, then obtain the polymer blended film felt of high porosity shitosan/multicomponent by step (8)～(9) operation.
CN201210109417.2A 2012-04-13 2012-04-13 High-porosity chitosan/macromolecule blending thin film felt and preparation method thereof Expired - Fee Related CN102605672B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1544097A (en) * 2003-11-27 2004-11-10 四川大学 Biologic material for medical use and its preparing process and usage
CN101405038A (en) * 2006-03-20 2009-04-08 株式会社Jms Porous bioabsorbable material and method of producing the same
CN101538371A (en) * 2009-04-13 2009-09-23 重庆文理学院 Preparation method of high-strength degradable polysaccharide blend film
CN102206387A (en) * 2011-03-30 2011-10-05 东华大学 High molecule and inorganic nano-particle hybrid film and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1544097A (en) * 2003-11-27 2004-11-10 四川大学 Biologic material for medical use and its preparing process and usage
CN101405038A (en) * 2006-03-20 2009-04-08 株式会社Jms Porous bioabsorbable material and method of producing the same
CN101538371A (en) * 2009-04-13 2009-09-23 重庆文理学院 Preparation method of high-strength degradable polysaccharide blend film
CN102206387A (en) * 2011-03-30 2011-10-05 东华大学 High molecule and inorganic nano-particle hybrid film and preparation method thereof

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