CN105063803A - Preparation method of chitosan precipitation fiber - Google Patents
Preparation method of chitosan precipitation fiber Download PDFInfo
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- CN105063803A CN105063803A CN201510609592.1A CN201510609592A CN105063803A CN 105063803 A CN105063803 A CN 105063803A CN 201510609592 A CN201510609592 A CN 201510609592A CN 105063803 A CN105063803 A CN 105063803A
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- shitosan
- fibrid
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Abstract
The invention relates to a preparation method of a chitosan precipitation fiber. The method comprises the following steps: (1) degrading chitosan with the deacetylation degree being greater than 90% into a hydrogen peroxide solution with the concentration being 30wt%, preparing low-molecular weight chitosan with different molecular weights, and dissolving the low-molecular weight chitosan with acetic acid to prepare a chitosan solution; (2) taking a NaOH water solution as a coagulating bath of the chitosan precipitation fiber; and (3) injecting the coagulating bath into an airtight shear settling device with a stainless steel blade which is controlled by a variable-speed motor by a circulating pump, injecting the chitosan solution into the coagulating bath by a micro pump from the side surface of the container, forming the precipitation fiber at the moment that the chitosan solution is injected into the coagulating bath, and controlling the temperature of a polymer solution to be 25-150 DEG C by a temperature control device outside an injector. According to the preparation method, the wettability, the tearing property, the folding property and the writing property of traditional cellulose paper are kept; and due to the addition of the chitosan precipitation fiber, the paper can have relatively good stretching and optical properties.
Description
Technical field
The present invention relates to fibrous material Application and preparation technical field, be specially a kind of preparation method of shitosan fibrid.
Background technology
Shitosan is also known as chitin, chitin, chitin.It is from the object of the animals such as natural seashell, crab shell, shrimp shell, fish-bone and insect.When chitin deacetylase degree reaches 55%, then become the most important antibiotic derivative shitosan of chitin.Shitosan can be applicable to agricultural, and nutriment and medical and other field, it is also studied in the multiple application of field of textiles.Fibrid (fibrid is also called filament or pulp) is a kind of fibrous material of film-form, and thickness is one to several micron, and length is not from tens microns to several millimeters etc.It injects a large amount of coagulating agent in intensively stirred dilute polymer, or polymer solution is injected the coagulating bath precipitating of high-speed stirred and the fiber that obtains with the form of thread.
Report about fibrid starts from last century 50, the sixties, and the overwhelming majority mainly concentrates on aramid fiber fibrid and aramid paper.Patent relevant to aramid fiber fibrid and aramid paper has in addition reached tens thousand of item, defines tight patent group.A kind of preparation method of aramid fiber fibrid is disclosed in Chinese invention patent " a kind of production method of meta-position aramid paper fibrid " (CN102660795A), m-phenylene diamine (MPD) and m-phthaloyl chloride are mainly aggregated into PMIA resin (poly(isophthaloyl metaphenylene diamine) resin) by its method in DMAC (DMA); The hydrogen chloride gas that neutralization reaction produces; By resins dilute, in mother liquor, also precipitating is disperseed to become to meet the fibrid suspension manufacturing meta-position aramid fiber paper condition.Fibrid suspension and deionized water are passed into washing filter, the solvent, auxiliary agent and the moisture content that comprise in removing fibrid, obtain meeting the fibrid manufacturing meta-position aramid fiber paper condition.
Form sharp contrast therewith, about the report of shitosan fibrid is few.Shitosan fibrid has good physical property and biocompatible property, has good application potential at bio-medical and tissue engineering material field.At present, have researcher to utilize shitosan fibrid to prepare the dressing sponge drawn, this dressing sponge has good physical mechanical and biological property, can be applied to the treatment of different phase wound, and its moisture pick-up properties is also better than general sponge.Study in addition and also find, add paper obtained by shitosan fibrid and traditional cellulose paper to have and similar to soak, tear, fold and writing quality, and the paper adopting shitosan fibrid obtained is after simple ethanol post processing, can obtains and better stretch and optical property.
Accompanying drawing explanation
Fig. 1 be in the present invention embodiment 1 ~ 3 under an optical microscope to gained shitosan fibrid qualification figure.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of shitosan fibrid, and then solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme: a kind of preparation method of shitosan fibrid, comprises the following steps:
Step one, is that the shitosan of more than 90% is degrade in the hydrogen peroxide solution of 30wt% in concentration by deacetylation, prepares the low-molecular weight chitoglycan of different molecular weight, then prepare chitosan solution with acetate dissolution low-molecular weight chitoglycan.
Step 2, the coagulating bath using the NaOH aqueous solution as shitosan fibrid.
Step 3, coagulating bath is injected in the shearing settler of an airtight stainless steel blade controlled with variable-speed motor by circulating pump, chitosan solution injects coagulating bath by micro pump from container side, the moment that fibrid injects coagulating bath at chitosan solution is formed, and the temperature that the attemperating unit outside syringe controls polymer solution is 25 DEG C ~ 150 DEG C.
As further technical scheme of the present invention: described hydrogen peroxide solution and the mol ratio of shitosan are 2:1.
As further technical scheme of the present invention: described degradation condition is: time 2 ~ 8h, temperature 20 ~ 80 DEG C; Described acetic acid quality concentration is 1 ~ 5%.
As further technical scheme of the present invention: the concentration of the described NaOH aqueous solution is 5wt% ~ 20wt%, described coagulating bath injection rate is 20 ~ 100 times of chitosan solution.
As further technical scheme of the present invention: the rotating speed of described shearing settler is 1000 ~ 7000 revs/min.
As further technical scheme of the present invention: be 0.3 ~ 1 millimeter for chitosan solution being injected the syringe needle internal diameter of coagulating bath, injection flow is 1 ~ 10 ml/min.
Compared with prior art, the invention has the beneficial effects as follows: the preparation method of this shitosan fibrid,
1) wetting what maintain that traditional cellulose paper has, tear, outside folding and writing quality, add shitosan fibrid and paper also can be made to have better stretch and optical property.
2) due to the biocompatible property that shitosan fibrid is good, for bio-medical and tissue engineering material field provide new basic material.
3) the present invention has expanded the Application Areas of fibrid, and the scientific research personnel also for constantly finding the how new application direction of fibrid provides thinking.
The present invention has filled up a shitosan fibrid vacancy in the patent.In addition, the paper added obtained by shitosan fibrid not only have to traditional cellulose paper similar to soak, tear, folding and writing quality, it is after simple ethanol post processing, also can obtain and better stretch and optical property.
Detailed description of the invention
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of technical scheme: a kind of preparation method of shitosan fibrid, is characterized in that: comprise the following steps:
Step one, is that the shitosan of more than 90% is degrade in the hydrogen peroxide solution of 30wt% in concentration by deacetylation, prepares the low-molecular weight chitoglycan of different molecular weight, then prepare chitosan solution with acetate dissolution low-molecular weight chitoglycan.
Step 2, the coagulating bath using the NaOH aqueous solution as shitosan fibrid.
Step 3, coagulating bath is injected in the shearing settler of an airtight stainless steel blade controlled with variable-speed motor by circulating pump, chitosan solution injects coagulating bath by micro pump from container side, the moment that fibrid injects coagulating bath at chitosan solution is formed, and the temperature that the attemperating unit outside syringe controls polymer solution is 25 DEG C ~ 150 DEG C.
Embodiment 1:
A kind of preparation method of shitosan fibrid, concrete steps are: the shitosan 5g selecting deacetylation to reach 90% degrades in the hydrogen peroxide solution 15ml of 30wt%, time of control degradation is that 6h and temperature are 80 DEG C and prepare a certain amount of low-molecular weight chitoglycan, then is that the acetum 100ml of 5wt% dissolves the low-molecular weight chitoglycan 3g preparing gained and prepares chitosan solution with concentration; Take concentration as the coagulating bath of the NaOH aqueous solution as shitosan fibrid of 15wt%, setting rate depends on the concentration of NaOH; Coagulating bath is injected in the shearing settler of an airtight stainless steel blade controlled with variable-speed motor by circulating pump, and rotating speed 6000 revs/min, flow is 50 times of chitosan solution.Chitosan solution injects coagulating bath by micro pump from container side, and the moment that fibrid injects coagulating bath at chitosan solution is formed.The temperature that attemperating unit outside syringe controls polymer solution is 80 DEG C.
Embodiment 2:
A kind of preparation method of shitosan fibrid, concrete steps are: the shitosan 5g selecting deacetylation to reach 90% degrades in the hydrogen peroxide solution 15ml of 30wt%, time of control degradation is that 4h and temperature are 70 DEG C and prepare a certain amount of low-molecular weight chitoglycan, then is that the acetum 100ml of 4wt% dissolves the low-molecular weight chitoglycan 2g preparing gained and prepares chitosan solution with concentration; Take concentration as the coagulating bath of the NaOH aqueous solution as shitosan fibrid of 10wt%, setting rate depends on the concentration of NaOH; Coagulating bath is injected in the shearing settler of an airtight stainless steel blade controlled with variable-speed motor by circulating pump, and rotating speed 5000 revs/min, flow is 50 times of chitosan solution.Chitosan solution injects coagulating bath by micro pump from container side, and the moment that fibrid injects coagulating bath at chitosan solution is formed.The temperature that attemperating unit outside syringe controls polymer solution is 70 DEG C.
Embodiment 3:
A kind of preparation method of shitosan fibrid, concrete steps are: the shitosan 5g selecting deacetylation to reach 90% degrades in the hydrogen peroxide solution 15ml of 30wt%, time of control degradation is that 2h and temperature are 60 DEG C and prepare a certain amount of low-molecular weight chitoglycan, then dissolves with the acetum 100ml of concentration 3wt% the low-molecular weight chitoglycan 1g preparing gained and prepare chitosan solution; Take concentration as the coagulating bath of the NaOH aqueous solution as shitosan fibrid of 10wt%, setting rate depends on the concentration of NaOH; Coagulating bath is injected in the shearing settler of an airtight stainless steel blade controlled with variable-speed motor by circulating pump, and rotating speed 4000 revs/min, flow is 50 times of chitosan solution.Chitosan solution injects coagulating bath by micro pump from container side, and the moment that fibrid injects coagulating bath at chitosan solution is formed.The temperature that attemperating unit outside syringe controls polymer solution is 60 DEG C.
Embodiment four:
To the qualification that embodiment 1 ~ 3 gained shitosan fibrid is correlated with, its result is as shown in table 1.
Table 1 embodiment 1-3 shitosan fibrid properties of sample
For the fibrid prepared by embodiment 1, after being uniformly dispersed in water, in paper machine, manufacture paper with pulp into body paper, eventually pass high-temperature high-pressure ray machine hot forming at 300 DEG C, obtain shitosan fibrid paper, its result is as table 2.
Table 2 shitosan fibrid paper performance
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (6)
1. a preparation method for shitosan fibrid, is characterized in that: comprise the following steps:
Step one, is that the shitosan of more than 90% is degrade in the hydrogen peroxide solution of 30wt% in concentration by deacetylation, prepares the low-molecular weight chitoglycan of different molecular weight, then prepare chitosan solution with acetate dissolution low-molecular weight chitoglycan;
Step 2, the coagulating bath using the NaOH aqueous solution as shitosan fibrid;
Step 3, coagulating bath is injected in the shearing settler of an airtight stainless steel blade controlled with variable-speed motor by circulating pump, chitosan solution injects coagulating bath by micro pump from container side, the moment that fibrid injects coagulating bath at chitosan solution is formed, and the temperature that the attemperating unit outside syringe controls polymer solution is 25 DEG C ~ 150 DEG C.
2. the preparation method of a kind of shitosan fibrid according to claim 1, is characterized in that: described hydrogen peroxide solution and the mol ratio of shitosan are 2:1.
3. the preparation method of a kind of shitosan fibrid according to claim 1, is characterized in that: described degradation condition is: time 2 ~ 8h, temperature 20 ~ 80 DEG C; Described acetic acid quality concentration is 1 ~ 5%.
4. the preparation method of a kind of shitosan fibrid according to claim 1, is characterized in that: the concentration of the described NaOH aqueous solution is 5wt% ~ 20wt%, and described coagulating bath injection rate is 20 ~ 100 times of chitosan solution.
5. the preparation method of a kind of shitosan fibrid according to claim 1, is characterized in that: the rotating speed of described shearing settler is 1000 ~ 7000 revs/min.
6. the preparation method of a kind of shitosan fibrid according to claim 1, is characterized in that: be 0.3 ~ 1 millimeter for chitosan solution being injected the syringe needle internal diameter of coagulating bath, and injection flow is 1 ~ 10 ml/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109537353A (en) * | 2018-12-11 | 2019-03-29 | 江苏宝德新材料有限公司 | A kind of injecting type precipitating device |
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| CN103435717A (en) * | 2013-08-16 | 2013-12-11 | 江苏顺心德生物科技有限公司 | Chitosan oligosaccharide |
| CN103556501A (en) * | 2013-10-30 | 2014-02-05 | 齐齐哈尔大学 | Cation dyeing auxiliary of linen reactive dye, preparation method and application of cation dyeing auxiliary |
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2015
- 2015-09-22 CN CN201510609592.1A patent/CN105063803A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982601A (en) * | 2010-10-18 | 2011-03-02 | 南通曙光染织有限公司 | Preparation method of ecological non-iron cotton high-grade fabric |
| CN103435717A (en) * | 2013-08-16 | 2013-12-11 | 江苏顺心德生物科技有限公司 | Chitosan oligosaccharide |
| CN103556501A (en) * | 2013-10-30 | 2014-02-05 | 齐齐哈尔大学 | Cation dyeing auxiliary of linen reactive dye, preparation method and application of cation dyeing auxiliary |
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| 任娟等: "沉析纤维的纤维性能与应用", 《纺织导报》 * |
| 朱婉萍等: "《甲壳素及其衍生物的研究与应用》", 30 November 2014 * |
| 沉析纤维的纤维性能与应用;任娟等;《纺织导报》;20141018;第68-70页 * |
| 路艳华等: "《壳聚糖及纳米材料在柞蚕丝功能改性中的应用》", 31 August 2012 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109537353A (en) * | 2018-12-11 | 2019-03-29 | 江苏宝德新材料有限公司 | A kind of injecting type precipitating device |
| CN109537353B (en) * | 2018-12-11 | 2021-01-12 | 江苏宝德新材料有限公司 | Jet type settling device |
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Application publication date: 20151118 |