CN104004113A - Preparation method of temperature-sensitive hydroxyalkyl chitin - Google Patents
Preparation method of temperature-sensitive hydroxyalkyl chitin Download PDFInfo
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- CN104004113A CN104004113A CN201410201414.0A CN201410201414A CN104004113A CN 104004113 A CN104004113 A CN 104004113A CN 201410201414 A CN201410201414 A CN 201410201414A CN 104004113 A CN104004113 A CN 104004113A
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- chitin
- temperature
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Abstract
The invention relates to a new reparation method of temperature-sensitive hydroxyalkyl chitin. The method of the invention enables chitin to directly dissolve at a low temperature by using an aqueous solvent to obtain a chitin aqueous solution. The chitin aqueous solution is further used to react with various etherifying agents. Impurities in the reaction solution are removed through dialysis, and water-soluble hydroxyalkyl chitin is obtained through freeze drying. The method can achieve the effect of homogeneous reaction. Through control of feed ratio, reaction temperature, and reaction time, hydroxyalkyl chitin with different substitution degrees can be obtained. Chitin derivatives prepared by the method have very good water solubility and a phase transition temperature lower than human body physiological temperature, and can be gelatinized at a very low mass concentration. The preparation method is simple and practical, avoids the usage of a lot of organic solvents, and also reduces the production cost. The temperature-sensitive hydroxyalkyl chitin prepared in the invention is applicable to various fields in production and living.
Description
Technical field
The present invention relates to the preparation method that a class has the chitin derivativ of Thermo-sensitive, belong to natural biological polymeric material field, also belong to biomedical materials field.
Background technology
Chitin is again chitin, chitin, is extracted from the shell of shrimp crab or insect, is a kind of natural biological high molecular polymer, at occurring in nature, has huge reserves, and it is the renewable natural organic matter of reserves maximum on the earth after Mierocrystalline cellulose.Therefore develop chitin resource for building a resource-conserving society, Sustainable development has great significance.The de-acetyl product chitosan of chitin and part thereof is having consequence aspect useful for drug delivery, organizational project especially wound auxiliary material.
Temperature-sensitive material is the class intelligent macromolecule material that a class can produce physics or chemical property change under the stimulation of outside temperature.Regulate its low critical consolute temperature (LCST) near Human Physiology temperature, temperature-sensitive macromolecular can be used for medicine and controls release, the aspects such as organizational project.PNIPAM (poly N-isopropyl acrylamide), PEO-PLGA-PEO (polyethylene oxide-PLGA-polyethylene oxide triblock copolymer), hydroxypropylcellulose
7, the thermosensitive polymers such as Vltra tears by preliminary application in these areas.
Within very long for some time, people have designed and have synthesized large quantities of temperature-sensitive macromoleculars.But there are some shortcomings and deficiencies in these temperature-sensitive macromoleculars mostly.The synthetic difficulty of temperature-sensitive macromolecular of synthetic class is difficult to industrialization, in partial synthesis polymer body, cannot degrade.Although modified natural polymer industrialization already as lower in its production costs such as hydroxypropylcelluloses, its LCST is all higher than Human Physiology temperature.
Summary of the invention
The present invention be intended to not use under the condition of any organic solvent, prepare to less energy-consumption have water-soluble and temperature sensitivity hydroxyalkyl chitin.
The step that the present invention prepares hydroxyalkyl chitin is 3 steps.
First chitin is dissolved in aqueous solvent.Aqueous solvent is containing 10wt%NaOH, and all the other are water.
Second step adds quantitative etherifying agent to seal above-mentioned chitin water soluble liquid and continues stirring at 5-55 ℃.Reaction times is 0.5-72h.
The 3rd step above-mentioned reaction solution is used in hydrochloric acid and after pack dialysis tubing (8000-10000) into and be placed in deionized water and dialyse, remove small molecular weight impurity.After freeze-drying, can obtain hydroxyalkyl chitin.
Accompanying drawing explanation
Fig. 1 is that the rheology of gained 1wt% ethoxyl chitin characterizes.
Fig. 2 is that the rheology of gained 1wt% Hydroxypropyl chitosan characterizes.
Fig. 3 is the temperature sensitive phase transformation photo of 1wt% Hydroxypropyl chitosan solution.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.But the present invention is not limited to the following example.
Embodiment 1:
Take 5g dissolution of sodium hydroxide in 7.5g water, add 0.5g chitin, stir and add 37g trash ice simultaneously at low temperatures, can obtain chitin uniform solution.In chitin solution, add 15 ℃, 5mL oxyethane to stir 12h.Reaction solution use hydrochloric acid be neutralized to neutrality pack in dialysis tubing, dialyse three days after freeze-drying both Natvosol.This product is completely water-soluble.Its 1wt% solution phase transition temperature is at 37 ℃.
Embodiment 2:
Take 5g dissolution of sodium hydroxide in 7.5g water, add 0.5g chitin, stir and add 37g trash ice simultaneously at low temperatures, can obtain chitin uniform solution.In chitin solution, add 15 ℃ of 5mL propylene oxide to stir 12h.Reaction solution use hydrochloric acid be neutralized to neutrality pack in dialysis tubing, dialyse three days after freeze-drying both hydroxypropylcellulose.This product is completely water-soluble.Its 1Wt% solution phase transition temperature is at 26 ℃.
Claims (7)
1. a preparation method for hydroxyalkyl chitin, is characterized in that the product obtaining has good solubility and adjustable temperature sensitivity.
2. a preparation method for hydroxyalkyl chitin, is characterized in that preparation process carries out in aqueous phase system, does not relate to organic phase.
3. the preparation method of a hydroxyalkyl chitin, it is characterized in that preparing by following three steps: (1) by stirring and dissolving chitin on the rocks in aqueous sodium hydroxide solution, sodium hydroxide ultimate density is 10% (2) to add different etherifying agents and react under differing temps, and (3) dialysis freeze-drying obtains white product.
4. in the solution of chitin described in claim 3, massfraction is 0.2%-5%.
5. described in claim 3, obtaining the reaction times is 0.5-72h, and temperature of reaction is 5-55 ℃.
6. the etherifying agent described in claim 3 comprises methyl iodide, ethylene bromohyrin, oxyethane, propylene oxide and blend thereof.
7. its phase transition temperature of the temperature sensitivity described in claim 1 is at 10-50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410201414.0A CN104004113A (en) | 2014-05-08 | 2014-05-08 | Preparation method of temperature-sensitive hydroxyalkyl chitin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410201414.0A CN104004113A (en) | 2014-05-08 | 2014-05-08 | Preparation method of temperature-sensitive hydroxyalkyl chitin |
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| Publication Number | Publication Date |
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| CN104004113A true CN104004113A (en) | 2014-08-27 |
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| CN201410201414.0A Pending CN104004113A (en) | 2014-05-08 | 2014-05-08 | Preparation method of temperature-sensitive hydroxyalkyl chitin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104761658A (en) * | 2015-04-14 | 2015-07-08 | 南开大学 | Preparation method of completely water-soluble temperature-sensitive bydroxylpropyl chitin |
| CN107202814A (en) * | 2017-05-02 | 2017-09-26 | 江苏银基烯碳能源科技有限公司 | A kind of assay method of temperature sensitive reversible gel powder solution temperature |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284884A (en) * | 2008-02-19 | 2008-10-15 | 上海其胜生物材料技术研究所有限公司 | Preparation method of temperature sensitivity chitosan derivate-hydroxybutyl chitosan |
| CN103951764A (en) * | 2014-04-25 | 2014-07-30 | 武汉大学 | Method for homogeneously preparing hydroxypropyl modified chitin with low degree of deacetylation |
-
2014
- 2014-05-08 CN CN201410201414.0A patent/CN104004113A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284884A (en) * | 2008-02-19 | 2008-10-15 | 上海其胜生物材料技术研究所有限公司 | Preparation method of temperature sensitivity chitosan derivate-hydroxybutyl chitosan |
| CN103951764A (en) * | 2014-04-25 | 2014-07-30 | 武汉大学 | Method for homogeneously preparing hydroxypropyl modified chitin with low degree of deacetylation |
Non-Patent Citations (2)
| Title |
|---|
| SEONG SOO KIM ET AL.: "Thermal characteristics of chitin and hydroxypropyl chitin", 《POLYMER》 * |
| 江志强，等: "温敏性羟丙基壳聚糖的制备及其性能", 《材料科学与工程学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104761658A (en) * | 2015-04-14 | 2015-07-08 | 南开大学 | Preparation method of completely water-soluble temperature-sensitive bydroxylpropyl chitin |
| CN107202814A (en) * | 2017-05-02 | 2017-09-26 | 江苏银基烯碳能源科技有限公司 | A kind of assay method of temperature sensitive reversible gel powder solution temperature |
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Application publication date: 20140827 |