Method for preparing poly(pseudo)rotaxanes with gamma-cyclodextrin and polyvinyl alcohol

A technology of polyvinyl alcohol and quasi-polyrotaxane, which is applied in the field of new polymer material preparation, can solve problems such as unreported, and achieve the effects of good water solubility, simple preparation process and broad application prospect.

Inactive Publication Date: 2009-11-25
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention uses polyvinyl alcohol as a macromolecular chain to prepare pseudopolyrotaxanes by assembling with γ-cyclodextrin. At present, this preparation method has not been reported at home and abroad

Method used

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  • Method for preparing poly(pseudo)rotaxanes with gamma-cyclodextrin and polyvinyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Preparation of polyvinyl alcohol: 50ml of vinyl acetate was added to 250ml of methanol, 1.2g of azobisisobutyronitrile was added, the weight ratio of azobisisobutyronitrile to vinyl acetate was 0.026:1, and nitrogen was blown to remove After oxygen, put it into a constant temperature water bath with a temperature of 65°C under the protection of nitrogen, and polymerize for 6 hours to obtain polyvinyl acetate; use a rotary evaporator to evaporate the unreacted vinyl acetate monomer at 40°C under reduced pressure; The solution of polyvinyl acetate was transferred to a 250mL three-neck flask equipped with a stirrer and a thermometer, and 2.0mL of NaOH solution with a concentration of 10mol / L was added dropwise, and the molar ratio of the NaOH solution added dropwise to vinyl acetate was 0.037:1. Then alcoholyze in a water bath with a temperature of 35°C for 1.5 hours; the product after alcoholysis is centrifuged at a high speed of 11000r / min, and the solid powder obtaine...

Embodiment 2

[0028] 1) Preparation of polyvinyl alcohol: add 50ml of vinyl acetate to 472ml of methanol, add 1.7g of azobisisobutyronitrile, the weight ratio of azobisisobutyronitrile to vinyl acetate is 0.037:1, blow nitrogen to remove After oxygen, put it in a constant temperature water bath with a temperature of 65°C under the protection of nitrogen, and polymerize for 8 hours to obtain polyvinyl acetate; use a rotary evaporator to evaporate the unreacted vinyl acetate monomer at 40°C under reduced pressure; The solution of polyvinyl acetate was transferred to a 250mL three-necked flask equipped with a stirrer and a thermometer, and 0.9mL of a 10mol / L NaOH solution was added dropwise. The molar ratio of the added NaOH solution to vinyl acetate was 0.017:1, and then Alcoholysis in a water bath at 40°C for 2 hours; the product after alcoholysis was centrifuged at a high speed of 11000r / min, and the solid powder obtained after centrifugation was washed twice with methanol; then dissolved in...

Embodiment 3

[0032] 1) Preparation of polyvinyl alcohol: the same as in Example 1.

[0033] 2) Preparation of pseudopolyrotaxane: Dissolve 2.0g of polyvinyl alcohol in 20ml of deionized water and stir until completely dissolved at 85°C; then add 3.0g of γ-cyclodextrin solid powder, γ-cyclodextrin and polyvinyl alcohol The molar ratio is 10:1, stirred at 80°C for 80 hours; after the reaction, evaporate the reaction solution to about 5ml with a rotary evaporator, and vacuum-dry the obtained concentrated solution to obtain γ-cyclodextrin and polyethylene Alcohol pseudopolyrotaxanes.

[0034] The prepared γ-cyclodextrin and polyvinyl alcohol pseudopolyrotaxane were analyzed by thermogravimetric analysis and infrared spectrum. The thermal gravimetric spectrum shows that the decomposition temperature of polyvinyl alcohol is 276°C, the thermal decomposition temperature of γ-CD is 321°C, and the thermal decomposition temperature of γ-cyclodextrin and polyvinyl alcohol pseudopolyrotaxane is 337°C....

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Abstract

The present invention discloses a method for preparing poly(pseudo)rotaxanes with gamma-cyclodextrin and polyvinyl alcohol, wherein the method comprises the following steps: using the vinyl acetate as a monomer, the methanol as a solvent and azobisisobutyronitrile as an initiating agent for preparing the polyvinyl alcohol through adjusting the concentration of the monomer or the initiating agent in the system; dissolving the prepared polyvinyl alcohol into the water, after mixing to dissolved, adding the solid powder of gamma-cyclodextrin, and assembling the gamma-cyclodextrin and the polyvinyl alcohol in the temperature of 80 DEG C while mixing; and after evaporating the solvent, vacuum-drying the obtained concentrated liquor for obtaining the gamma-cyclodextrin and polyvinyl alcohol poly(pseudo)rotaxanes. The method of the invention has the advantages of simple preparing technique, excellent bioavailability of the prepared poly(pseudo)rotaxanes, no toxicity of the product and excellent water solubility. The poly(pseudo)rotaxanes assembled by the cyclodextrin and the macromolecule has broad application prospect in the directions of medicine releasing, protein separating purifying, etc.

Description

technical field [0001] The invention relates to a novel polymer material preparation technology, in particular to a method for preparing pseudopolyrotaxanes by using gamma-cyclodextrin and polyvinyl alcohol. Background technique [0002] Molecular assembly refers to the process in which molecules and molecules are spontaneously connected into molecular aggregates with stable structure under certain conditions, relying on the force of non-covalent intermolecular bonds (Li Qin, Cui Yan, Zhang Wanxi, Dou Yanli, Li Min, Zhang Chengyi. Gao Molecular Materials Science and Engineering, 2004, 20:33-36). Through molecular assembly, we can obtain assembled materials with unique optical, electrical, and catalytic functions and characteristics, especially the assembled membrane materials that are now receiving widespread attention in nonlinear optical devices, chemical biosensors, information storage materials, and biological macromolecules. Synthetic aspects have broad application pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/02C08B37/16A61K47/40
Inventor 郭敏杰高婷樊志么敬霞刘靖王小聪陈鑫景作亮刁春华王存璐
Owner TIANJIN UNIV OF SCI & TECH
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