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Method for preparing silk protein ionic liquid solution

A technology of ionic liquid and silk protein, which is applied in the field of silk protein treatment, can solve negative problems such as reducing the solubility of solutes such as proteins, solution uniformity, and serious degradation of protein molecular chains, and achieve cost reduction, easy recycling, and solubility high effect

Active Publication Date: 2012-12-12
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of these patents obtain solutions by direct microwave heating or long-term high-temperature heating under nitrogen or helium atmosphere, so there is a problem of serious degradation of protein molecular chains by microwave or long-term high temperature; in addition, none of the existing related patents involves dissolution The effect of moisture in the process
As we all know, ionic liquids can easily absorb moisture in the air, which seriously reduces the solubility of solutes such as proteins and the uniformity of the solution, and has negative effects on subsequent processing such as spinning and tape casting.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: will use Na 2 CO 3 The degummed and dried silk fibers were mixed with the ionic liquid 1-methyl-3-butylimidazolium chloride (BmimCl) at a ratio of 10:90 (mass ratio) at room temperature and frozen in liquid nitrogen for 10 minutes, then placed in freeze-drying Remove water in the machine for 72 hours; then place it in an oil bath at 100°C and stir, start vacuum distillation for 1 hour after BmimCl melts to remove air bubbles and possible residual traces of water in the liquid, seal to ensure that the mixture is in a negative pressure environment for 2.5 hours, stop heating and stirring , a uniform and transparent solution was obtained, a white solid was obtained after the temperature was lowered to room temperature, and a uniform and transparent solution was recovered after the temperature was raised to 65°C.

Embodiment 2

[0021] Embodiment 2: the NaHCO 3 The degummed and dried silk fibers were mixed with ionic liquid 1-allyl-3-methylimidazolium chloride (EmimAc) at a ratio of 15:85 at room temperature and frozen with liquid nitrogen for 5 min, then placed in a freeze dryer to remove Water for 12 hours; then placed in a 50°C oil bath and stirred, accompanied by vacuum distillation to remove air bubbles and possible residual traces of water in the liquid, stop heating and stirring after 1.5 hours to obtain a uniform and transparent solution, cool to room temperature, and obtain a yellow color Viscous transparent solution.

Embodiment 3

[0022] Embodiment 3: the NaHCO 3 The degummed and dried silk fibers were mixed with 1-ethyl-3-methylimidazolium acetate (EmimAc) at a ratio of 30:70 at room temperature and frozen with liquid nitrogen for 5 minutes, and placed in a freeze dryer to remove water for 24 hours ;Put it in an oil bath at 80°C and stir, distill under reduced pressure for 10 minutes to remove a small amount of air bubbles and possible residual traces of water in the liquid, seal the mixture to ensure that it is under negative pressure for 2.5 hours, stop heating and stirring, cool to room temperature, and obtain uniform and transparent yellow viscous liquid.

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Abstract

The invention belongs to the technical field of silk protein treatment and particularly relates to ionic liquid solution of regenerated silk protein and a preparation method thereof. The preparation method comprises a step of freeze-drying dewatering and a step of dissolving under reduced pressure and particularly comprises: uniformly mixing a silk or silk protein material and ionic liquid, freezing under a liquid nitrogen condition, and dewatering in a freezer dryer; and heating the dried mixture in an oil bath with stirring, removing air bubbles and possible residual water from the system under a reduced pressure to prepare the ionic liquid solution of the silk protein. The concentration of the final product is 1 to 35 weight percent, and the silk protein conformation in the solution ismainly random coil. In the invention, nontoxic, non-volatile and easily-recoverable ionic liquid is used as a solvent, so the method is quick, simple and easy; and the room-temperature storage performance under a water-free condition of the solution of the silk protein is high, and all physical and chemical indexes of the solution can be kept stable for a long time.

Description

technical field [0001] The invention belongs to the technical field of silk protein treatment, and in particular relates to an ionic liquid solution of high-concentration regenerated silk protein and a preparation method thereof. Background technique [0002] Silk is a product of ancient Chinese civilization. It has been widely used as a clothing material since ancient times due to its softness, good air permeability, and soft texture. In recent decades, due to the characteristics of non-toxicity, good biocompatibility and easy degradability of silk protein, its application in the fields of medicine, biotechnology and daily chemical industry has also been continuously developed, for example, it is used as a slow-release carrier for medicine , enzyme immobilization materials, cosmetics and smart hydrogels, etc. [0003] Most of the applications of silk protein except in the field of fabrics are based on the regeneration solution of silk protein. In recent years, people have...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/11C08L89/00
Inventor 邵正中王芹杨宇红
Owner FUDAN UNIV
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