Method for preparing porous hydrogel through freezing-illumination

Patent metadata

Field	Value
Publication number	US-10358516-B2
Application number	US-201715415692-A
Country	US
Kind code	B2
Filing date	Jan 25, 2017
Priority date	Jan 26, 2016
Publication date	Jul 23, 2019
Grant date	Jul 23, 2019

Abstract

The present invention discloses a freezing-illumination method for preparing porous gels, comprising the steps of: (a) synthesizing the gels containing dynamic exchangeable bonds; (b) illuminating the gels under frozen state by certain wavelength light source; (c) elevating the temperature and melt the ice crystals within the gels to get the porous structure. The dynamic exchangeable bonds existing in the gels include double/multi-sulfur bond, hydrazine bond, boronic ester bond. Catalyst is also included in the gel composition to activate the bond exchange reactions under illumination. This new method for preparing porous gels is easy to operate and suitable for most kinds of gels. Meanwhile, it can spatially control the pore structure within the gels by local illumination.

First claim

The invention claimed is:

1. A freezing-illumination method for preparing a porous hydrogel, the method comprising the following steps in the following order:
(a) synthesizing by polymerization a gel containing exchangeable bonds under room temperature or heating and using water as solvent;
(b) freezing the gel containing exchangeable bonds to prepare a gel containing exchangeable bonds in a frozen state, and illuminating the gel containing exchangeable bonds in the frozen state by a light source so that the exchangeable bonds contained therein exchange; and
(c) exposing to an elevated temperature the gel containing exchangeable bonds in the frozen state to melt ice crystals therein to obtain the porous hydrogel.

2. The method of claim 1 , wherein the exchangeable bonds are selected from at least one of the following: bonds between two or more sulfur bonds, hydrazine bonds, boronic ester bonds, and host-guest interaction bonds.

3. The method of claim 1 , wherein the porous hydrogel comprises a catalyst which can activate the exchangeable bonds when the catalyst is illuminated with a light source; and wherein the amount of the catalyst ranges 0.05-5% by weight of all dry ingredients in the porous hydrogel.

4. The method of claim 1 , characterized in that:
the exchangeable bonds are bonds between two or more sulfur atoms and the porous hydrogel further comprises a photo-radical initiator as a catalyst; or
the exchangeable bonds are hydrazine bonds and the porous hydrogel further comprises a photo-base generator as a catalyst; or
the exchangeable bonds are boronic ester bonds and the porous hydrogel further comprises a photo-acid generator as a catalyst; or
the exchangeable bonds are host-guest interaction bonds and the porous hydrogel does not comprise a catalyst.

5. The method of claim 3 , wherein addition of the catalyst includes in situ introduction during step (a) or diffusion into the gel containing exchangeable bonds after step (a).

6. The method of claim 1 , wherein wavelength of the light source is 200-470 nm, and illuminating occurs for is 0.5 min-24 hours.

7. The method of claim 1 , wherein the illuminating includes is uniform irradiation or local irradiation by a mask.

8. The method of claim 1 , wherein, in step (b), freezing includes uniformly freezing or directionally freezing.

Assignees

• Univ Zhejiang

Inventors

• Zhao Qian
• Wu Jingjun
• Xie Tao
• Chen Di

Classifications

• C08J2333/26

  Homopolymers or copolymers of acrylamide or methacrylamide · CPC title

• C08J2371/08

  Polyethers derived from hydroxy compounds or from their metallic derivatives (C08J2371/02 takes precedence) · CPC title

• C08J3/075

  Macromolecular gels · CPC title

• C08G65/48

  Polymers modified by chemical after-treatment · CPC title

• C08J9/28

  by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum · CPC title