Photosensitive modified chitosan, preparation method and application thereof

A technology of photosensitivity and chitosan, applied in the field of composite materials, can solve the problems of the decrease of the apparent quality of the gel, the high requirements of the hardware of the forming equipment and the control precision, etc., to achieve the effect of enhancing the mechanical properties

Active Publication Date: 2021-11-19
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the influence of factors such as liquid tension and gravity during the printing process, the apparent quality of the gel decreases after layer-by-layer accumulation.
From the above analysis, it is easy to know that although the above method has laid the foundation for the feasibility and application of chitosan gel printing, it has the problem of high requirements on the hardware and control precision of the forming equipment.

Method used

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  • Photosensitive modified chitosan, preparation method and application thereof
  • Photosensitive modified chitosan, preparation method and application thereof
  • Photosensitive modified chitosan, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1 prepares photosensitive modified chitosan (CH-MA)

[0048] Add methacrylic anhydride (MA) in the chitosan (CH) solution of 1.5% (w / v), react 4h, reaction process is as follows figure 1 shown. The resulting product was added dropwise to sodium bicarbonate solution to neutralize and remove excess anhydride. Then dialyzed to obtain methacrylic acid modified chitosan (CH-MA). Change the ratio of methacrylic anhydride to amino groups in chitosan (1:1, 2:1, 4:1, 5:1, 7:1, 8:1, 10:1, 15:1, 16:1) , to explore the effect of grafting ratio on the water solubility of modified chitosan, the prepared modified chitosan were named as CH-MA 1, CH-MA 2, CH-MA 4, CH-MA 5, CH-MA 7, CH-MA 10, CH-MA 15, CH-MA16. Specific steps are as follows:

[0049] Add 0.5±0.025mg chitosan and 0.5±0.08ml acetic acid to 30±0.5ml deionized water and mix well. Add a certain proportion of methacrylic anhydride at 40±20°C, the volume fraction of methacrylic anhydride added is 1% (v / v) to 15...

Embodiment 2

[0050] Example 2 Preparation of photosensitive 3D printing ink (CH-MA / GE)

[0051] Weigh a certain amount of CH-MA, add 0.05-0.4wt% I2959 photoinitiator and gelatin solution, stir evenly, and put the solution into a 3D printing barrel to obtain 3D printing ink.

[0052]S1 adds 200±10mg of photosensitive chitosan fiber and 5-40mg (0.05wt%-0.4wt%) photoinitiator I2959 (2-hydroxyl-2-methyl-1-[4- (2-hydroxyethoxy) phenyl]-1-propanone), after stirring evenly, the mixed solution was obtained for subsequent use.

[0053] Preparation of S2 gelatin solution: Prepare a 5w / v%-12w / v% gelatin solution at 40±5°C for later use.

[0054] Preparation of S3 ink: At room temperature, mix the mixed solution obtained in S1 with the gelatin solution in equal volumes to obtain 3D printing ink.

Embodiment 3

[0055] Embodiment 3 Ink characterization:

[0056] The successful grafting of methacrylic anhydride to chitosan was verified by infrared spectroscopy (FTIR) and hydrogen nuclear magnetic spectroscopy (1H NMR). Nicolet Impact410 infrared spectrometer was used for measurement, and the test resolution was 4

[0057]

[0058] cm -1 , the number of scans is 32 times, and the test range is 400-4000cm -1 . Utilizing the selective absorption characteristics of different substances for different wavelengths of infrared rays, high-resolution infrared spectroscopy is used to detect CH-MA, and the main components in the sample can be qualitatively analyzed according to the characteristic peaks that are characterized. at the same time through 1 Quantitative analysis of modified chitosan by H NMR can determine the grafting rate of MA on CH. The formula for calculating the grafting ratio (DS) of CH-MA is as follows:

[0059] where A H(5.5&6.0) Corresponding to the vinyl proton peak...

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Abstract

The invention provides a preparation method of photosensitive modified chitosan. The method comprises the following steps: 1) dissolving a proper amount of chitosan and acetic acid in deionized water, and uniformly mixing to obtain a mixed solution; 2) adding a proper amount of methacrylic anhydride into the mixed solution to obtain a reaction mixed solution, and carrying out heat preservation and stirring reaction at 40-80 DEG C, wherein the volume fraction of the methacrylic anhydride in the reaction mixed solution is 1-15%, preferably 6-8%; and 3) after the reaction, adjusting the pH value to 7 by using a sodium bicarbonate solution, and purifying and drying to obtain the photosensitive modified chitosan. The invention further provides the gelatin-photosensitive modified chitosan ink prepared on the basis of the method and application of the gelatin-photosensitive modified chitosan ink. The gelatin-modified chitosan membrane provided by the invention has a microporous structure, shows relatively high (more than 90%) separation efficiency in an oil-water separation experiment, and also keeps the membrane flux for pump oil with relatively high viscosity at 1000 Lm<-2>h<-1> or above.

Description

technical field [0001] The invention relates to the technical field of composite materials, in particular to new materials for environmental protection and 3D printing technology, in particular to a photosensitive modified chitosan and its preparation method and application. Background technique [0002] Chitosan is the second largest type of biological polysaccharide after cellulose. It has good biocompatibility and biodegradability, and is cheap and easy to obtain, non-toxic and harmless. At the same time, there are a large number of Amino, hydroxyl and other hydrophilic functional groups ensure that it has a certain application potential in the field of oil-water separation. However, pure chitosan solution system cannot be directly applied to 3D printing technology because of its good fluidity, and it needs to be modified or blended with other high polymers. [0003] Due to the problems of poor solution stability and solubility in most existing chitosan solvent systems, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08C09D11/14C09D11/04B33Y70/00B01D67/00B01D71/08B01D17/022
CPCC08B37/003C09D11/14C09D11/04B33Y70/00B01D67/0002B01D71/08B01D17/02B01D17/085
Inventor 冯昭璇徐亚男吴明铂房海秋
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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