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Chemical synthesis method of hydroxypropyl chitin

A technology of chemical synthesis of hydroxypropyl chitin, applied in chitin polysaccharide coatings, hyaluronic acid coatings, etc., can solve problems such as industrial application restrictions, and achieve good sealing, dense and uniform film layers, and good water solubility.

Inactive Publication Date: 2019-05-14
青岛凯玉盈商贸有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chitin can only be dissolved in a mixed solvent of 5% lithium chloride, hexafluoroisopropanol, hexafluoroacetone, 1,2-dichloroethane, dimethylformamide and trichloroacetic acid, and insoluble in other organic solvents And dilute acid, alkali solution, its industrial application is greatly restricted

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Pulverization: pulverize chitin into 200-mesh powder with a pulverizer to obtain chitin powder for subsequent use;

[0022] Swelling: Soak 1kg of chitin powder in 3kg of 23% sodium hydroxide aqueous solution at minus 19°C for 18 hours, then thaw at room temperature;

[0023] Synthesis: Put thawed chitin into the reaction kettle, inject 9kg of isopropanol and 0.15kg of catalyst pyranpolyamine polyester, stir, gradually raise the temperature to 40°C, keep warm for 1.5 hours, then add 3kg of propylene oxide, condense and reflux , reacted for 7 hours, after the reaction ended, cooled to normal temperature;

[0024] Purification: Filter out the solvent in the reaction kettle, add 0.5kg of deionized water, neutralize it with 50% hydrochloric acid to PH=7, put the solution into another reaction kettle with 10kg of acetone, precipitate for 2 hours, and remove it by filtration Acetone solvent, washed 3 times with 85% ethanol, and then washed once with absolute ethanol, and vacu...

Embodiment 2

[0028] Pulverization: pulverize chitin into 100-mesh powder with a pulverizer to obtain chitin powder for later use;

[0029] Swelling: Soak 1kg of chitin powder in 3kg of 20% sodium hydroxide aqueous solution for 24 hours at minus 18°C, then thaw at room temperature;

[0030] Synthesis: Put thawed chitin into the reaction kettle, inject 10kg of isopropanol and 0.1kg of catalyst pyranpolyamine polyester (CAPP), stir, gradually raise the temperature to 35°C, keep warm for 1.5 hours, then add 3kg of propylene oxide , condensed and refluxed, reacted for 8 hours, after the reaction was finished, cooled to normal temperature;

[0031] Purification: Filter out the solvent in the reaction kettle, add 0.4kg of deionized water, neutralize it with 50% hydrochloric acid to PH=7, put the solution into another reaction kettle with 10kg of acetone, precipitate for 2 hours, and remove it by filtration Acetone solvent, washed twice with 85% ethanol, and then washed twice with absolute ethano...

Embodiment 3

[0035] Pulverization: pulverize chitin into 40-mesh powder with a pulverizer to obtain chitin powder for subsequent use;

[0036] Swelling: Soak 1kg of chitin powder in 3kg of 25% sodium hydroxide aqueous solution for 12 hours at minus 20°C, then thaw at room temperature;

[0037] Synthesis: Put thawed chitin into the reaction kettle, inject 8kg of isopropanol and 0.2kg of catalyst pyranpolyamine polyester (CAPP), stir, gradually raise the temperature to 45°C, keep warm for 1.5 hours, then add 3kg of epoxy chlorine Propane, condensed and refluxed, reacted for 5 hours, after the reaction was finished, cooled to normal temperature;

[0038] Purification: Filter out the solvent in the reaction kettle, add 0.6kg of deionized water, neutralize it with 50% hydrochloric acid to PH=7, put the solution into another reaction kettle with 10kg of acetone, precipitate for 2 hours, and remove it by filtration Acetone solvent, washed 3 times with 85% ethanol, and then washed 2 times with ab...

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PUM

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Abstract

The invention discloses a chemical synthesis method of water-soluble hydroxypropyl chitin, and belongs to the technical field of organic synthesis chemistry. The chemical synthesis method of the hydroxypropyl chitin comprises the following steps: crushing chitin into powder with meshes of 40 or above; soaking chitin powder with a 20-25% sodium hydroxide aqueous solution for 12-24 hours at a temperature of 18-20 DEG c, and unfreezing; and synthesizing and purifying after unfreezing to obtain the hydroxypropyl chitin. The mass ratio of the raw materials is as follows: chitin: sodium hydroxide aqueous :pyranopolyamine polyester: isopropanol: propylene oxide or epichlorohydrin: acetone: deionized water= 1: 3: 0.1-0.2: 8-10: 3: 1: 0.4-0.6; and the hydroxypropyl chitin synthesized by the invention has good water solubility, film forming property and excellent air tightness.

Description

technical field [0001] The invention relates to a chemical synthesis method of water-soluble hydroxypropyl chitin, which belongs to the technical field of organic synthesis chemistry. Background technique [0002] Chitin is a natural polysaccharide mainly found in the shells of shrimps, crabs and other organisms. The molecular structure of chitin is similar to that of cellulose, except that the hydroxyl group at the C2 position is replaced by an acetamide group. Due to the strong hydrogen bond in the chitin molecule, there is an ordered structure between the molecules, which makes the crystal dense and stable. [0003] Chitin can only be dissolved in a mixed solvent of 5% lithium chloride, hexafluoroisopropanol, hexafluoroacetone, 1,2-dichloroethane, dimethylformamide and trichloroacetic acid, and insoluble in other organic solvents And dilute acid, alkali solution, its industrial application is greatly restricted. Therefore, chemically synthesizing and modifying chitin t...

Claims

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Application Information

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IPC IPC(8): C08B37/08C09D105/08
Inventor 宋丛恺
Owner 青岛凯玉盈商贸有限公司
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