O-hydroxypropyl chitosan and preparation method thereof

A technology of hydroxypropyl chitosan and chitosan, which is applied in the field of chitosan, can solve the problems of low molecular weight of hydroxypropyl chitosan, unclear modification sites, unsuitable for flocculation products, etc., and achieve product High relative molecular weight, improved water solubility, and low production cost

Inactive Publication Date: 2018-03-27
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The modification site is not clear, it takes a long time, and the relative molecular weight of the modified hydroxypropyl chitosan is low, so it is not suitable for the use of flocculation products

Method used

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  • O-hydroxypropyl chitosan and preparation method thereof
  • O-hydroxypropyl chitosan and preparation method thereof
  • O-hydroxypropyl chitosan and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Step 1, dissolving 9g of sodium hydroxide in 30mL of distilled water to obtain a sodium hydroxide solution;

[0035] Step 2: Add 1g of chitosan to the above sodium hydroxide solution and alkalize for 30 minutes; pour off the upper layer of lye, add the alkalized chitosan to 20mL of isopropanol, and stir for 30 minutes at 25r / min , and the temperature was raised to 60° C., and then slowly added 8 g of propylene oxide and 2 mL of tetramethylammonium hydroxide solution with a mass fraction of 10%, and continued to react for 6 hours to obtain a suspension a;

[0036] Step 3, the suspension a was left to stand for 30min, the supernatant was poured off, and the hydrochloric acid solution with a mass fraction of 18.5% was added to adjust the pH of the solution to 7; 2:1, suction filtration after standing, and then wash with acetone and ethanol successively to obtain filter cake b;

[0037] Step 4, the filter cake b was Soxhlet extracted with ethanol as a solvent for 8 hours, ...

Embodiment 2

[0042] Step 1, dissolving 12g of sodium hydroxide in 30mL of distilled water to obtain a sodium hydroxide solution;

[0043] Step 2: Add 1 g of chitosan to the above-mentioned sodium hydroxide solution, and alkalize for 60 minutes; remove the upper layer of lye, add the alkalized chitosan to 20 mL of isopropanol, and stir at 25 r / min for 30 minutes. And raise the temperature to 60°C, then slowly add 10g of propylene oxide and 2mL of tetramethylammonium hydroxide solution with a mass fraction of 10%, and continue the reaction for 6h to obtain a suspension a;

[0044] Step 3, the suspension a was left to stand for 40 minutes, the supernatant liquid was poured off, and hydrochloric acid with a mass fraction of 18.5% was added to adjust the pH of the solution to 7; then 50 mL of a mixed solution of acetone and ethanol was added, and the volume ratio of ethanol and acetone was 2:1, suction filtration after standing, and then wash with acetone and ethanol successively to obtain filt...

Embodiment 3

[0050] Step 1, dissolving 9g of sodium hydroxide in 30 parts of mL distilled water to obtain a sodium hydroxide solution;

[0051]Step 2: Add 1 g of chitosan to the above-mentioned sodium hydroxide solution, and alkalize for 10 minutes; remove the upper layer of lye, add the alkalized chitosan to 20 mL of isopropanol, and stir at 25 r / min for 30 minutes. And raise the temperature to 80°C, then slowly add 15g of propylene oxide and 2mL of tetramethylammonium hydroxide solution with a mass fraction of 10%, and continue the reaction for 3h to obtain suspension a;

[0052] Step 3, the suspension a was left to stand for 50 minutes, the supernatant was poured off, and hydrochloric acid with a mass fraction of 18.5% was added to adjust the pH of the solution to 7.5; then 50 mL of a mixed solution of acetone and ethanol was added, and the volume ratio of ethanol and acetone was 2 : 1, suction filtration after standing, then wash with acetone and ethanol successively, obtain filter cak...

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Abstract

Provided are O-hydroxypropyl chitosan and a preparation method thereof, wherein the preparation method comprises the steps: adding chitosan to a sodium hydroxide solution, alkalizing, then adding intoisopropanol, stirring evenly, heating up to 40-80 DEG C, then adding a tetramethylammonium hydroxide solution and epoxypropane, continuing to carry out reaction for 3-8 h, allowing to stand, pouringto remove an upper-layer supernatant, adjusting the pH value to 6.5-7.5, then adding a mixed solution of acetone and ethanol, carrying out suction filtration to obtain a filter cake, carrying out Soxhlet extraction, and drying to obtain O-hydroxypropyl chitosan. O-hydroxypropyl chitosan is prepared by a nucleophilic substitution reaction of chitosan and epoxypropane. -OH of a C6 site of chitosan is activated by alkalization of sodium hydroxide, the modification position is clear, the purity is high, the post treatment is simple, and the product has good flocculation performance.

Description

technical field [0001] The invention belongs to the technical field of chitosan, and relates to an O-hydroxypropyl chitosan and a preparation method thereof. Background technique [0002] Chitosan is the only cationic polysaccharide existing in nature, and its chemical name is (1,4)-2-amino-2-deoxy-β-D-glucose. Chitosan is an important derivative of chitin, which is obtained by deacetylation of chitin. Because of its wide source, non-toxic and harmless, and biodegradable, it is widely used in many fields such as drug sustained release, wastewater treatment, papermaking additives, and daily chemical industry. Chitosan structure contains living wave -OH, -NH 2 It can adsorb impurity particles, metal ions, and organic dyes in wastewater, and has a good flocculation effect. However, due to the regularity of the chitosan molecule itself and the effect of intramolecular and intermolecular hydrogen bonds, the molecule is easy to form a crystalline region, thus having a crystalli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
Inventor 郭睿张瑶王宁韩双冯文佩霍文生李秀环刘雪艳
Owner SHAANXI UNIV OF SCI & TECH
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