Hyperbranched polythioether polyamine, and preparation method and use thereof

A polysulfide and application technology, which is applied in the field of hyperbranched polysulfide polyamine and its preparation, can solve the problems of high equipment requirements and strict reaction conditions, and achieves the effects of low equipment requirements, simple preparation method and mild reaction conditions.

Active Publication Date: 2016-12-21
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional synthesis method of polyetheramine uses highly toxic acrylonitrile as raw material, and also uses high-pressure catalytic hydrogenation reaction, which requires high equipment and strict reaction conditions

Method used

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  • Hyperbranched polythioether polyamine, and preparation method and use thereof
  • Hyperbranched polythioether polyamine, and preparation method and use thereof
  • Hyperbranched polythioether polyamine, and preparation method and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] A kind of preparation method of hyperbranched polysulfide polyamine proposed by the present invention comprises the following steps;

[0028] S1: Put 1.12 grams (0.01 moles) of propynyl glycidyl ether and 2.27 grams (0.02 moles) of cysteamine hydrochloride into the reactor, and add 128 milligrams (0.5 millimoles) of benzoin dimethyl Ether and 30.5 grams of methanol, and under the irradiation of a 200W high-pressure mercury lamp, reacted at room temperature for 4 hours to obtain the α-epoxy-ω-amine hydrochloride solution. The chemical structure of α-epoxy-ω-amine hydrochloride was characterized by NMR, the results are as follows figure 1 shown.

[0029] S2: Add 10.13 g (0.10 moles) of triethylamine to the above-mentioned concentrated product, turn on the stirring device, and raise the temperature to the reflux temperature of the solvent for 24 hours to obtain hyperbranched polythioether polyamine hydrochloride. Its antibacterial and bactericidal properties are shown in...

Embodiment 2

[0032] A kind of preparation method of hyperbranched polysulfide polyamine proposed by the present invention comprises the following steps;

[0033] S1: Put 1.12 g (0.01 mol) of propynyl glycidyl ether and 1.70 (0.015 mol) of cysteamine hydrochloride into the reactor, and add 0.05 mmol of 2-hydroxymethylphenylpropane-1 -ketone and 42.3 grams of methanol-ethanol mixed solvent (volume ratio 7:3), and under the irradiation of a 100W high-pressure mercury lamp, reacted in an ice-water bath for 12 hours to obtain an α-epoxy group-ω-amine hydrochloride intermediate The solution;

[0034] S2: Add 1.52 g (0.015 mol) of triethylamine to the above product, turn on the stirring device, raise the temperature to 65° C., and react for 60 hours. Obtain hyperbranched polythioether polyamine hydrochloride solution;

[0035] S3: Add 2.70 g (0.015 mol) of sodium methoxide-methanol solution (concentration: 30%) to the above hyperbranched polythioether polyamine hydrochloride solution, and conti...

Embodiment 3

[0037] A kind of preparation method of hyperbranched polysulfide polyamine proposed by the present invention comprises the following steps;

[0038] S1: 1.12 g (0.01 mol) of propynyl glycidyl ether and 1.70 g (0.015 mol) of cysteamine hydrochloride were added to the reactor, and 0.15 mmol of 2-methyl-1-[4- Methylthiophenyl]-2-morpholino-1-propanone and 33.84 grams of methanol-water solution (volume ratio 4:1), and at 12000μW / cm 2 Under the irradiation of a special ultraviolet lamp, react at room temperature for 6 hours to obtain the methanol solution of the α-epoxy-ω-amine hydrochloride intermediate;

[0039] S2: Add 3.04 grams (0.030 moles) of triethylamine to the above solution, turn on the stirring device, raise the temperature to reflux temperature, and continue the reaction for 32 hours to obtain a hyperbranched polythioether polyamine hydrochloride solution;

[0040] S3: Add 0.81 g (0.015 mol) of sodium methoxide to the hyperbranched polythioether polyamine hydrochlorid...

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Abstract

The invention relates to the field of preparation methods of polyetheramine, and especially relates to a hyperbranched polythioether polyamine, and a preparation method and a use thereof. The preparation method is simple, raw materials are nontoxic and are easy to obtain, cysteamine hydrochloride can be prepared through hydrolyzing human and animal hair, alkynyl glycidyl ether can be directly purchased, and the method also has the advantages of low requirements of devices involved in the preparation process, no special or strict conditions, and mild reaction conditions. The molecular periphery of the hyperbranched polythioether polyamine has a plurality of primary amino groups, so the hyperbranched polythioether polyamine can be used as an epoxy resin flexible curing agent; and hyperbranched polythioether polyamine hydrochloride which is the precursor of the hyperbranched polythioether polyamine has a strong fluorescence effect, a good antibacterial performance and a good sterilizing performance.

Description

technical field [0001] The invention relates to the field of preparation methods of polyether amines, in particular to a hyperbranched polysulfide polyamine, its preparation method and application. Background technique [0002] Polyether amine compounds have low toxicity and low volatility, and are often used as curing agents for epoxy resins, which can greatly improve the flexibility of cured products. The traditional synthesis method of polyetheramine uses potassium hydroxide as a catalyst to react acrylonitrile and diethylene glycol to synthesize polyethernitrile; then, polyethernitrile undergoes hydrogenation reaction under the catalysis of Raney nickel to obtain polyetheramine. The traditional synthesis method of polyetheramine uses highly toxic acrylonitrile as raw material, and also uses high-pressure catalytic hydrogenation reaction, which requires high equipment and strict reaction conditions. Contents of the invention [0003] The purpose of the present inventio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G59/50B01J20/26A01N33/12A01N33/08A01P3/00A01P1/00C09K11/06
CPCA01N33/08A01N33/12B01J20/262C08G59/50C08G75/02C09K11/06C09K2211/14
Inventor 郑耀臣张新涛高正国张慧敏邸秀丽
Owner YANTAI UNIV
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