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Preparation method of R-122-based episulfide resin

A technology of R-122 and epoxy resin, applied in the field of synthesizing R-122-based episulfide resin, can solve the problems of complicated curing process, lower melting point of resin and high melting point, and achieve simple process, short reaction time and low reaction temperature. Effect

Inactive Publication Date: 2011-08-31
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the problem that the existing technology has a high melting point, resulting in a complicated curing process, the present invention synthesizes R-122 episulfide resin through R-122, reduces the melting point of the resin, and solves the problem of its curing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: Get 20g of R-122 epoxy resin, 40mL of ethanol, the mass concentration of described ethanol is 95%, join in the three-necked container that is placed in the constant temperature water bath successively, stir until R-122 epoxy resin completely dissolved. Put the catalyst into the system, pass N 2 . Simultaneously add 9.29g thiourea and 92.9mL water thiourea aqueous solution and drop them evenly into the reaction system within 3h. At this time, the molar ratio of R-122 epoxy resin to thiourea is 5:1. After the dropwise addition, the reaction stage was formally entered, and the reaction temperature was controlled at 40° C.; the reaction time was 3 hours. Stir at a constant speed during the reaction, and the whole process is N 2 protection, filtering the reaction product, washing the resulting solid product with water, and recrystallizing to obtain an R-122-based episulfide resin; the episulfide resin is a white crystal;

[0021] The catalyst used is 0.012g...

Embodiment 2

[0022] Embodiment 2: Get 20g of R-122 epoxy resin, 40mL of ethanol, the mass concentration of described ethanol is 95%, join in the three-necked container that is placed in the constant temperature water bath successively, stir until R-122 epoxy resin completely dissolved. Put the catalyst into the system, pass N 2 . Simultaneously add 13g of thiourea and 130mL of water to the thiourea aqueous solution and drop them evenly into the reaction system within 3 hours. At this time, the molar ratio of R-122 epoxy resin to thiourea is 7:1. After the dropwise addition, the reaction stage is formally entered, and the reaction temperature is controlled at 30° C.; the reaction time is 5 hours. Stir at a constant speed during the reaction, and the whole process is N 2 protection, filtering the reaction product, washing the resulting solid product with water, and recrystallizing to obtain an R-122-based episulfide resin; the episulfide resin is a white crystal;

[0023] Used catalyzer ...

Embodiment 3

[0024] Embodiment 3: Get 20g of R-122 epoxy resin, 40mL of ethanol, the mass concentration of described ethanol is 95%, add in sequence in the three mouthful container that is placed in the constant temperature water bath, stir until R-122 epoxy resin completely dissolved. Put the catalyst into the system, pass N 2 . At the same time, add 5.57g of thiourea and 55.7mL of water in the thiourea aqueous solution and drop them evenly into the reaction system within 3 hours. At this time, the molar ratio of R-122 epoxy resin to thiourea is 3:1. After the dropwise addition, the reaction stage is formally entered, and the reaction temperature is controlled at 70° C.; the reaction time is 2 hours. Stir at a constant speed during the reaction, and the whole process is N 2 protection, filtering the reaction product, washing the resulting solid product with water, and recrystallizing to obtain an R-122-based episulfide resin; the episulfide resin is a white crystal;

[0025] The catal...

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PUM

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Abstract

The invention provides a preparation method of R-122-based episulfide resin. The ratio of the weight (g) of R-122 epoxy resin to the volume (mL) of ethanol is 1:2 and the mass concentration of ethanol is 95%. The preparation method comprises the following steps: adding the raw materials in a three-necked container in turn which is placed in a thermostatic water bath, stirring to ensure that R-122 epoxy resin is completely dissolved, adding catalyst, introducing N2, evenly dropping a thiourea solution in 3 hours to react under uniform stirring, wherein the ratio of the weight (g) of thiourea to the volume (mL) of water is 1:10, the molar ratio of R-122 epoxy resin to thiourea is 3:(1-7):1, the reaction temperature is controlled to 30-70 DEG C and the response time is 1-5 hours and the reaction is protected by N2; and filtering the reaction product, rinsing the obtained solid product, and recrystallizing to obtain the target product, wherein the melting point of the target product is 135-145 DEG C, which is 40 DEG C lower than the melting point of R-122 epoxy resin. The catalyst has low pollution, the cost performance of the product is low, the reaction temperature is low, the reaction time is short and the yield of the product is up to 70%.

Description

technical field [0001] The invention relates to a method for synthesizing R-122-based episulfide resin by utilizing R-122 epoxy resin. Background technique [0002] Epoxy resins have been widely used in various fields. Because episulfide resins are similar in structure to epoxy resins, they also have the advantages of epoxy resins such as excellent chemical resistance, adhesion, heat resistance, mechanical properties and curing stability. . Compared with epoxy resin, episulfide resin has its own advantages: [0003] 1. The ring sulfur ring has high activity and is easy to open the ring; [0004] 2. After ring opening, the sulfide ion is more stable and easier to initiate the polymerization reaction, and has a fast reaction rate; [0005] 3. The episulfide functional group can also react with metals such as copper and iron, and its bonding performance is higher than that of epoxy resin; [0006] Therefore, episulfide resin is more suitable for low-temperature fast-curing ...

Claims

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Application Information

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IPC IPC(8): C08G75/00C08G59/14
Inventor 张龙赵洋
Owner CHANGCHUN UNIV OF TECH
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