Organic silicon episulfide resin and preparation method thereof

A technology of episulfide resin and silicon epoxy resin, which is applied in the direction of silicon organic compounds, can solve the problems of macroscopic phase separation and inability to achieve modification, and achieve the effects of high refractive index, high curing reactivity and low viscosity

Inactive Publication Date: 2011-10-19
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the direct blending of silicone material and epoxy resin will lead to macroscopic phase separation, the purpose of modification cannot be achieved

Method used

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  • Organic silicon episulfide resin and preparation method thereof
  • Organic silicon episulfide resin and preparation method thereof
  • Organic silicon episulfide resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add allyl glycidyl ether (35.7 grams, 0.31mol), toluene 50ml and 10ppm (in total weight of the reactant) chloroplatinic acid catalyst in a 250ml three-necked flask equipped with mechanical stirring, condenser and thermometer. The temperature of the above reaction mixture was raised to 70° C., (15 g, 0.0625 mol) octamethyltetrahydrocyclotetrasiloxane was added dropwise within 30 minutes, and the reaction was continued for 4 hours after the dropwise addition was completed. After the reaction was completed, the toluene solvent and unreacted reactants were removed with a rotary evaporator at 2mmHg / 80°C to obtain 41.5 grams of colorless and transparent silicone epoxy resin A with the following structural formula, and the yield was about 95.4%. The refractive index is 1.46.

[0028]

[0029] In a 100ml there-necked flask equipped with mechanical stirring and a thermometer, add the above-mentioned organosilicon epoxy resin A (8.7 grams, 0.0125mol), potassium thiocyanate (KS...

Embodiment 2

[0033] Add allyl glycidyl ether (14.4 grams, 0.125mol), toluene 50ml and 10ppm (in total weight of the reactant) chloroplatinic acid catalyst in a 250ml three-necked flask equipped with mechanical stirring, condenser and thermometer. The temperature of the resulting reaction solution was raised to 70° C., and (15 g, 0.0625 mol) octamethyltetrahydrocyclotetrasiloxane was added dropwise within 30 minutes, and the reaction was continued for 4 hours after the dropwise addition was completed. After the reaction was completed, the toluene solvent and unreacted reactants were removed with a rotary evaporator at 2mmHg / 80°C to obtain 28.1 grams of colorless and transparent silicone epoxy resin B with the following structural formula, and the yield was about 95.6%. The product The refractive index is 1.44.

[0034]

[0035] Add the organosilicon epoxy resin B (5.68 grams, 0.0125mol), potassium thiocyanate (KSCN) (2.43 grams, 0.05mol) (2.43 grams, 0.05mol), deionized water 10ml and Eth...

Embodiment 3

[0039] Add allyl glycidyl ether (35.7 grams, 0.31mol), toluene 50ml and 10ppm (in total weight of the reactant) chloroplatinic acid catalyst in a 250ml three-necked flask equipped with mechanical stirring, condenser and thermometer. The temperature of the resulting reaction solution was raised to 70° C., and (15 g, 0.112 mol) tetramethyldihydrodisiloxane was added dropwise within 30 minutes, and the reaction was continued for 4 hours after the dropwise addition was completed. After the reaction was completed, the toluene solvent and unreacted reactants were removed with a rotary evaporator at 2mmHg / 80°C to obtain 38.74 grams of colorless and transparent silicone epoxy resin C with the following structural formula, and the yield was about 95.6%. The refractive index is 1.45.

[0040]

[0041] Add the silicone epoxy resin C (9.05 grams, 0.025mol), potassium thiocyanate (KSCN) (14.58 grams, 0.15mol) and 40ml of deionized water obtained above in a 100ml three-necked flask equip...

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Abstract

The invention relates to an organic silicon episulfide resin and a preparation method thereof. The preparation method comprises the steps of: mixing organic silicon epoxy resin with deionized water, ethanol and potassium thiocyanate or thiocarbamide, and reacting the mixture at temperature of 15-45 DEG C for 12-36 hours; and after reaction is finished, adding organic solvent so as to divide the reacted mixture into two layers, separating out and washing an organic phase to be neutral, adding anhydrous sodium sulfate into the organic phase, and drying for 5-15 hours, filtering to remove sodiumsulfate, and removing the organic solvent at 2-10mmHg / 45-60 DEG C, thus obtaining organic silicon episulfide resin with the following structure. The organic silicon episulfide resin has the advantages of lower viscosity, high purity, high cure reaction activity, high refractive index, small heat release amount during condensate reaction, high glass transition temperature, low water absorption rate, and the like, thus being expected to be applied in the fields coating, adhesives, electronic device packaging, composite material matrix resin and the like.

Description

technical field [0001] The invention relates to an organosilicon episulfide resin and a preparation method thereof. Background technique [0002] Epoxy resin has many advantages such as good mechanical properties, high bonding strength, and good process performance, and is widely used in adhesives, coatings, composite material matrix resins, electronic packaging and other fields. However, epoxy resins are brittle and usually require toughening modifications. Among them, the use of elastomers for toughening is one of the most successful modification methods. Due to the excellent heat resistance, moisture resistance, and UV aging resistance of silicone elastomers, silicone-modified epoxy resins have been more and more widely studied in recent years. Since the direct blending of silicone material and epoxy resin will lead to macroscopic phase separation, the purpose of modification cannot be achieved. Therefore, it is necessary to synthesize polymers or monomers that contain...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/392C07F7/21C07F7/08
Inventor 黄伟蓝小康赵晓娟张瑛余云照
Owner INST OF CHEM CHINESE ACAD OF SCI
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