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Epoxy resin containing fluorine, phosphorus and silicon and preparation method thereof

A technology of epoxy resin and oxygen, which is applied in the direction of organic chemistry, can solve the problems of low heat release, only improving the heat resistance and flame retardancy of epoxy resin, and poor flame retardancy

Inactive Publication Date: 2016-03-16
HEFEI FUMING SEALING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The Chinese magazine "Acta Polymer Sinica" introduced on pages 148-153 of the second issue of February 2012 that organosilicon flame retardants have the characteristics of low burning rate, low heat release, anti-dripping, and good environmental performance. When used to modify epoxy resin, it can improve the flexibility and heat resistance of epoxy resin, but the flame retardant effect of silicon-containing epoxy resin is poor; studies have shown that silicon and phosphorus have a synergistic flame retardant effect, combining organic phosphorus and phosphorus When silicone is used to modify epoxy resin, the obtained epoxy resin has better flame retardancy and heat resistance
[0005] The technical solutions disclosed in the above prior art either only improve the water absorption of epoxy resin, or only improve the heat resistance and flame retardancy of epoxy resin, and there is no report that can effectively improve the water absorption of epoxy resin at the same time , heat resistance and flame retardancy technology

Method used

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  • Epoxy resin containing fluorine, phosphorus and silicon and preparation method thereof
  • Epoxy resin containing fluorine, phosphorus and silicon and preparation method thereof
  • Epoxy resin containing fluorine, phosphorus and silicon and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Mix 60g of o-chlorobenzotrifluoride with 45g of concentrated sulfuric acid (95%), wherein 95% in parentheses refers to the mass percent concentration of concentrated sulfuric acid, and then dropwise add 70g of concentrated nitric acid (65%) and 60g of concentrated sulfuric acid to the mixture (95%), stirred and reacted at 50°C for 4 hours, poured the reactant into 500ml of ice water, separated the oily substance in the lower layer, washed the oily substance with deionized water until neutral, distilled under reduced pressure, and The distilled concentrate was vacuum-dried at 60°C for 24 hours to obtain 2-chloro-5-nitro-trifluorotoluene;

[0046] Take 71.6g of bis(3-hydroxyphenoxy)phenyl phosphate and dissolve in 100ml of DMF solvent (DMF is the English alias of N,N-dimethylformamide), heat to dissolve, and then slowly dropwise add A mixture composed of 11.5g of methyldichlorosilane and 40ml of DMF, finally added 20.2g of triethylamine, reacted at 80°C for 24h, filtered ...

Embodiment 2

[0051] Mix 60g of o-chlorobenzotrifluoride with 45g of concentrated sulfuric acid (98%), then add dropwise a mixture of 50g of concentrated nitric acid (68%) and 90g of concentrated sulfuric acid (98%), and stir at 40°C After reacting for 5 hours, pour the reactant into 500ml of ice water, separate the oily substance in the lower layer, wash the oily substance with deionized water until neutral, distill under reduced pressure, and vacuum-dry the distillation concentrate at 60°C for 24h to obtain 2 -Chloro-5-nitro-trifluorotoluene;

[0052] Take 64.8g of 10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and dissolve it in 90ml of DMF solvent, heat to dissolve, Then slowly add dropwise a mixture of 12.9g of dimethyldichlorosilane and 50ml of DMF, and finally add 20.2g of triethylamine, react at 100°C for 20h, and filter to remove triethylamine generated during the reaction salt, the filtrate was distilled under reduced pressure to remove the solvent, a...

Embodiment 3

[0057] Mix 30g of o-chlorobenzotrifluoride with 25g of concentrated sulfuric acid (97%), then add dropwise a mixture of 30g of concentrated nitric acid (67%) and 40g of concentrated sulfuric acid (97%), and stir at 35°C After reacting for 5.5 hours, pour the reactant into 400ml of ice water, separate the oily substance in the lower layer, wash the oily substance with deionized water until neutral, distill under reduced pressure, and dry the distillation concentrate at 60°C for 24h in vacuum to obtain 2-Chloro-5-nitro-trifluorotoluene;

[0058] Take 64.8g of 10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and dissolve it in 120ml of DMF solvent, heat to dissolve, Then slowly add a mixture of 11.5g of methyldichlorosilane and 40ml of DMF dropwise, and finally add 21.4g of triethylamine, react at 60°C for 28h, and filter to remove the triethylamine salt generated during the reaction , the filtrate was distilled off under reduced pressure to remove the...

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Abstract

The invention discloses a fluorine-containing, phosphorus-containing and silicon-containing epoxy resin and a preparation method for the same. The preparation method for the fluorine-containing, phosphorus-containing and silicon-containing epoxy resin comprises the following steps of: taking 100 phr of bisphenol-A epoxy resin, 10-60 phr of a diamine curing agent, and 1-6 phr of a curing accelerator; uniformly mixing the three raw materials and then placing the mixture in a reaction die; and performing a curing reaction for 1-3 hours in the condition of 80-120 DEG C, and then performing a curing reaction for 2-4 hours in the condition of 130-170 DEG C, so as to obtain the fluorine-containing, phosphorus-containing and silicon-containing epoxy resin, wherein the diamine curing agent is a fluorine-containing, phosphorus-containing and silicon-containing diamine compound. The fluorine-containing, phosphorus-containing and silicon-containing epoxy resin is introduced with three elements of fluorine, phosphorus and silicon simultaneously, and is a new organic compound; simultaneously, the fluorine-containing, phosphorus-containing and silicon-containing epoxy resin has the characteristics of good surface performance, low water absorption, acid-base corrosion resistance, heat resistance and excellent flame resistance.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to an epoxy resin and a preparation method thereof. Background technique [0002] Epoxy resin has excellent chemical, dielectric and mechanical properties, and it is widely used in various industrial fields, such as adhesives, coatings, laminates, semiconductor packaging and insulating materials in electronic equipment, but epoxy resin has resistance The disadvantages of poor thermal performance, flammability and easy water absorption limit its application in high-end fields. [0003] The Chinese magazine "China Adhesives" introduced on pages 55-60, Volume 19, Issue 3, 2010, that the introduction of fluorine into epoxy resin can improve its surface tension, and fluorine-containing epoxy resin has good hydrophobicity and oil resistance. . [0004] The Chinese magazine "Acta Polymer Sinica" introduced on pages 148-153 of the second issue of February 2012 that o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/50C07F19/00
Inventor 徐文总任明元
Owner HEFEI FUMING SEALING MATERIAL