Epoxy group-containing organosilicon compound and preparation method thereof, and epoxy resin composition and preparation method thereof

A technology of organosilicon compound and epoxy group, which is applied in the field of polyetheramine and organosilicon synergistically toughened fast-curing epoxy resin composition and its preparation, which can solve the problems of high curing temperature, singleness, and limited toughness improvement effect , to achieve the effect of good flexibility

Active Publication Date: 2021-03-30
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Patent CN108250684A adopts the method of chemically modifying the curing agent to prepare a flexible curing agent, CN102604117A adopts the method of chemically modifying the epoxy resin, and patent CN101525519A directly uses the curing agent with good toughness to improve the epoxy cured product. Toughness, although the toughness of the cured product has been improved, but the types of curing agents used in these three patents all have the disadvantages of high curing temperature and slow curing speed
Patent CN110819283A also uses a high-toughness curing agent to toughen the epoxy cured product, but the scheme of only using a high-toughness curing agent for toughening is too simple, and the effect of improving toughness is very limited

Method used

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  • Epoxy group-containing organosilicon compound and preparation method thereof, and epoxy resin composition and preparation method thereof
  • Epoxy group-containing organosilicon compound and preparation method thereof, and epoxy resin composition and preparation method thereof
  • Epoxy group-containing organosilicon compound and preparation method thereof, and epoxy resin composition and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0074] Preparation of cured product test samples: first raise the temperature of the polytetrafluoroethylene mold to 40°C and keep it warm for 10-20 minutes. According to the above curing process, mix A and B components, defoam, pour into the mold to level off naturally, and cure at 40°C for 5 hours. Wait for the mold to cool down naturally, and demould.

[0075] Process the above cured sample into 50×10×4mm 3 According to the national standard GB / T 2567 "Resin Casting Body Performance Test Method", the elongation at break was tested with a universal material testing machine (Germany, Zwick / Roell Z020).

[0076] 3. Gel content test of cured epoxy resin

[0077] The gel content of cured epoxy resin was determined by extraction method. Take 0.25g cured product test sample, cut into several 1.5×1.5×1mm 3 small piece, weighed as m 1 , with xylene as the extractant, extracted in a Soxhlet extractor for 24 hours, rinsed with xylene three times after the sample was taken out, th...

Embodiment 1

[0111] To prepare 1,1,3,3-tetramethyl-1-vinyl-3-epoxydisiloxane, the steps are:

[0112] 1) m-chloroperoxybenzoic acid was dissolved in dichloromethane to prepare solution A of 0.696mol / L;

[0113] 2) Dissolving tetramethyldivinyldisiloxane in dichloromethane to prepare 0.4mol / L solution B;

[0114] 3) Add solution A dropwise to solution B (the molar ratio of m-chloroperoxybenzoic acid to tetramethyldivinyldisiloxane is 2.5:1) under the condition of 0-4°C ice bath, dropwise The time was 1 hour. After the addition was completed, the temperature was raised to 50° C., and the reaction was refluxed for 47 hours; the progress of the reaction was monitored by thin-layer chromatography (using a mixed solvent with a mass ratio of hexane and ethyl acetate of 5:3). After the reaction finished, the crude product obtained was subjected to two times of pickling (using 5wt% 2,3-dihydroxysuccinic acid aqueous solution) and three times of alkali washing (using 5% NaHCO 3 aqueous solution), ...

Embodiment 2

[0117] To prepare 1,1,3,3-tetramethyl-1-vinyl-3-epoxydisiloxane, the steps are:

[0118] 1) Dissolving m-chloroperoxybenzoic acid in methylene chloride is prepared as solution A of 0.6mol / L;

[0119] 2) Dissolving tetramethyldivinyldisiloxane in dichloromethane to prepare 0.3mol / L solution B;

[0120] 3) Add solution A dropwise to solution B (the molar ratio of m-chloroperoxybenzoic acid to tetramethyldivinyldisiloxane is 2:1) under the condition of 0-4°C ice bath, dropwise The time was 1 hour. After the addition was completed, the temperature was raised to 55° C., and the reaction was refluxed for 46 hours; the progress of the reaction was monitored by thin-layer chromatography (using a mixed solvent with a mass ratio of hexane and ethyl acetate of 5:3). After the reaction finished, the crude product obtained was subjected to two times of pickling (using 5wt% 2,3-dihydroxysuccinic acid aqueous solution) and three times of alkali washing (using 5% NaHCO 3 aqueous solution), ...

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Abstract

The invention relates to an epoxy group-containing organosilicon compound and a preparation method thereof, and an epoxy resin composition and a preparation method thereof. Molecules of the organosilicon compound contain -Si-O-C- bonds, and the organosilicon compound has the characteristics of large bond angle, long bond length, low surface tension and the like. By utilizing the reactivity of an epoxy group in the organosilicon compound, an organosilicon molecular long chain is introduced into an epoxy resin cross-linked network and has a synergistic effect with polyether amine and the like, so that the curing rate can be increased, the toughness of an epoxy resin cured product is greatly improved, and the mechanical property is improved; meanwhile, the light/heat aging resistance of the cured product is also greatly improved, so that the organosilicon compound can be widely applied to the fields of adhesives, wind turbine blades and the like.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to an epoxy group-containing organosilicon compound and a preparation method thereof, and a polyetheramine and organosilicon synergistically toughened fast-curing epoxy resin composition prepared therefrom and its preparation method. Background technique [0002] Epoxy resin has the advantages of high storage stability, good processing performance, flexible formula design, low volume shrinkage during curing, etc., and its cured product has excellent mechanical properties, dimensional stability, chemical resistance, and electrical properties. , bonding properties, etc., have been widely used in various fields of production and life, such as adhesives, composite materials, machinery manufacturing, electronics, aerospace, transportation, construction, military and other fields. However, the cured epoxy resin generally has low toughness, which leads to limitations in its prac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/14C08G77/06C08L63/00C08L83/06C08L71/00C08K5/17
CPCC08G77/045C08G77/06C08L63/00C08L2205/03C08L2201/08C08L83/06C08L71/00C08K5/17
Inventor 张文清刘赵兴刘大伟周萌张春
Owner WANHUA CHEM GRP CO LTD
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