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A kind of preparation method of attapulgite-based MQ silicone resin

A technology of organosilicon and attapulgite, which is applied in the field of preparation of attapulgite-based MQ silicone resin, to achieve the effects of strong adsorption performance, high heat resistance and large surface energy

Active Publication Date: 2016-04-27
SHANDONG CAYON TESTING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, this method has not been reported in the literature

Method used

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  • A kind of preparation method of attapulgite-based MQ silicone resin
  • A kind of preparation method of attapulgite-based MQ silicone resin
  • A kind of preparation method of attapulgite-based MQ silicone resin

Examples

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Effect test

Embodiment 1

[0028] 1. Preparation of fibrous nano silica and water glass mixture: disperse attapulgite into sodium hydroxide solution, stir at 100°C for 24 hours to prepare fibrous nano silica and water glass mixture, in which sodium hydroxide The concentration of the solution is 20mol / L, and the mass ratio of attapulgite to sodium hydroxide solution is 0.05:1;

[0029] 2. Preparation of attapulgite-based MQ silicone resin dispersion: under constant stirring, add the mixture of fibrous nano-silica and water glass to concentrated hydrochloric acid, adjust the pH value to 0.5, hydrolyze for 1 min, and then add hexamethyl di Ethanol solution of siloxane, co-hydrolyzed for 120min, the mass ratio of hexamethyldisiloxane and attapulgite initially added was 1:1, and the co-hydrolysis temperature was controlled at 100°C to obtain attapulgite-based MQ silicone resin dispersion ;

[0030] 3. Post-treatment: extract with toluene, take the upper oil layer, wash until neutral and then dry at 120°C to...

Embodiment 2

[0032] 1. Preparation of the mixture of fibrous nano-silica and water glass: disperse attapulgite into potassium hydroxide solution, stir at 20°C for 0.5h to prepare a mixture of fibrous nano-silica and water glass, in which The concentration of potassium solution is 0.5mol / L, and the mass ratio of attapulgite to potassium hydroxide solution is 0.25:1;

[0033] 2. Preparation of attapulgite-based MQ silicone resin dispersion: under constant stirring, add a mixture of fibrous nano-silica and water glass to concentrated hydrochloric acid, adjust the pH value to 5, hydrolyze for 60 minutes, and then add trimethyl chloride The methanol solution of silane was co-hydrolyzed for 1 min, the mass ratio of trimethylchlorosilane to initially added attapulgite was 0.01:1, and the co-hydrolysis temperature was controlled at 20°C to obtain an attapulgite-based MQ silicone resin dispersion;

[0034] 3. Post-treatment: extract with xylene, take the upper oil layer, wash until neutral and then...

Embodiment 3

[0036] 1. Preparation of the mixture of fibrous nano-silica and water glass: disperse attapulgite into sodium hydroxide and stir at 80°C for 4 hours to prepare a mixture of fibrous nano-silica and water glass, in which the sodium hydroxide solution The concentration is 10mol / L, and the mass ratio of attapulgite to lye is 0.1:1;

[0037] 2. Preparation of attapulgite-based MQ silicone resin dispersion: under constant stirring, add the mixture of fibrous nano-silica and water glass to concentrated hydrochloric acid, adjust the pH value to 2, hydrolyze for 15 minutes, and then add γ-aminopropyl The absolute ethanol solution of γ-aminopropyltriethoxysilane was hydrolyzed for 60 minutes. The mass ratio of γ-aminopropyltriethoxysilane to the initially added attapulgite was 0.1:1, and the cohydrolysis temperature was controlled at 80°C to obtain attapulgite Earth-based MQ silicone resin dispersion;

[0038] 3. Post-processing: extract with silicone oil, take the upper oil layer, was...

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Abstract

The invention discloses a method for preparing an attapulgite-based MQ organic silicon resin. The resin is prepared by the following steps of firstly, preparing the attapulgite into a mixture of fiber nanosilicon dioxide and sodium silicate in the presence of alkali, subsequently, in the presence of acid and M chain link organic silicon end-capping reagent, forming a dispersion liquid of the attapulgite-based MQ organic silicon resin, and treating to obtain a product. The resin has a synergic reinforcing effect on white carbon black and the MQ organic silicon resin, is relatively good in dispersity, large in specific surface area, good in thermal resistance and low in cost, and can be widely applied to fields such as surfactants, reinforcing materials, tackifiers, demolding agents, anti-sticking agents, brightening agents, scratch resisting agents and the like.

Description

technical field [0001] The invention relates to the technical field of preparation of silicone resin, in particular to a preparation method of attapulgite-based MQ silicone resin. Background technique [0002] MQ silicone resin is a very unique type of siloxane. It is a silicone resin composed of tetrafunctional siloxane polycondensation chains (Q) and monofunctional siloxane chains (M). Its molar mass is average. It is 1000-8000. The ratio of the amount of M chains to Q chains in the molecular structure and the structure determine the properties and application range of the resin. MQ silicone resin is mainly used in the following fields: first, surface treatment agents, such as silicone pressure-sensitive adhesives, mobile phone button glue, epoxy adhesive surface bonding, etc.; second, reinforcing materials, used in RTV glue, HTV Glue, addition type liquid silicone rubber, heat vulcanized rubber, potting glue for semiconductor components, etc.; the third is tackifier, use...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06C08G77/26C08G77/20C08K9/02C08K7/10C08K3/34
Inventor 张桂花杨安静康娇娇吕桂芝刘元元张国庆
Owner SHANDONG CAYON TESTING TECH
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