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Low molecular siloxane and preparation method thereof as well as used catalyst and preparation method thereof

A molecular siloxane and catalyst technology, applied in metal/metal oxide/metal hydroxide catalysts, heterogeneous catalyst chemical elements, physical/chemical process catalysts, etc., can solve the problem of wide molecular weight distribution of reaction products and difficult products. Separation, waste liquid polluting the environment, etc., to achieve the effects of high practical value, multiple reuse times, and strong reaction selectivity

Active Publication Date: 2017-01-11
岳阳凯门水性助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regarding the telomerization process, it has been reported in the literature that concentrated sulfuric acid or strongly acidic cation exchange resins were used as catalysts, but the results were not satisfactory.
When concentrated sulfuric acid is used as a catalyst, the product is not easy to separate, it needs to be neutralized and washed, the waste liquid pollutes the environment, and the catalytic effect is weak
Strongly acidic cation exchange resin itself has a high water content, resulting in a wide molecular weight distribution of the reaction product and low product quality

Method used

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  • Low molecular siloxane and preparation method thereof as well as used catalyst and preparation method thereof
  • Low molecular siloxane and preparation method thereof as well as used catalyst and preparation method thereof
  • Low molecular siloxane and preparation method thereof as well as used catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Preparation of catalyst

[0036] The first step: Slowly drop 500ml, 0.5mol / L ammonia water into 100ml, 0.5mol / L Zr(NO 3 ) 4 In the aqueous solution, to pH = 9-10, zirconium hydroxide precipitates, and then reflux in an oil bath at 100°C for 24 hours. The precipitate was repeatedly washed with deionized water and filtered to pH = 7, and the filter cake was dried at 105 °C to obtain 5.37 g of ZrO 2 , take 1gZrO 2 Soak in 16.5ml, 1mol / LH 8 N 2 o 4 In the W solution, add 10L, 2.0mol / LAl(NO 3 ) 3 aqueous solution, the mixture was refluxed at 120°C for 18 hours, then dried at 110°C for 10 hours, and calcined for 3 hours to obtain 1020 g of crude product.

[0037] The second step: take 20g of the product of the first step and soak it in 32ml, 0.005mol / L chloroplatinic acid aqueous solution, overnight, dry at 110°C for 10 hours, and roast for 3 hours to obtain Pt / WO 3 / ZrO 2 -γ-Al 2 o 3 Supported solid acid catalyst 20.05g.

Embodiment 2

[0039] The difference from Example 1 is that the H 8 N 2 o 4 W solution is replaced by sulfuric acid solution, other reaction conditions are the same, and finally Pt / SO 4 2- / ZrO 2 -γ-Al 2 o 3Supported solid acid catalyst.

Embodiment 3

[0041] The difference with Example 1 is that the ratio of the chloroplatinic acid aqueous solution to the first step product is different, and the product 20g of the first step is immersed in 32ml, in the 0.001mol / L chloroplatinic acid aqueous solution

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Abstract

The invention provides a preparation method of low molecular siloxane as well as a used catalyst and a preparation method thereof. The catalyst is a solid acid catalyst formed by a supporter loaded active component, wherein the active component at least contains platinum and zirconium oxide in a ratio of 1:(1-5). The preparation method of the low molecular siloxane comprises the following steps: by taking high hydrogen-containing silicone oil as a raw material, carrying out telomerization at the temperature of 50-110 DEG C in presence of a blocking agent and the catalyst, so that the low molecular siloxane is obtained. A novel catalyst is provided for preparation of the low molecular siloxane by adopting a telomerization process, and the catalyst has the advantages of high catalysis efficiency, specific product and high reutilization frequency.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing low-molecular siloxane, a catalyst used therefor, and a preparation method. Background technique [0002] High-hydrogen pentasiloxane and hexasiloxane are relatively small types of silicone oil products, but they have broad application prospects and are the starting materials for modified silicone oil. A variety of modified silicone oils can be obtained from the active group hydrogen in the main chain of siloxane, and many other active groups through the hydrosilylation reaction, such as polyether modified silicone oil, epoxy hydrocarbon modified silicone oil, long chain Alkyl silicone oil, etc. It is characterized by small molecular weight, can be cross-linked at low temperature to form a film, and forms a waterproof layer on the surface of the substance. The wetting effect of the product after the hydrosilylation reaction is particularly prominent, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08B01J23/652B01J27/053
CPCB01J23/002B01J23/652B01J27/053B01J2523/00B01J2523/31B01J2523/48B01J2523/69
Inventor 卓耀文周海军向阳
Owner 岳阳凯门水性助剂有限公司
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