A kind of preparation method of high-purity methyl silicone oil

A methylsilicone oil, high-purity technology, applied in the field of preparation of high-purity methylsilicone oil, can solve problems such as affecting the polymerization reaction of methylsilicone oil, reduction of catalyst active sites, malodorous odor, etc., and achieves excellent metal ion adsorption performance, excellent The effect of denitrification performance and high catalytic activity

Active Publication Date: 2022-07-19
JIANGMEN SHENGPENG CHEM IND CO LTD
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Problems solved by technology

[0003] The method of using waste silicone rubber to produce and refine silicone oil has become a well-known technology in the industry. This method enables the waste to be effectively used again, which is worthy of vigorous promotion. However, the purity of the silicone oil obtained by this method is relatively low, mainly because the waste silicone rubber has undergone catalytic cracking. There are impurities such as sulfur-containing compounds, nitrogen-containing compounds and metal ions in the obtained DMC (Methylcyclosiloxane Mixed Ring Body). The presence of sulfur-containing compounds not only makes the product have a foul smell, but also affects the process of synthesizing methyl silicone oil. Safety, nitrogen-containing compounds are easy to react with the hydrogenation active center of the catalyst, resulting in the reduction of catalyst active sites, affecting the subsequent polymerization of methyl silicone oil, and the existence of metal ions affects the performance of methyl silicone oil. Therefore, how to improve silicon The purity of rubber catalytic cracking DMC is the key point for the preparation of high-purity methyl silicone oil, and the selection of catalysts is also very important in the production of methyl silicone oil. At present, the catalysts mainly include acid catalysts and basic catalysts. These catalysts need to be neutralized after use. , water washing, filtration and other processes, and there is a hazard of corrosion equipment, while tetramethylammonium hydroxide catalyzes the preparation of dimethyl silicone oil with mild reaction conditions, simple process, and no need for neutralization, which is suitable for continuous production, but tetramethylammonium hydroxide It is very easy to absorb water and promote the production of hydroxy silicone oil. Therefore, how to improve the purity of the catalytic cracking product of silicone rubber and select a suitable catalyst is the key point for the preparation of high-purity methyl silicone oil.

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  • A kind of preparation method of high-purity methyl silicone oil

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Embodiment 1

[0030] The present embodiment provides a kind of composite deamination agent, which is made by the following steps:

[0031] Step C1, put 0.1 mol of chloromethyl triazole, 0.1 mol of sodium ethoxide, and 100 mL of absolute ethanol in a three-necked flask, stir and react at 70 °C for 8 h under nitrogen protection, then add 0.1 mol of KH-550, and heat up to reflux for 24 h , filtered, and the filtrate was distilled under reduced pressure to remove dehydrated alcohol to obtain Intermediate 1;

[0032] Step C2: Mix 0.11 mol of intermediate 1, 0.11 mol of 3-propane sultone and 100 mL of absolute ethanol, stir at 50 °C for 8 h, add dropwise 12.3 mL of sulfuric acid solution with a concentration of 0.1 mol / L, and stir the reaction at 50 °C 12h, washed with anhydrous ether for three times, then distilled under reduced pressure to remove ethanol and ether to obtain Intermediate 2;

[0033] In step C3, 0.4 g of intermediate 2, 1 g of attapulgite and 100 mL of anhydrous toluene were pla...

Embodiment 2

[0035] The present embodiment provides a kind of composite deamination agent, which is made by the following steps:

[0036] Step C1, put 0.1 mol of chloromethyl triazole, 0.1 mol of sodium ethoxide, and 120 mL of absolute ethanol in a three-necked flask, stir and react at 70 °C for 8 h under nitrogen protection, then add 0.1 mol of KH-550, and heat up to reflux for 24 h , filtered, and the filtrate was distilled under reduced pressure to remove dehydrated alcohol to obtain Intermediate 1;

[0037] Step C2: Mix 0.11 mol of Intermediate 1, 0.11 mol of 3-propane sultone and 120 mL of absolute ethanol, stir at 50 °C for 8 h, dropwise add 13.5 mL of sulfuric acid solution with a concentration of 0.1 mol / L, and stir at 50 °C for reaction 12h, washed with anhydrous ether for three times, then distilled under reduced pressure to remove ethanol and ether to obtain Intermediate 2;

[0038] Step C3, put 0.6 g of intermediate 2, 1 g of attapulgite and 100 mL of anhydrous toluene in a th...

Embodiment 3

[0042] The present embodiment provides a solid catalyst, which is made by the following steps:

[0043] Step B1: Stir and mix 1 g of diatomaceous earth and 2.5 mL of deionized water for 20 minutes, add 0.5 mL of a 15% sulfuric acid solution, stir and react at 100°C for 4 hours, then add deionized water to dilute to 4 times the original volume, and continue The reaction was stirred for 1 hour, and then filtered. The filter cake was washed with deionized water until the washing liquid became neutral, dried at 100 °C for 4 hours, and calcined at 600 °C for 2 hours to obtain acidified diatomaceous earth;

[0044] Step B2: Dissolve zirconium oxychloride in distilled water, add acidified diatomaceous earth, irradiate with microwave for 3 minutes in a microwave oven with a power of 450W, then dry at 110°C, pre-bake at 700°C for 2 hours, and then use sulfuric acid with a concentration of 0.1mol / L. The solution was immersed for 1h, the liquid-solid ratio was 15mL / g during immersion, fi...

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Abstract

The invention relates to a method for preparing high-purity methyl silicone oil, belonging to the technical field of methyl silicone oil preparation. In the rowing kettle, after the rearrangement is completed, nitrogen is bubbled for cooling, filtered, and the filtrate is qualified DMC; the second step, the qualified DMC is placed in the polymerization kettle, and after the polymerization reaction is completed, the solid catalyst is recovered, and the high efficiency is removed. Purity methyl silicone oil, the present invention removes the impurities of DMC crude oil by adding refined preparation, uses solid catalyst to replace traditional acid-base catalyst, and obtains methyl silicone oil with volatile matter below 0.2%, ring body (D4, D5, D6) ) content is below 0.1%, the refractive index is below 1.35, the ROHS six-phase, potassium content, halogen content, and residual hydroxyl content are all relatively low, and have high purity.

Description

technical field [0001] The invention belongs to the technical field of methyl silicone oil preparation, and in particular relates to a preparation method of high-purity methyl silicone oil. Background technique [0002] Methyl silicone oil has the characteristics of excellent spreading performance, lubricity, high and low temperature resistance, weather resistance, radiation resistance, high flash point, low surface tension and physiological inertia. It is mainly used in daily chemical, mechanical, electrical, textile, coating , pharmaceutical and food industries. [0003] The method of using waste silicone rubber to produce and refine silicone oil has become a well-known technology in the industry. This method enables the waste to be effectively utilized again and is worthy of vigorous promotion. However, the purity of the silicone oil obtained by this method is relatively low. The main reason is that the waste silicone rubber undergoes catalytic cracking. There are impuri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/08C08G77/34
Inventor 钟裕强钟德志马小军刘来刘明光陆志飞魏文培龙小兰李耀满
Owner JIANGMEN SHENGPENG CHEM IND CO LTD
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