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Method for preparing solvent-free high hydrogen containing silicone oil

A high-hydrogen-containing silicone oil and solvent-free technology, which is applied in the chemical industry, can solve the problems of high-hydrogen-containing silicone oil quality deterioration and achieve the effects of high hydrogen content, energy saving, and pollution reduction

Active Publication Date: 2012-10-31
TANGSHAN SANYOU SILICON IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing technology is mostly produced by the solvent method, and it is inevitable to leave residues when removing the solvent, which makes the quality of high hydrogen-containing silicone oil worse

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 1000kg of methyldichlorosilane and 15kg of trimethylchlorosilane into the reaction kettle and mix well. Control the flow rate of the inorganic salt hydrochloric acid solution, keep the temperature in the reactor not exceeding 45°C, and when the system no longer emits hydrogen chloride gas, separate layers, wash with water, dry with anhydrous sodium carbonate, and neutralize. The product is catalyzed and reacted with strong acidic cation exchange resin at 20-60°C for 1-6 hours, filtered, and low-molecular weight and impurities are removed under negative pressure to obtain high-hydrogen-containing silicone oil.

Embodiment 2

[0022] Add 500kg of methyldichlorosilane and 10kg of trimethylchlorosilane into the reaction kettle and mix well. Keep the temperature in the reactor at -5-45°C, control the flow rate, add 1 / 2 metered soft water, and then add inorganic salt hydrochloric acid solution at a certain flow rate until the reaction is completed. After drying and neutralizing the reactants, catalyze the reaction with acid clay for 1-6 hours at 20-60°C, filter, and remove low molecular weight and impurities under negative pressure to obtain high hydrogen-containing silicone oil.

Embodiment 3

[0024] Add 500kg of methyldichlorosilane and 6kg of trimethylchlorosilane to the reaction kettle, control the flow rate of the inorganic salt hydrochloric acid solution, keep the temperature in the reaction kettle not exceeding 45°C, and when the system no longer emits hydrogen chloride gas, separate layers to oxidize Calcium dry. Add sulfuric acid with a concentration of 70-98% as a catalyst, react at 20-60°C for 6 hours, neutralize the catalyst, remove low molecular weight and impurities, and obtain high hydrogen-containing silicone oil.

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PUM

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Abstract

The invention relates to a method for preparing solvent-free high hydrogen containing silicone oil, belonging to the field of chemical engineering and comprising the following steps of: adding methyl dichloresilane and methyl chlorosilane as raw materials in proportion in an agitated reactor, mixing uniformly; on the premise of stirring, adding excessive inorganic salt or hydrochloric acid or a mixed solution of inorganic salt or hydrochloric acid in the agitated reactor at a certain speed, controlling the temperature in the agitated reactor, keeping the temperature to be -5 DEG C-4 DEG C until the reaction is ended, standing and demixing, drying upper components with anhydrous sodium carbonate or sodium bicarbonate or calcium oxide and neutralizing remained acid; and aggregating the dried and neutralized upper components, and removing low-boiling-point substances to obtain the solvent-free high hydrogen containing silicone oil. The invention avoids using the solvent toluene when the high hydrogen containing silicone oil is synthesized by using chlorosilane monomers in the traditional process, saves the energy sources, lowers the pollution to the environment, and can obtain an excellent-quality product with transparent appearance, high hydrogen content and no solvent odor.

Description

technical field [0001] The invention relates to a method for preparing solvent-free high-hydrogen silicone oil, which belongs to the field of chemical industry. Background technique [0002] High hydrogen silicone oil has many unique properties, such as excellent thermal stability, chemical stability, water repellency and reactivity, etc. These unique properties make high-hydrogen silicone oils widely used in many fields, such as antifouling, oil repellent, and waterproof treatment agents for buildings; raw materials for preparing modified silicone oils, used for natural and synthetic fabrics, silk, and leather. Waterproofing agent and textile auxiliary agent for softening agent; waterproofing and anti-sticking agent for paper; waterproofing agent for glass fiber; crosslinking agent for liquid silicone rubber; anti-yellowing agent for high temperature rubber, etc. [0003] Methyldichlorosilane, the raw material of high hydrogen-containing silicone oil, is one of the by-prod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/12C08G77/06
Inventor 李献起赵洁李全昶
Owner TANGSHAN SANYOU SILICON IND