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Method for synthesizing 1,1,1,3,5,5,5-heptamethyl trisiloxane by utilizing hydrogen containing silicone oil low-boiling-point substance

A technology of heptamethyltrisiloxane and hexamethyldisiloxane, which is applied in the field of organosilicon compound synthesis, can solve the problems of complex components of low boilers, high purification costs, and low product yields, reaching dangerous The effect of reduction and simple process

Active Publication Date: 2019-09-20
JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the complex composition of low boilers, the product yield is low during recycling, and impurities such as chlorinated alkanes, olefins, hydrocarbons, etc. will accumulate after a certain number of hydrolysis reactions and cannot be used. Boiler Utilization Efficiency
Another way is to sell it as liquid waste to professional companies for processing, and the corresponding professional companies may be used to extract effective components, such as D 4 H (Tetramethylcyclotetrasiloxane), but the purification cost is high

Method used

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  • Method for synthesizing 1,1,1,3,5,5,5-heptamethyl trisiloxane by utilizing hydrogen containing silicone oil low-boiling-point substance
  • Method for synthesizing 1,1,1,3,5,5,5-heptamethyl trisiloxane by utilizing hydrogen containing silicone oil low-boiling-point substance
  • Method for synthesizing 1,1,1,3,5,5,5-heptamethyl trisiloxane by utilizing hydrogen containing silicone oil low-boiling-point substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Feed hexamethyldisiloxane, hydrogen-containing silicone oil low boilers, and acid clay catalyst at a mass ratio of 10:1:0.05, the total amount of feed is 300g, and add them to the reactor equipped with mechanical stirring, thermometer and reflux condenser , heat up under stirring, control the temperature at 65°C for 8 hours, then cool down and filter to obtain a synthetic solution containing 1,1,1,3,5,5,5-heptamethyltrisiloxane, after analysis 1,1, The content of 1,3,5,5,5-heptamethyltrisiloxane was 21.5%. The synthesis liquid is rectified by atmospheric pressure, the top temperature is controlled at 99-101°C to steam out MM, and then the temperature is lowered to below 50°C, the vacuum pump is started (the pressure is -0.095MPa), and the transition is evaporated between 65-70°C Fraction, 58.05g of 1,1,1,3,5,5,5-heptamethyltrisiloxane product with a content greater than 99% was distilled at 76-79°C (accounting for 1,1,1, 90% of the total amount of 3,5,5,5-heptamethyltr...

Embodiment 2

[0049] Feed hexamethyldisiloxane, hydrogen-containing silicone oil low boilers, and acid clay catalyst at a mass ratio of 8:1:0.05, with a total amount of 300 g, and add them to a reactor equipped with mechanical stirring, a thermometer, and a reflux condenser , heat up under stirring, control the temperature at 65°C for 8 hours, then cool down and filter to obtain a synthetic solution containing 1,1,1,3,5,5,5-heptamethyltrisiloxane, after analysis 1,1, The content of 1,3,5,5,5-heptamethyltrisiloxane was 23.2%.

[0050] According to the method of Example 1, atmospheric distillation and vacuum distillation were performed on the synthesis liquid to obtain a 1,1,1,3,5,5,5-heptamethyltrisiloxane product with a content greater than 99%. The amount of 1,1,1,3,5,5,5-heptamethyltrisiloxane in the obtained transition fraction accounts for 1,1,1,3,5,5,5-heptamethyltrisiloxane in the synthetic liquid About 10% of the total amount of trisiloxane. The high-boiling mixture after vacuum di...

Embodiment 3

[0052] Feed hexamethyldisiloxane, hydrogen-containing silicone oil low boilers, and acid clay catalyst at a mass ratio of 6:1:0.05, with a total amount of 300 g, and add them to a reactor equipped with mechanical stirring, a thermometer, and a reflux condenser , heat up under stirring, control the temperature at 65°C for 8 hours, then cool down and filter to obtain a synthetic solution containing 1,1,1,3,5,5,5-heptamethyltrisiloxane, after analysis 1,1, The content of 1,3,5,5,5-heptamethyltrisiloxane was 26%.

[0053] According to the method of Example 1, atmospheric distillation and vacuum distillation were performed on the synthesis liquid to obtain a 1,1,1,3,5,5,5-heptamethyltrisiloxane product with a content greater than 99%. The amount of 1,1,1,3,5,5,5-heptamethyltrisiloxane in the obtained transition fraction accounts for 1,1,1,3,5,5,5-heptamethyltrisiloxane in the synthetic liquid About 10% of the total amount of trisiloxane. The high-boiling mixture after vacuum dist...

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Abstract

The invention provides a method for preparing 1,1,1,3,5,5,5-heptamethyl trisiloxane by utilizing a hydrogen containing silicone oil low-boiling-point substance and hexamethyl disiloxane in the presence of a catalyst. According to the method, the hydrogen containing silicone oil low-boiling-point substance is utilized, which belongs to waste utilization, so that the method is environmentally friendly and is low in comprehensive cost, and the problems in treatment, utilization and safety of a byproduct, i.e., the hydrogen containing silicone oil low-boiling-point substance of production of high-hydrogen-content silicone oil are effectively solved.

Description

technical field [0001] The invention belongs to the field of organosilicon compound synthesis, and in particular relates to a process for synthesizing organosilicon products by using production by-products and turning waste into treasure. Background technique [0002] Surfactants have been widely used in modern industrial and agricultural production due to their important role in interfacial interactions. Among non-ionic surfactants, trisiloxane surfactants have super-dispersion properties, which can quickly wet and expand aqueous solutions on low-energy surfaces such as polyethylene films and plant leaves, and are suitable for water-based paints and adhesives As an additive for products that must be completely wetted on the solid surface to function well, trisiloxane surfactants have become the focus of interfacial phenomenon research due to their extraordinary wetting ability, and have broad application prospects . 1,1,1,3,5,5,5-heptamethyltrisiloxane (MD H M) is an int...

Claims

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Application Information

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IPC IPC(8): C07F7/08C07F7/20
CPCC07F7/0896C07F7/20
Inventor 张磊
Owner JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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