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A method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by utilizing low-boiling substance of hydrogen-containing silicone oil

A technology of heptamethyltrisiloxane and hexamethyldisiloxane, which is applied in the field of organosilicon compound synthesis, can solve the problems of high purification cost, complex components of low boilers, and low product yield, and achieve simple process , the effect of risk reduction

Active Publication Date: 2022-05-27
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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  • A method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by utilizing low-boiling substance of hydrogen-containing silicone oil
  • A method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by utilizing low-boiling substance of hydrogen-containing silicone oil
  • A method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by utilizing low-boiling substance of hydrogen-containing silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The hexamethyldisiloxane, hydrogen-containing silicone oil low-boiling matter, and acid clay catalyst are charged in a mass ratio of 10:1:0.05, and the total amount of charging is 300 g, and added to a reactor with mechanical stirring, a thermometer and a reflux condenser. , heat up with stirring, control the temperature to react at 65°C for 8h, then cool down and filter to obtain a synthesis solution containing 1,1,1,3,5,5,5-heptamethyltrisiloxane. After analysis of 1,1, The content of 1,3,5,5,5-heptamethyltrisiloxane was 21.5%. The synthetic solution is subjected to atmospheric distillation, the top temperature is controlled to be 99-101°C to steam out MM, then the temperature is lowered to below 50°C, the vacuum pump is started (pressure is -0.095MPa), and the transition is steamed between 65-70°C Distillate, 58.05g of 1,1,1,3,5,5,5-heptamethyltrisiloxane products with a content of more than 99% were distilled at 76-79°C (accounting for 1,1,1, 90% of the total amoun...

Embodiment 2

[0049] The hexamethyldisiloxane, the hydrogen-containing silicone oil low boiler, and the acid clay catalyst are charged in a mass ratio of 8:1:0.05, and the total amount of the charging is 300 g, and added to a reactor with a mechanical stirring, a thermometer and a reflux condenser. , heat up with stirring, control the temperature to react at 65°C for 8h, then cool down and filter to obtain a synthetic solution containing 1,1,1,3,5,5,5-heptamethyltrisiloxane. After analysis of 1,1, The content of 1,3,5,5,5-heptamethyltrisiloxane was 23.2%.

[0050] The synthetic liquid was subjected to atmospheric distillation and vacuum distillation according to the method of Example 1 to obtain a 1,1,1,3,5,5,5-heptamethyltrisiloxane product with a content of more 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 synthesis solution About 10% of the total amount of trisiloxanes. The high...

Embodiment 3

[0052] The hexamethyldisiloxane, the hydrogen-containing silicone oil low boiler, and the acid clay catalyst are charged in a mass ratio of 6:1:0.05, and the total amount of the charging is 300 g, and added to a reactor with a mechanical stirring, a thermometer and a reflux condenser. , heat up with stirring, control the temperature to react at 65°C for 8h, then cool down and filter to obtain a synthesis solution containing 1,1,1,3,5,5,5-heptamethyltrisiloxane. After analysis of 1,1, The content of 1,3,5,5,5-heptamethyltrisiloxane was 26%.

[0053] The synthetic liquid was subjected to atmospheric distillation and vacuum distillation according to the method of Example 1 to obtain a 1,1,1,3,5,5,5-heptamethyltrisiloxane product with a content of more 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 synthesis solution About 10% of the total amount of trisiloxanes. The high-b...

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Abstract

The invention provides a method for preparing 1,1,1,3,5,5,5-heptamethyltrisiloxane using hydrogen-containing silicone oil low boilers and hexamethyldisiloxane in the presence of a catalyst . The method utilizes hydrogen-containing silicone oil low boilers, belongs to waste utilization, is not only environmentally friendly but also has low overall cost, and effectively solves the problems of treatment, utilization and safety of hydrogen-containing silicone oil low boilers, a by-product in the production of high hydrogen-containing silicone oil.

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 utilizing 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 the non-ionic surfactants, trisiloxane surfactants have super dispersing properties, which can rapidly wet and expand the aqueous solution on low-energy surfaces such as polyethylene films and plant leaves, and are suitable for water-based paints and adhesives. Auxiliary for products that must be fully wetted on the solid surface to function well. Trisiloxane surfactants have become the focus of research on interfacial phenomena due to their extraordinary wetting ability, and have broad application prospects. . 1,1,1,3,5,5,5-heptamethyltrisiloxane (MD H M) is a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08C07F7/20
CPCC07F7/0896C07F7/20
Inventor 张磊
Owner JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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