Method and production system for continuous catalytic synthesis and separation of high-purity low-viscosity dimethyl silicone oil

A technology of dimethicone and dodecamethylpentasiloxane is applied in the field of continuous catalytic synthesis and separation of high-purity and low-viscosity dimethicone, and can solve the problems that the product cannot be used, the dimethicone is not separated, and the like, Achieve the effect of improving the level of automation control, the reaction is smooth, efficient and stable, and the raw materials are easily available

Active Publication Date: 2020-02-21
RUNHE ORGANICSILICONE NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method realizes continuous production, it does not separate simethicone, and the product cannot be applied in cosmetics

Method used

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  • Method and production system for continuous catalytic synthesis and separation of high-purity low-viscosity dimethyl silicone oil
  • Method and production system for continuous catalytic synthesis and separation of high-purity low-viscosity dimethyl silicone oil
  • Method and production system for continuous catalytic synthesis and separation of high-purity low-viscosity dimethyl silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Mix hexamethyldisiloxane (MM) and methylcyclosiloxane (DMC) uniformly at a mass ratio of 3:1, pump the mixture into a fixed-bed reactor, and control the reaction temperature at 40°C to a certain The flow rate passes through a fixed bed equipped with an acidic resin. When the mixture passes through the fixed bed, it is catalyzed and balanced under the action of the acidic resin. The reaction time is controlled by controlling the flow rate of the reactant. The reaction residence time is 10 hours, and octamethyltrisilicon is synthesized. A mixture of low-viscosity simethicone oils such as oxane, decamethyltetrasiloxane, dodecamethylpentasiloxane, and tetradecamethylhexasiloxane, accounting for 29.4%, 15.6%, and 7.3%, respectively %, 3.2%.

Embodiment 2

[0038] Mix hexamethyldisiloxane (MM) and methylcyclosiloxane (DMC) uniformly at a mass ratio of 1:3, pump the mixture into a fixed-bed reactor, and control the reaction temperature at 60°C to a certain The flow rate passes through a fixed bed equipped with an acidic resin. When the mixture passes through the fixed bed, it is catalyzed and balanced under the action of the acidic resin. The reaction time is controlled by controlling the flow rate of the reactant. The reaction residence time is 6 hours, and octamethyl trisilicon is synthesized. A mixture of low-viscosity simethicone oils such as oxane, decamethyltetrasiloxane, dodecamethylpentasiloxane, and tetradecamethylhexasiloxane, accounting for 12.8%, 13.1%, and 12.1%, respectively %, 10.8%.

[0039] Two, fractionation: the reaction mixture synthesized by embodiment 2 is pumped into the separation tower, and the separation step: the separation tower comprises a lowering tower, a first separating tower, a second separating t...

Embodiment 3

[0041] The tower pressure is 5-10KPa, the kettle temperature is 90-95°C, and the reflux ratio is 40L / h, so as to collect low-boilers such as hexamethyldisiloxane and octamethyltrisiloxane for reuse. pump into the first separation tower;

[0042] The pressure of the first separation tower is 5-10KPa, the kettle temperature is 110-115°C, and the reflux ratio is 30L / h. Hexasiloxane 99% are used as finished products, and the bottom part of the tower is pumped into the second separation tower;

[0043] The pressure of the second separation tower is 5-10KPa, the kettle temperature is 125-130°C, and the reflux ratio is 25L / h. Hexasiloxane 99% are used as finished products, and the bottom part of the tower is pumped into the de-elevation tower;

[0044] The pressure of the tower is 5-10KPa, the kettle temperature is 140-150°C, the reflux ratio is 20L / h, and the collection of decamethyltetrasiloxane 99%, the heavy components at the bottom of the tower are returned for reuse.

[0...

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Abstract

The invention relates to a production method of cosmetic silicone oil, and in particular, relates to a method and production system for continuous catalytic synthesis and separation of high-purity low-viscosity dimethyl silicone oil. The method comprises the following steps: 1) a synthesis step; and 2) a separation step. The separation step comprises the steps: (1) discharging light components hexamethyldisiloxane and octamethyltrisiloxane from the tower top of a light component removal tower, condensing, enabling the condensed liquid to automatically flow to a low-boiling-point receiving tankof the light component removal tower, and conveying to an external low-boiling-point substance storage tank; and pumping heavy components at the bottom of the light component removal tower to a firstseparation tower; (2) discharging a component decamethyltetrasiloxane from the tower top of the first separation tower, and pumping a heavy component at the tower bottom to a second separation tower;(3) discharging a component dodecylmethylpentasiloxane from the tower top of the second separation tower, and pumping a heavy component at the tower bottom to a heavy component removal tower; and (4)discharging tetradecylmethylhexasiloxane from the tower top of the heavy component removal tower, and discharging a heavy component from the tower bottom of the heavy component removal tower. According to the method, continuous operation is carried out, and high-purity decamethyltetrasiloxane, dodecylmethylpentasiloxane and tetradecylmethylhexasiloxane can be prepared by continuously separating amixture through a separation tower.

Description

technical field [0001] The invention relates to a production method of cosmetic silicone oil, in particular to a method and production system for continuous catalytic synthesis and separation of high-purity and low-viscosity dimethyl silicone oil. Background technique [0002] Octamethylcyclotetrasiloxane (decamethyltetrasiloxane) and dodecamethylcyclohexasiloxane (tetramethylhexasiloxane), which are widely used in cosmetics, have been confirmed to belong to PBT (persistent Potent, bioaccumulative and toxic) and vPvB (very persistent, very bioaccumulative) substances, decamethylcyclopentasiloxane (dodecamethylpentasiloxane) was confirmed to be a vPvB substance. On January 11, 2018, the European Commission (EU) Amendment No. 2018 / 35 formally revised Appendix XVII of (EC) No 1907 / 2006 (ie the REACH Regulation) - adding the 70th restricted substance. Content of Octamethylcyclotetrasiloxane (Decamethyltetrasiloxane) and Decamethylcyclopentasiloxane (Dodecamethylpentasiloxane) i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08G77/06C08G77/36C07F7/18
CPCC07F7/188C08G77/045
Inventor 许银根宋春燕易有彬李勉李童成彭艳
Owner RUNHE ORGANICSILICONE NEW MATERIAL
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