A kind of method and device for rectifying organosilicon ring mixture

An organosilicon ring and mixture technology, which is applied in the field of ring separation, can solve the problems of poor technical and economic benefits, low main content of D3 products, and influence on the quality of downstream products, so as to achieve easy control of the process flow and overcome serious high-temperature corrosion of equipment. , The effect of production conditions is not harsh

Active Publication Date: 2018-11-16
HUBEI XINGRUI SILICON MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing ring body distillation purification process, vacuum distillation is generally used. This method has low operating temperature, D3 is cut from the top of the tower, and the reflux flow is large. The main content of D3 products is low and there are many impurities.
Due to the poor separation effect, there are many impurities in the DMC product, and the quality is not up to standard, which has a certain impact on the quality of downstream products
The device system is complicated, the construction investment is large, the corrosion is serious during the operation of the equipment, and it is easy to block, which directly leads to obviously poor technical and economic benefits

Method used

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  • A kind of method and device for rectifying organosilicon ring mixture

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Distillation tower 1 (1a) and reboiler 1 (3a) are fed with heat conduction oil for heating. After the temperature at the top of the tower slowly reaches 137-139°C, reflux for 10 minutes, take a sample from the top of the tower to analyze the D3 content of 97%, and start the rectification tower (1a) Feed pump, adjust the feed rate to 10m³ / h, and preheat to 135°C through the preheater (6a). Open the valve of the top production pipeline, the production volume is 0.5m³ / h, open the regulating valve of the production pipeline in the tower kettle, the production volume is 9.5m³ / h, and the production volume in the tower kettle goes to the rectification tower three (1c), and the rectification tower three (1c ) The top temperature is controlled at 102°C, and the vacuum degree is -0.095MPa to obtain DMC product with D3 content of 0.8%. DMC chromatographic analysis shows that the total amount of impurity peaks that appear before D4 is 7ppm, and the total impurity content is 46ppm. ...

Embodiment 2

[0010] Distillation tower one (1a) and reboiler one (3a) are fed with heat conduction oil for heating. After the temperature at the top of the rectification tower slowly reaches 100-105°C, reflux for 10 minutes, take a sample at the top of the tower to analyze the MM content of 96%, and start the refining process. Distillation column one (1a) feed pump, adjust the feed rate to 15m³ / h, and preheat to 140°C through the preheater (6a). Open the valve of the top production pipeline, the production volume is 0.75m³ / h, open the regulating valve of the production pipeline in the tower kettle, the production volume is 14.25m³ / h, the production volume in the tower kettle goes to the rectification tower three (1c), and the rectification tower three (1c ) The top temperature is controlled at 99-103°C, the vacuum degree is -0.095MPa, the DMC product is extracted from the top, and the chromatographic analysis shows that the content of D3 is 5.0%, the total amount of impurity peaks that appe...

Embodiment 3

[0012] Reboiler 1 (3a) of rectification tower 1 (1a) is fed with heat conduction oil for heating. After the top temperature of rectification tower 1 (1a) rises slowly to 109-111°C, reflux for 10 minutes, take a sample at the top of the tower to analyze the MM content 60%, start the feed pump of the rectification tower, adjust the feed rate to 10m³ / h, and preheat to 140°C through the preheater (6a). Open the top production pipeline valve, the production volume is 0.3m³ / h, open the tower bottom production pipeline regulating valve, the production volume is 9.7m³ / h, the tower bottom production goes to the second rectification tower (1b), the second rectification tower (1b ) The top temperature of the tower is controlled at 83-85°C, the vacuum degree is -0.065MPa to obtain D3 product, the output is 0.4m³ / h, and the D3 content is 98.5%. , the top temperature of the rectification tower four (1d) is controlled at 87-89°C, the vacuum degree is -0.096, and the D4 product is extracted f...

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Abstract

The invention provides a distillation method and device for an organosilicon cyclic compound mixture. The method is characterized in that a cyclic compound mixture obtained through pyrolysis of organosilicon hydrolysate enters a distillation column I, a reboiler I is arranged in the distillation column I, the temperature in the distillation column I is controlled to be 170-220 DEG C through heating by a heat source in the reboiler I, a gas phase is condensed by an overhead condenser I, one part of the gas phase enters the column through self-refluxing to participate in mass and heat transfer, and the other part is taken as a product to be extracted; a liquid phase in the distillation column I is pumped into a distillation column II, a reboiler II is arranged in the distillation column II, the temperature in the distillation column II is controlled to be 120-145 DEG C through heating by a heat source in the reboiler II, a gas phase is condensed by an overhead condenser II, then one part of the gas phase enters the column through self-refluxing to participate in mass and heat transfer, the other part is taken as a product to be extracted, and distillation column residues are hydrolyzed. A closed loop of materials is formed, equipment types are strictly selected through selection of process routes and regulation of process parameters, and the method and the device are suitable for producing MM, D3, D4, D5 and DMC products of various specifications.

Description

technical field [0001] The invention relates to a method and a device for separating ring bodies in organic silicon production, belonging to the technical field of organic silicon production. Background technique [0002] Silicone rings are the main raw materials for the production of silicone downstream products (silicone oil, silicone rubber, silicone resin, silane coupling agent), and the rings mainly include DMC, D3, D4, and high rings. The organosilicon ring is obtained by hydrolyzing dimethyldichlorosilane and cleavage of the hydrolyzate. Since the downstream products of organic silicon have high requirements on the quality of the annulus and various specification requirements, it is necessary to further rectify and separate the annulus after cracking. In the existing purification process of ring body rectification, vacuum rectification is generally used. This method has low operating temperature, D3 is cut off at the top of the tower, and the reflux flow is large. Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/14
CPCB01D3/143
Inventor 高英张浩聂兴臻苗刚何云飞沈维云万培知
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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