Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of dimethyl silicone oil with high conversion rate and low ring content

A technology of simethicone oil and high conversion rate, which is applied in the field of synthesis of simethicone oil with high conversion rate and low ring body content, and can solve the problems of low primary conversion rate, difficulty in removing a small amount of residual ring body, and wide molecular weight distribution. , to achieve the effects of simplifying the production process, promoting redistribution, and excellent product performance

Pending Publication Date: 2022-01-07
HUBEI XINGRUI SILICON MATERIAL CO LTD
View PDF4 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the technical difficulties in the prior art such as the low primary conversion rate of raw materials, the production of a large amount of volatile cyclosiloxane oligomers in the process of equilibrium reaction, the wide molecular weight distribution and the difficulty in removing a small amount of residual rings, the present invention provides a A method for synthesizing simethicone oil with high conversion rate and low ring body content, using high linear body siloxane hydrolyzate as raw material, linear phosphazene chloride as catalyst, and preparing low ring body content methyl silicone oil through polycondensation reaction of silanol group

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of dimethyl silicone oil with high conversion rate and low ring content
  • Preparation method of dimethyl silicone oil with high conversion rate and low ring content
  • Preparation method of dimethyl silicone oil with high conversion rate and low ring content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation method of linear phosphazene chloride catalyst

[0030] Add 20.5g of phosphorus pentachloride, 2.6g of ammonium chloride, and 100mL of tetrachloroethane into a 250ml three-necked flask, reflux at 150°C for 6 hours, cool to room temperature after the reaction, inject the reaction solution into 100ml of petroleum ether, and precipitate Precipitation. After the precipitation was washed with petroleum ether for many times, the residual petroleum ether was removed under reduced pressure to obtain a linear phosphazene chloride catalyst. The structural formula is as follows, and the nuclear magnetic spectrum is shown in the attached figure 1 .

[0031]

[0032] Linear phosphazene chloride structure.

Embodiment 2

[0034] Add 300g of highly linear siloxane hydrolyzate into a three-necked flask, stir and heat up to 70°C, add 40g of simethicone oil with a viscosity of 10cSt, stir well and add 0.7g of dimethicone with a content of 2wt% linear phosphazene chloride Methyl silicone oil solution. (2wt% means that the amount of linear phosphazene chloride in the catalyst solution is 2wt%, and the examples 3-12 all have the same meaning, only the addition amount is different) Under the negative pressure condition of 0.08Mpa lower than the atmospheric pressure, react for 3h, After the reaction, restore the system pressure to normal pressure, add 0.1 g of hexamethyldisilazane and stir for 0.5 h to neutralize the catalyst, raise the temperature to 200° C., cool down to obtain the finished product. The conversion rate is 98.21%, the viscosity is 14040cp, and the volatile matter is 0.21%.

Embodiment 3

[0036] Add 300g of highly linear siloxane hydrolyzate into a three-necked flask, stir and heat up to 70°C, add 41g of simethicone oil with a viscosity of 2cSt, stir well and add 0.84g of dimethicone with a content of 2wt% linear phosphazene chloride Methyl silicone oil solution, adjust the system pressure to 0.02Mpa lower than the atmospheric pressure and react for 2 hours. After the reaction, restore the system pressure to normal pressure, add 0.134g of hexamethyldisilazane and stir for 0.5h to neutralize the catalyst. Raise the temperature to 200°C to lower the temperature, cool and filter to obtain the finished product. The appearance of the finished product is transparent, the conversion rate is 98.46%, the viscosity is 88cSt, and the volatile matter is 0.14%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
volatile matteraaaaaaaaaa
volatile matteraaaaaaaaaa
volatile matteraaaaaaaaaa
Login to View More

Abstract

The invention relates to the technical field of polysiloxane synthesis, and provides a synthesis method of dimethyl silicone oil with high conversion rate and low ring content. The technical scheme is as follows: high-linearity siloxane hydrolysate is taken as a raw material, an end-capping reagent and a linear phosphonitrile chloride catalyst are added, reaction is performed for 1-4 hours at the temperature of 70-150 DEG C and under the negative pressure condition, hexamethyldisilazane is added to neutralize the catalyst after the reaction is finished, and low-temperature removal is conducted on the product to obtain the dimethyl silicone oil. The catalytic system is high in activity, the one-time conversion rate can reach 99% or above, the raw material utilization rate is extremely high, no obvious cyclosiloxane is generated in the reaction process, the low-temperature removal energy consumption is greatly reduced, and the final product is excellent in performance.

Description

technical field [0001] The invention relates to a method for synthesizing simethicone oil with high conversion rate and low ring body content, and belongs to the technical field of polysiloxane synthesis. Background technique [0002] Simethicone is a colorless, odorless, non-volatile transparent liquid with stable chemical properties, high boiling point, low freezing point, and a wide temperature range as a liquid. It has excellent heat resistance, weather resistance, physiological inertia, electrical insulation and small surface tension, and also has a low viscosity-temperature coefficient and high compression resistance. It is widely used in various sectors of the national economy such as machinery, electricity, textiles, coatings, and medicine. It is a class of polymers with a large scale of development and early industrialization. With the development of medical, food, electronic information and other industries, higher requirements are put forward for the performance ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/08
CPCC08G77/08
Inventor 李岩松孙刚李海娟陈泽雨肖靖
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com