A kind of neutralizing agent for synthesizing polyfluorosiloxane and its preparation method and application

A technology of polyfluorosiloxane and trifluoropropylmethylcyclotrisiloxane, which can be used in chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, organic chemistry, etc., and can solve poor compatibility. , neutralize the problems of inhomogeneity and deterioration, and achieve the effect of consistent reactivity, low production cost and convenient process.

Active Publication Date: 2021-11-09
新元化学(山东)股份有限公司 +1
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the above neutralizing agents, α-chloroethanol, propionic acid, acetic acid, silicon-based phosphate, carbon dioxide, phosphoric acid, hydrochloric acid, trimethylchlorosilane, trimethylsilyl phosphate, etc. are compatible with polyfluorosiloxane poor sex
Although vinyl silyl phosphate has slightly better compatibility with polyfluorosiloxane, and has a better neutralization effect on polyfluorosiloxane oligomers, when the molecular weight of polyfluorosiloxane increases to gel, vinyl The neutralization effect of silicon-based phosphate ester will be significantly worse, and use vinyl silicon-based phosphate ester to neutralize, the vinyl group cannot be fully utilized, and the residual vinyl group will have an adverse effect on the vulcanization of high-temperature rubber. Phosphoric acid and D 3 The acid gel produced by the F reaction has good compatibility with high molecular weight polyfluorosiloxane, but after neutralization, it will cause hydroxyl end-blocking, which will cause degradation at high temperature and easily cause difficulty in mixing high molecular weight fluorosilicone polymers.
In addition, there are also literatures that use vinyl acyloxy polysiloxane for neutralization, but it is a mixture of materials with different molecular weights, and the activity of acetoxy groups is not completely the same, which is easy to cause uneven neutralization, and it is difficult to accurately measure it. Acetoxy content for neutralization
[0005] The existing technology cannot well solve the problems of rapid and accurate neutralization after the completion of the anionic polymerization reaction of high molecular weight polyfluorosiloxane and the absence of excess hydroxyl groups in the neutralized material.

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
  • A kind of neutralizing agent for synthesizing polyfluorosiloxane and its preparation method and application
  • A kind of neutralizing agent for synthesizing polyfluorosiloxane and its preparation method and application
  • A kind of neutralizing agent for synthesizing polyfluorosiloxane and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A kind of preparation method for the neutralizing agent of synthetic polyfluorosiloxane, comprises steps as follows:

[0034] (1) Add 370g of divinyltetramethyldisilazane to a reactor equipped with a stirring and dropping device, add 260g of acetic acid dropwise, maintain the reaction temperature in a water bath at 40-50°C, and add the dropwise time for 2 hours, After the dropwise addition, keep the system temperature at 40-50°C and continue to react for 1 hour, filter, and rectify the filtrate under atmospheric pressure under the protection of nitrogen. dimethylacetoxysilane;

[0035] (2) Add 216g vinyldimethylacetoxysilane and 468g D 3 F, cool down to 5-15°C, add 3g trifluoromethanesulfonic acid, react for 1.5h, add 2g sodium acetate to neutralize the catalyst after the reaction, stir for 0.5h, filter the reaction solution after returning to room temperature, and decompress the filtrate under 266Pa vacuum Rectify, according to the reflux ratio of 8:1, collect the fr...

Embodiment 2

[0039] A kind of preparation method for the neutralizing agent of synthetic polyfluorosiloxane, comprises steps as follows:

[0040] (1) Add 322g of hexamethyldisilazane to the reactor with a stirring and dropping device, add dropwise 250g of acetic acid, maintain the reaction temperature in a water bath at 40-50°C, add the time for 2 hours, and complete the dropping Afterwards, keep the system temperature at 40-50°C and continue to react for 1h, filter, and the filtrate is rectified under normal pressure under the protection of argon. Oxysilane;

[0041] (2) Add 198g trimethylacetoxysilane and 468g D 3 F, lower the temperature to 5-15°C, add 3g of trifluoromethanesulfonic acid, react for 2h, add 2g of sodium acetate to neutralize the catalyst after the reaction, stir for 0.5h, filter the reaction solution after returning to room temperature, and filter the filtrate under vacuum at 266Pa Distillation, according to the reflux ratio of 8:1 to collect the 92 ~ 95 ° C fraction, ...

Embodiment 3

[0044] A kind of preparation method for the neutralizing agent of synthetic polyfluorosiloxane, comprises steps as follows:

[0045] (1) Add 370g of divinyltetramethyldisilazane to a reactor equipped with a stirring and dropping device, add 245g of acetic acid dropwise, maintain the reaction temperature in a water bath at 40-50°C, and add the dropwise time for 1h, After the dropwise addition, keep the system temperature at 40-50°C and continue to react for 1 hour, filter, and rectify the filtrate under atmospheric pressure under the protection of nitrogen. Dimethylacetoxysilane;

[0046] (2) Add 375g vinyl dimethyl acetoxy silane and 468g D 3 F, lower the temperature to 5-15°C, add 2g trifluoromethanesulfonic acid, react for 1.5h, add 1.5g sodium acetate to neutralize the catalyst after the reaction, stir for 0.5h, filter the reaction solution after returning to room temperature, and reduce the filtrate under vacuum at 266Pa Pressure rectification, according to the reflux ra...

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
decomposition temperatureaaaaaaaaaa
Login to view more

Abstract

The invention relates to a neutralizing agent for synthesizing polyfluorosiloxane, a preparation method and application thereof. The preparation method comprises the steps of: (1) adding acetic acid dropwise to dihydrocarbyltetramethyldisilazane, filtering after reaction, and rectifying the filtrate under a protective gas to obtain hydrocarbyl dimethylacetoxysilane; (2) Hydrocarbyldimethylacetoxysilane and trifluoropropylmethylcyclotrisiloxane (D 3 F) Mix evenly, continue to add catalyst for reaction, add sodium acetate after the reaction, stir for 0.5 to 1 hour, filter, and rectify the filtrate under reduced pressure to obtain a neutralizing agent for synthesizing polyfluorosiloxane. Compared with the traditional neutralizing agent, the neutralizing agent used in the synthesis of polyfluorosiloxane provided by the invention has a purity of more than 99%, the neutralizing agent has the same reactivity, and the amount of the neutralizing agent can be accurately calculated and added. Compared with traditional neutralizers, the neutralization is more thorough, and the initial decomposition temperature of polyfluorosiloxane after neutralization can reach above 480°C.

Description

technical field [0001] The invention relates to a neutralizing agent for synthesizing polyfluorosiloxane, a preparation method and application thereof, and belongs to the field of organic silicon. Background technique [0002] The polymerization process of organopolysiloxane is generally divided into anionic polymerization and cationic polymerization. Among them, cationic polymerization requires the use of strong acid, and the post-neutralization and post-treatment process is complicated. Generally, only a few special organosilicon polymers use this process, and anionic polymerization catalysts are used. It is widely used in the preparation of polysiloxane, especially the preparation of high molecular weight polysiloxane. Anionic polymerization is used to prepare polysiloxane. After the polymerization reaction is completed, acidic substances are added to neutralize the basic catalyst, so as not to affect product quality or cause degradation of polysiloxane, especially fluoro...

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 Patents(China)
IPC IPC(8): C08G77/24C08G77/06C07F7/18
CPCC07F7/1896C08G77/06C08G77/24
Inventor 田志钢侯志伟邵军强夏金鹏林峰周建民解乐福
Owner 新元化学(山东)股份有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap