Synthesis method of hydroxyl polysiloxane

A technology of hydroxypolysiloxane and synthesis method, which is applied in the field of synthesis of hydroxypolysiloxane, can solve problems such as complex process, many side reactions, and oil floating, and achieve reduction of side reactions, omission of protection steps, and cost reduction Effect

Pending Publication Date: 2021-06-18
SHENZHEN ANPIN SILICONE MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of synthesizing silicone-modified acrylate emulsion, due to the poor compatibility between PDMS and polyacrylate, phase separation easily occurs during synthesis and film formation, resulting in oil floating or coagulation. At the same time, the large-scale phase separation leads to low light transmittance of the coating film, which cannot well reflect the characteristics of silicone
[0004] Patent CN105801769B describes a method of introducing vinyl silicone oil through emulsion polymerization to improve the anti-graffiti performance of the surface. However, due to the low reactivity of the double bond of vinyl silicone oil, the emulsion polymerization method cannot obtain higher grafting efficiency. Stability is at risk
The modification of hydroxy silicone oil is an effective way to modify silicone, but the synthesis of hydroxy silicone oil has the disadvantages of complex process and many side reactions, which affect the application of this modification scheme

Method used

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  • Synthesis method of hydroxyl polysiloxane
  • Synthesis method of hydroxyl polysiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Add 300g of octamethylcyclotetrasiloxane to a 1L three-necked flask, add 5.4g of concentrated sulfuric acid and 600g of toluene and slowly raise the temperature to 75°C, react for 3 hours, add 45g of potassium trimethylsiliconate and 270g of THF and raise the temperature to 80°C for 10 hours , cooled to room temperature, 33g of dimethyl monochlorosilane was added dropwise under ice bath conditions, kept for 20 hours, filtered, and the filtrate was distilled under reduced pressure at 90°C to remove low boilers to obtain hydrogen-terminated silicone oil, and its number average molecular weight was tested It is 1000, and the hydrogen content is 0.10%.

Embodiment 2

[0045] Add 300g of octamethylcyclotetrasiloxane to a 1L three-necked flask, add 0.9g of trifluoromethanesulfonic acid and 90g of toluene and slowly raise the temperature to 75°C, add 15g of potassium trimethylsiliconate and 45g of THF and raise the temperature to 80°C after 3 hours of reaction React at ℃ for 10 hours, cool to room temperature, add 11g dimethyl monochlorosilane dropwise under ice bath conditions, keep warm for 20 hours, filter, and distill the filtrate under reduced pressure at 90℃ to remove low boilers to obtain hydrogen-terminated silicone oil. The number average molecular weight is 2700, and the hydrogen content is 0.037%.

Embodiment 3

[0047] Add 300g of octamethylcyclotetrasiloxane to a 1L three-necked flask, add 1.5g of concentrated sulfuric acid and 300g of toluene and slowly raise the temperature to 75°C, react for 3h, then add 25g of potassium trimethylsiliconate and 25gTHF and raise the temperature to 80°C for 10h , cooled to room temperature, 18.5g dimethyl monochlorosilane was added dropwise under ice bath conditions, kept for 20 hours, filtered, and the filtrate was distilled under reduced pressure at 90°C to remove low boilers to obtain hydrogen-terminated silicone oil. The molecular weight is 1700, and the hydrogen content is 0.059%.

[0048] The preparation example of hydroxyl polysiloxane is given below, wherein the viscosity is the dynamic viscosity value at 25°C, the test method refers to GB / T2794-1995, and the test method of hydroxyl content refers to GB / T 12008.3-2009; at the same time, the content of the reaction product is tested Hydrogen content, to investigate the reaction rate of silico...

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Abstract

The invention discloses a synthesis method of hydroxyl polysiloxane. According to the synthesis method, a compound with a (methyl)acrylate group reacts with polysiloxane with a silicon hydrogen group in the presence of a buffer solution. The synthesis method is used for preparing the hydroxyl-containing organopolysiloxane, is further used for modification synthesis and the like, and has the advantages of simple steps, few byproducts and low solvent dosage.

Description

technical field [0001] The invention relates to the field of organosilicon synthesis, in particular to a method for synthesizing hydroxypolysiloxane. [0002] technical background [0003] Organosilicon compounds have good properties of temperature resistance, hydrophobicity, weather resistance, aging resistance, and UV resistance. Whether they are used alone as materials or used for modification of other materials, their applications in the chemical industry are constantly being broadened, including organosilicon modification. Silicone modified polymer emulsion can endow it with excellent water resistance and temperature resistance after film formation, which can make up for the defects of polymer emulsion in application. For example, vinyl silicone oil has good weather resistance, aging resistance, UV resistance and flexibility, and can react with polyurethane, acrylic and other organic materials to prepare high-performance anti-corrosion and weather-resistant coatings. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/12
CPCC08G77/38C08G77/12
Inventor 彭派潜唐建振吴光飞游正林陈巧站宾家辉
Owner SHENZHEN ANPIN SILICONE MATERIAL
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