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A modified monomer and organomodified polysiloxane prepared therefrom

A polysiloxane and organosilicon technology, which is applied in organic chemistry, silicon organic compounds, cosmetic preparations, etc., can solve the problems of unfavorable target product synthesis, many telomerization processes, and low degree of polymerization, etc., and achieve a wide range of products , Strong designability and simple process

Active Publication Date: 2016-03-02
广州星业科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One of its synthesis methods is the acid-catalyzed down-regulation polymerization of high hydrogen-containing silicone oil and cyclopolydimethylsiloxane mixture (DMC) or octamethylcyclotetrasiloxane (D4) into low-hydrogen silicone oil. There are many reaction steps, complicated operation, and the degree of polymerization is not high; the second synthesis method is to use hydrogen-containing double head, and / or) tetramethylcyclotetrasiloxane (D4H), and octamethylcyclotetrasiloxane (D4H), and octamethylcyclotetrasiloxane Siloxane (D4) synthesizes the target product. The synthesis process is the same as method 1. There are many processes, cumbersome operation, and the degree of polymerization is not high.
[0008] The quaternary ammonium base disclosed in U.S. Patent No. 7,605,284B2 is a catalyst, and it can also be an equilibrium catalyst for polydimethylsiloxane. Using this method to synthesize organically modified polydimethylsiloxane is easy to reduce the molecular weight due to the equilibrium reaction. Not conducive to the synthesis of the target product

Method used

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  • A modified monomer and organomodified polysiloxane prepared therefrom
  • A modified monomer and organomodified polysiloxane prepared therefrom
  • A modified monomer and organomodified polysiloxane prepared therefrom

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Take by weighing 162.3g stearyl alcohol and join into 500mL four-necked flask (the four-necked flask is equipped with thermometer, reflux device, stirring device and nitrogen (N 2 ) lead-in device, where the return device is interchangeable with the vacuum device as required), N 2 Add 0.15g of tetramethylammonium hydroxide pentahydrate under the atmosphere, turn on the vacuum pump, control the vacuum at -0.08MPa, slowly raise the temperature to 60°C and melt the material. After the melting is completed, stir and dehydrate for 1 hour. After the dehydration is completed, release the vacuum, N 2 Under the atmosphere, use a reflux device instead, raise the temperature to 65°C, and add 54.2g of tetramethyldihydrodisiloxane dropwise within 1 hour. After the addition, raise the temperature to 70°C, and react for 2 hours. After the reaction, the temperature was raised to 140° C. and kept for 1.5 hours to decompose the catalyst to obtain the modified monomer.

Embodiment 2

[0057] Take by weighing 145.47g palmitic alcohol and join into 500mL four-necked flask (the four-necked flask is equipped with thermometer, reflux device, stirring device and N 2 induction unit, where the return unit is interchangeable with the vacuum unit as required), N 2 Add 0.12g of tetramethylammonium hydroxide pentahydrate under the atmosphere, turn on the vacuum pump, control the vacuum at -0.095MPa, slowly raise the temperature to 55°C and melt the material. After the melting is completed, stir and dehydrate for 1.5h. After the dehydration is completed, release the vacuum, N 2 Under the atmosphere, use a reflux device instead, raise the temperature to 50°C, add 52.7g of tetramethyldihydrodisiloxane dropwise within 2h, and then raise the temperature to 80°C, and react for 1.5h. After the reaction, the temperature was raised to 150° C. and kept for 1 hour to decompose the catalyst to obtain the modified monomer.

Embodiment 3

[0059] Weigh 200g of polyether polyol (hydroxyl value 60mgKOH / g) into a 500mL four-necked flask (the four-necked flask is equipped with a thermometer, reflux device, stirring device and N 2 induction unit, where the return unit is interchangeable with the vacuum unit as required), N 2 Add 0.12g of tetramethylammonium hydroxide pentahydrate under the atmosphere, turn on the vacuum pump, control the vacuum at -0.09MPa, slowly raise the temperature to 50°C and melt the material. After the melting is completed, stir and dehydrate for 2 hours. After the dehydration is completed, release the vacuum, N 2 Under the atmosphere, use a reflux device instead, raise the temperature to 80°C, add 13.2g of 2,4,6,8-tetramethylcyclotetrasiloxane dropwise within 1 hour, and then raise the temperature to 100°C to react 1h. After the reaction, the temperature was raised to 160°C and kept for 0.5h to decompose the catalyst to obtain the modified monomer.

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Abstract

The invention belongs to the field of fine chemical engineering production technologies, and discloses a modified monomer and organic modified polysiloxane prepared thereby. Firstly, dehydrogenation reaction is carried out on a monomer containing Si-H bond and a compound containing hydroxyl (-OH) so as to synthesize a modified monomer, then in the presence of a catalyst and / or end-capping reagent, equilibration reaction is carried out on the modified monomer and common organosilicone monomer so as to synthesize the organic modified polysiloxane. The prepared organic modified polysiloxane can be used as cosmetic additive, lubricant additive and brake oil additive. The preparation method is simple, is easy to operate and control, and less erodes the equipment; the prepared organic modified polysiloxane is well compatible with organic compounds and / or water soluble compounds, and also can be used as a reaction intermediate for synthesizing high molecular materials continuously, thus having extensive use.

Description

technical field [0001] The invention belongs to the technical field of fine chemical production, and in particular relates to a modified monomer and organic modified polysiloxane prepared from the modified monomer. Background technique [0002] Polydimethylsiloxane has many special properties such as hydrophobicity, interface activity, and thermal stability, and is widely used in industrial production, such as polyurethane foam stabilizers, emulsifiers, defoamers, and mold release agents. However, polydimethylsiloxane is poorly soluble in organic solvents and water, thus limiting the application of polydimethylsiloxane. By organically modifying polydimethylsiloxane, introducing oil-soluble and / or water-soluble organic groups into polysiloxane chain ends, and / or both ends, and / or side ends, can effectively solve this problem. One problem makes polydimethylsiloxane more widely used. [0003] The organic functional group is connected to the polydimethylsiloxane molecular chai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/00C07F7/18C07F7/21C08G77/46C08G77/20C08G77/18A61K8/894A61K8/893C10M155/02
Inventor 谭意平孟巨光
Owner 广州星业科技股份有限公司
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