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A kind of preparation method of organosilicon polymer

A polymer and silicone technology, applied in the field of silicone polymer preparation, can solve problems such as difficulty in ultra-thinning, low separation coefficient, difficult control of polymerization reaction rate and molecular weight, etc., to achieve appropriate viscosity and molecular weight, and excellent coating performance Effect

Active Publication Date: 2021-11-16
广州从化兆舜新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Among them, polydimethylsiloxane (PDMS) is one of the most important organosilicon polymers. The silicon-oxygen bond on the main chain of PDMS and its easy rotation make the molecular chain of PDMS have a large free volume and are very flexible. Therefore, PDMS is often used to prepare membrane materials with elasticity and high gas permeability, such as gas separation membranes. However, the cohesive energy density between PDMS polymer chains is low, and the separation coefficient α is low, making it difficult to ultra-thin. In view of the above defects, the existing technology often modifies the main chain and side chain of PDMS to improve its film-forming performance.
[0004] A common method for modifying the molecular chain of PDMS, such as introducing long-chain alkanes as side groups, hydrogenating monoalkylsiloxane and long-chain terminal olefins under the action of a hydrogenation catalyst, introducing long chain, and then add catalyst and cyclosiloxane to carry out cationic or anionic polymerization. The hydrogenation catalyst used in the above method is mostly expensive noble metals such as platinum black. Moreover, in the subsequent polymerization step, if the reaction system uses cationic Polymerization, the polymerization reaction rate is fast, but the molecular weight is not easy to control, and the catalyst is not easy to remove. If anionic polymerization is used, although the catalyst is easy to remove, the reaction speed is slow

Method used

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  • A kind of preparation method of organosilicon polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Silicone Polymer 1 was prepared by the following steps:

[0048] Step (1), add 1 mol of water to 1 mol of methyl tributylketoxime silane, hydrolyze at 35 ° C for 4 hours, vacuumize the reaction system to a vacuum of 0.05Mpa, remove the butanone oxime produced by hydrolysis, and then add to the reaction Add 4mol of higher alcohol 1-octanol into the system, let it stand for 2 hours, then carry out the condensation reaction, the reaction temperature is 60°C, the reaction time is 15 hours, and the reaction system is vacuumed to a vacuum degree of 0.02Mpa for vacuum treatment to remove the remaining small molecules, resulting in condensation products;

[0049] Step (2), add 10mol octamethylcyclotetrasiloxane and catalyst tetramethylammonium hydroxide in the condensation product that obtains in step (1), make the concentration of catalyst in the reaction system be 100ppm, keep vacuum constant , stirred at 80°C for 30 hours to carry out the chain extension reaction, and the c...

Embodiment 2

[0052] Silicone polymer 2 was prepared by the following steps:

[0053] The only difference from Example 1 is that in step (1), methyl tributylketoxime silane is replaced by vinyl tributylketoxime silane, the amount of water added is 0.8mol, and the hydrolysis condition is a hydrolysis temperature of 45°C , The hydrolysis time is 2h, the higher alcohol is 1-hydroxyhexadecane, the condensation reaction temperature is 80°C, and the condensation reaction time is 6h.

[0054] Example 2 obtains silicone polymer 2.

Embodiment 3

[0056] Silicone polymer 3 was prepared by the following steps:

[0057] The only difference from Example 1 is that the addition of octamethylcyclotetrasiloxane in step (2) is 15 mol, the temperature of constant temperature stirring is 120 ° C, the time is 8 h, and the reaction reaches a viscosity of 48000 mPa·s chain extension products.

[0058] Example 3 yielded silicone polymer 3.

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Abstract

The invention relates to a method for preparing an organosilicon polymer. The preparation method comprises the following steps: (1) hydrolyzing the raw material butanone oxime silane, removing the butanone oxime produced by the hydrolysis, and then adding a higher alcohol therein for condensation reaction, Vacuum treatment to remove the remaining small molecules to obtain a condensation product; (2) add dialkylcyclosiloxane and a catalyst to the condensation product obtained in step (1), keep the vacuum constant, and stir at a constant temperature to carry out the chain extension reaction Obtaining a chain extension product with a viscosity of 500 to 50000mPa·s; (3) adding a chain terminator to the chain extension product obtained in step (2) to carry out a chain termination reaction, stirring at a constant temperature to carry out medium breaking treatment, and then vacuum treatment to obtain The organosilicon polymer, the organosilicon polymer coating film obtained by the present invention has excellent properties, suitable viscosity and molecular weight, and is suitable for preparing thin film materials for oxygen separation, and the selective permeability of oxygen in the air can reach 600 :1.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing an organosilicon polymer. Background technique [0002] Silicone polymer is the most researched compound except for organic polymers containing C, N, and O. Silicone rubber and its products are the most productive varieties of silicone polymers. Silicone rubber is composed of high molar mass linear polymers. After siloxane is vulcanized, it forms an elastomer with a network structure, which has excellent high and low temperature resistance, weather resistance, ozone resistance, arc resistance, electrical insulation, high air permeability and physiological inertness. Silicone rubber products have excellent With comprehensive performance and good economic benefits, it has been widely used in aviation, aerospace, electrical, electronic, electrical, chemical, instrumentation, automobile, machinery and other industries, as well as in various fields of medical ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/26B01D53/22B01D71/70
CPCB01D53/228B01D71/70B01D2256/12C08G77/26
Inventor 黄永军林旭锋刘金明胡国新陈寒
Owner 广州从化兆舜新材料有限公司