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A polymer and organosilicon technology, applied in the field of organosilicon polymer preparation, can solve the problems of difficult ultra-thinning, low separation coefficient, low cohesive energy density, etc. Effect
Active Publication Date: 2018-09-14
广州从化兆舜新材料有限公司
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[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
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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 preparation method of an organic silicon polymer. The preparation method comprises the following steps: (1) hydrolyzing a raw material, i.e., butanonoximsilane, and removingdiacetylmonoxime generated by hydrolyzing; then adding high-grade alcohol and carrying out condensation reaction; treating in vacuum to remove residual small molecules, so as to obtain a condensationproduct; (2) adding dialkyl cyclosiloxane and a catalyst into the condensation product obtained by step (1); keeping the vacuum degree unchanged; stirring at constant temperature and carrying out chain extension reaction to obtain a chain extension product with the viscosity of 500 to 50000mPa.s; (3) adding a chain terminating agent into the chain extension product obtained by step (2) and carrying out chain terminating reaction; stirring at constant temperature and carrying out catalyst crushing treatment; then carrying out vacuum treatment to obtain the organic silicon polymer. The organicsilicon polymer obtained by the invention has good film coating performance and suitable viscosity and molecular weight; the organic silicon polymer is suitable for preparing a thin film material foroxygen separation, and the selective transmittance of oxygen in the air can reach 600 to 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...
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