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Method for producing hydroxyl-capped polymethylphenylsilixane

A technology of polymethylphenylsiloxane and methylphenylcyclosiloxane is applied in the field of preparation of hydroxyl-terminated polymethylphenylsiloxane, which can solve problems such as difficulty in controlling the degree of reaction, and achieve satisfactory results. The effect of reaction yield and product performance, easy control, and mild reaction conditions

Inactive Publication Date: 2009-09-16
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since water is an inorganic substance and polysiloxane is an organic phase, the two are immiscible, and the reaction is a heterogeneous reaction, so it is difficult to control the degree of reaction

Method used

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  • Method for producing hydroxyl-capped polymethylphenylsilixane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: In a 500ml three-necked reaction flask equipped with stirring, reflux condenser and thermometer, add 200g of hydroxyl-terminated polydimethylsiloxane (the degree of polymerization is 6, and the hydroxyl content is 7%), 50g of methyl Phenylcyclosiloxane (38% methylphenylcyclotrisiloxane, 47% methylphenylcyclotetrasiloxane, 15% methylphenylcyclopentasiloxane), 0.5 g of tetramethylammonium hydroxide siliconate (the content of tetramethylammonium hydroxide in the siliconate is 5%). The temperature was raised to 70°C with stirring and maintained for 30 minutes. Raise the temperature to 105°C and react for 6h. After the reaction, the temperature of the reaction system was raised to 170° C. and maintained for 1 hour to decompose tetramethylammonium hydroxide. Low boilers were removed at 180°C / 5mmHg for 1h. 237.5 g of transparent hydroxyl-terminated polymethylphenylsiloxane was obtained, the hydroxyl content was 5.2%, and the weight content of the methylphenylsilo...

Embodiment 2

[0033] Example 2: In a 500ml three-necked reaction flask equipped with stirring, reflux condenser and thermometer, add 200g of hydroxyl-terminated polydimethylsiloxane (the degree of polymerization is 20, and the hydroxyl content is 2%), 10g of methyl Phenylcyclotrisiloxane, 4.2 g tetramethylammonium hydroxide siliconate (5% tetramethylammonium hydroxide in siliconate). The temperature was raised to 70°C with stirring and maintained for 30 minutes. Raise the temperature to 105°C and react for 10h. After the reaction, the temperature of the reaction system was raised to 170° C. and maintained for 0.5 h to decompose tetramethylammonium hydroxide. Remove low boilers at 200°C / 10mmHg for 1h. 189 g of transparent hydroxyl-terminated polymethylphenylsiloxane was obtained, the hydroxyl content was 1.6%, and the weight content of the methylphenylsiloxane chain unit was 5.20%. The yield was 90.5%.

Embodiment 3

[0034] Embodiment three: in the 500ml three-neck reaction flask that is equipped with stirring, reflux condenser and thermometer, add 150g hydroxyl-terminated polydimethylsiloxane (polymerization degree is 13, and hydroxyl content is 3.4%), 150g methyl Phenylcyclotetrasiloxane, 3 g tetramethylammonium hydroxide siliconate (5% tetramethylammonium hydroxide in siliconate). The temperature was raised to 70°C with stirring and maintained for 30 minutes. Raise the temperature to 105°C and react for 3h. After the reaction, the temperature of the reaction system was raised to 170° C. and maintained for 1 hour to decompose tetramethylammonium hydroxide. Remove low boilers at 250°C / 8mmHg for 0.5h. 290 g of transparent hydroxyl-terminated polymethylphenylsiloxane was obtained, the hydroxyl content was 1.5%, and the weight content of the methylphenylsiloxane chain unit was 51.5%. Yield 96.7%.

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Abstract

The invention refers to the technical field of chemical industry, in particular to a preparation method of a hydroxyl-terminated polymethylphenylsiloxane. Using hydroxyl-terminated polydimethylsiloxane, methylphenyl cyclosiloxane and tetramethylammonium hydroxide as raw materials, selecting different ratios, and controlling a certain reaction time and temperature during the reaction process through polycondensation reaction , and the reaction is carried out in steps, and the hydroxyl-terminated polymethylphenylsiloxane can be prepared by selecting different temperatures and reaction times. Compared with the traditional base-catalyzed cyclosiloxane to prepare the hydroxyl-terminated polysiloxane, the method provided by the invention has the advantages of homogeneous reaction, mild reaction conditions and easy control. The product prepared according to the present invention has wide application in medical, construction and other industries.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of hydroxyl-terminated polymethylphenylsiloxane. Background technique [0002] Polysiloxane has excellent heat resistance, cold resistance, ozone resistance, good electrical properties, and physiological inertness. It has been widely used in aviation and aerospace, electrical and electronic, transportation, machinery, construction, medical and health fields, and has become an important One of the silicone polymer materials. As we all know, polydimethylsiloxane is the most important type of silicone material in the market, however, due to the introduction of phenyl groups, polymethylphenylsiloxane has great advantages in high and low temperature resistance, damping performance, and resistance to high and low temperatures. Radiation performance and compatibility with organic materials are superior to polydimethylsiloxane, so it has broader applicatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/14C08G77/06
Inventor 李美江蒋剑雄吕素芳邱化玉邓元
Owner HANGZHOU NORMAL UNIVERSITY