Method for preparing methylphenylcyclosiloxane

A technology of methylphenylcyclosiloxane and polymethylphenylsiloxane, applied in the direction of silicon organic compounds and the like, can solve the problem that methylphenyldichlorosilane cannot be directly applied, restricts the application field, and is difficult to achieve high efficiency. Methylphenyldichlorosilane and other problems, to achieve the effect of low cost, expanding application field and wide application

Inactive Publication Date: 2008-02-20
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the boiling points of the two are similar, 205.0°C (101.3kPa) and 201.0°C (101.3kPa) respectively, it is difficult to efficiently obtain methylphenyldichlorosilane without phenyltrichlorosilane even if it is separated by rectification
The existence of phenyltrichlorosilane makes the methylphenyldichlorosilane produced by thermal condensation method unable to be directly applied to the production of methylphenyl silicone oil and methylphenyl silicone rubber, which greatly limits its application field.

Method used

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  • Method for preparing methylphenylcyclosiloxane

Examples

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Effect test

Embodiment 1

[0017] Example 1. In a 1000ml flask equipped with a vacuum distillation device, add 700 grams of 10% T P Add 0.7 g of lithium hydroxide to methylphenylpolysiloxane, raise the temperature to 250° C. under 10 mmHg, and distill off a small amount of water produced by the condensation of methylphenylpolysiloxane. Raise the temperature to 350°C, increase the vacuum to 2mmHg, and collect 592 grams of distillate at 250-290°C, which is methylphenylcyclosiloxane. The yield is 94.0% of theory.

Embodiment 2

[0018] Example 2. In a 1000ml flask equipped with a vacuum distillation device, add 700 grams of 15% T P Add 38.5 grams of potassium carbonate to methylphenylpolysiloxane, heat up to 250°C under 10mmHg, and distill off a small amount of water produced by the condensation of methylphenylpolysiloxane. Raise the temperature to 350°C, increase the vacuum to 2mmHg, and collect 470 grams of distillate at 250-290°C, which is methylphenylcyclosiloxane. Yield 79.0% of theory.

Embodiment 3

[0019] Example 3. In a 1000ml flask equipped with a vacuum distillation device, add 700 grams of 10% T P Add 60.0 g of sodium carbonate to methylphenylpolysiloxane, heat up to 200°C at 7mmHg, and distill off a small amount of water produced by the condensation of methylphenylpolysiloxane. Raise the temperature to 340°C, increase the vacuum to 2mmHg, and collect 535 grams of distillate at 250-290°C, which is methylphenylcyclosiloxane. The yield is 84.9% of theory.

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Abstract

The invention relates to a preparation method of methyl phyenyl cyclosiloxane, aiming at solving the technical problem that the invention provides the preparation method of the methyl phenyl polysiloxane containing SiPhO1.5, namely TP under catalysis of alkali through thermal cracking. The particular steps are that: 1) polymethylphenyl sioxane containing TP is mixed evenly with catalysts (lithium hydroxide, potassium carbonate or sodium carbonate), and catalyst dosage is 0.1 to 10 percent of the polymethylphenyl sioxane dosage; 2) a low-boiling material condensed by the polymethylphenyl sioxane containing TP is removed under the vacuum and heating-up temperature of 200 to 250 DEG C; 3) the polymethylphenyl sioxane containing TP is cracked under high vacuum and highly heating-up temperature of 300 to 350 DEG C, thereby obtaining the product by collecting 250 to 290 DEG C/2mmHg distillations.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a method for preparing methylphenylcyclosiloxane from polymethylphenylsiloxane containing trifunctional phenylsiloxane chain members. Background technique [0002] A series of methylphenyl silicone materials such as methylphenyl silicone oil and methylphenyl silicone rubber are widely used in aerospace due to their excellent high and low temperature resistance, radiation resistance, physiological inertness, and electrical properties. , electronic and electrical, transportation, medical and health, people's daily life, etc., has increasingly become an important new type of silicone polymer in the national economy. Methylphenyl cyclosiloxane is one of the necessary raw materials for the preparation of methylphenyl silicone materials. [0003] By thermal cracking without trifunctional phenylsiloxane chains (T P ) polymethylphenylsiloxane to prepare methylphenylcyclosi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21
Inventor 李美江蒋剑雄来国桥邱化玉吕素芳苏丽
Owner HANGZHOU NORMAL UNIVERSITY
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