Preparation method of diphenyl cyclosiloxane

A technology of diphenylcyclosiloxane and diphenyldimethoxysilane is applied in the field of preparation of organosilicon intermediates, and can solve the problems of high cost, difficulty, and Pn quality of diphenylsiloxane. , to achieve the effect of avoiding VOCs emission, small thermal effect and low energy consumption

Pending Publication Date: 2020-04-28
仙桃市格瑞化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] 2. Due to the different times, in the above-mentioned patents or articles, there is no mention of the persistent harmfulness of polychlorinated biphenyls (hereinafter referred to as "PCBs") introduced by various raw materials, but the world today is very concerned about PCBs. Represents extremely strict restrictions on persistent harmful pollutants (the EU RoHS recommended inspection items continue to increase)
[0015] 3. The cost of diphenylsilanediol that meets the requirements is high, and half of the synthesized Pn products are linear cold polymers, which are difficult to purify by recrystallization, so the yield of Pn is too low
[0017] 5. Special emphasis should be placed on the method mentioned in the Chinese expired patent CN1096467C, which has insurmountable shortcomings: 1. Since the invention uses a substance with a generally low boiling point as a solvent, in the production process with a slightly larger batch, there are obvious The magnification effect of the concentrated and violent exo...

Method used

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  • Preparation method of diphenyl cyclosiloxane
  • Preparation method of diphenyl cyclosiloxane
  • Preparation method of diphenyl cyclosiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Add 120g of diethylene glycol dimethyl ether, 14g of water, and 2g of tetramethylammonium hydroxide (TMAOH) aqueous solution to the bottle, wherein the concentration of tetramethylammonium hydroxide aqueous solution is 1mol / L, and the kettle liquid is preheated to 95~ At 100°C, there is a slight reflux state on the bottle wall. Raise the temperature of the glass rectification column to 60°C and keep it. Slowly add 120g of diphenyldimethoxysilane with the total amount of treated PCBs less than 0.5ppm and the total amount of phenyltrimethoxysilane less than 0.5ppm into the bottle, adjust the heating according to the temperature of the kettle liquid, and keep the temperature of the kettle liquid At 95-100°C. From the beginning of the dropwise addition, the kettle liquid began to become turbid in about 1 hour. After 2 hours of dropwise addition, the methanol distilled from the top of the column was collected from the receiving bottle. This methanol only contains part of th...

Embodiment 2

[0055] Embodiment 2: 1: (0.06~0.2): (0.001~0.002)

[0056] Add 120g of diethylene glycol diethyl ether, 8g of water, and 1.2g of tetramethylammonium hydroxide (TMAOH) aqueous solution to the bottle, wherein the concentration of tetramethylammonium hydroxide aqueous solution is 1mol / L, and preheat the kettle liquid to 98°C , There is a slight reflux state on the bottle wall. Similarly, raise the temperature of the glass rectification column to 60°C and keep it. Slowly add 130g of diphenyldimethoxysilane with the total amount of treated PCBs less than 0.5ppm and the total amount of phenyltrimethoxysilane less than 0.5ppm into the bottle, adjust the heating according to the temperature of the kettle liquid, and keep the temperature of the kettle liquid At 95-100°C. From the beginning of the dropwise addition, the kettle liquid began to become turbid in about 1 hour, and was added dropwise for 2 hours.

[0057] The remaining processing steps were the same as in Example 1, and t...

Embodiment 3

[0059] Add 120g of ethylene glycol diethyl ether, 20g of water, and 2.3g of tetramethylammonium hydroxide (TMAOH) aqueous solution to the bottle, wherein the concentration of tetramethylammonium hydroxide aqueous solution is 1mol / L, and the kettle liquid is preheated to 99°C. There is a slight reflux state on the bottle wall. Similarly, raise the temperature of the glass rectification column to 60°C and keep it. Slowly add 115g of diphenyldimethoxysilane with the total amount of treated PCBs less than 0.5ppm and the total amount of phenyltrimethoxysilane less than 0.5ppm into the bottle, adjust the heating according to the temperature of the kettle liquid, and keep the temperature of the kettle liquid At 95-100°C. From the beginning of the dropwise addition, the kettle liquid began to become turbid in about 1 hour, and was added dropwise for 2 hours.

[0060] The remaining processing steps were the same as in Example 1, and finally the powder was dried under reduced pressure...

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Abstract

The invention relates to a preparation method of diphenyl cyclosiloxane. In the method, high-purity diphenyl dimethoxysilane free of polychlorinated biphenyl and a small amount of water are adopted asraw materials, diether series compounds such as ethylene glycol diethyl ether and diethylene glycol dimethyl ether with normal-pressure boiling points higher than 100 DEG C are used as solvents, a trace amount of an organic alkali such as tetramethylammonium hydroxide is used as a catalyst, generated methanol is distilled off in a micro-boiling state in a reaction kettle with a rectifying column,and commercial diphenyl cyclosiloxane is obtained in one step. The generated powdery diphenyl cyclosiloxane is extremely easy to separate from the liquid, all solvents are completely recycled and used mechanically, the byproduct methanol can also be rectified and purified for application, and no wastewater is discharged in the whole process.

Description

technical field [0001] The invention relates to a method for preparing an organosilicon intermediate, in particular to a method for preparing a bisphenylcyclosiloxane with an environment-friendly process. [0002] Background of the invention [0003] Due to the structural characteristics of silicon and oxygen atoms, when the general organocyclosiloxane is formed, it is naturally formed by the interaction of silicon and oxygen elements to form cyclotrisiloxane, cyclotetrasiloxane, cyclopentasiloxane, and cyclohexasiloxane. Oxanes and complex isomeric states. For the siloxane with two phenyl groups connected to the silicon atom, this rule is also followed when forming the ring body - that is to say, its composition is composed of hexaphenylcyclotrisiloxane (hereinafter referred to as "P3" refers to), octaphenylcyclotetrasiloxane (hereinafter referred to as "P4"), decaphenylcyclopentasiloxane (hereinafter referred to as "P5"), and P4, P5 also has two structures of "boat type" ...

Claims

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Application Information

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IPC IPC(8): C07F7/21
CPCC07F7/21
Inventor 熊永春邓道元
Owner 仙桃市格瑞化学工业有限公司
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