Silicone oil and continuous preparation method thereof

Abstract

The invention relates to silicone oil and a continuous preparing method thereof. The continuous preparing method of the silicone oil comprises the following steps of dissolving hexamethylcyclotrisiloxane into dispersing agent to obtain mixed liquid; dehydrating the mixed liquid; adding an end-capping agent into the mixed liquid; heating the mixed liquid to 30 DEG C-80 DEG C and conducting a reaction to obtain a reactant; removing low-boiling-point substances in the reactant to obtain the silicone oil. When the mixed liquid is dehydrated, condensate is adopted to spray dehydrated spilth; when the low-boiling-point substances in the reactant are removed to obtain the silicone oil, the condensate is adopted to spray the removed low-boiling-point substances. By means of the continuous preparing method of the silicone oil, the danger is avoided that hexamethylcyclotrisiloxane is directly heated and molten into a liquid phase, which easily causes an explosion; the problems are solved that hexamethylcyclotrisiloxane is condensed in a condenser and a vacuum pipe, which causes that a reaction system is clogged, the product unit consumption and energy consumption are too high, and the yieldis lowered.

Description

technical field

[0001] The invention relates to the technical field of preparation of silicon-containing compounds, in particular to a silicone oil and a continuous preparation method thereof. Background technique

[0002] Silicone oil is one of the most common polysiloxane products on the market. It is a liquid linear polysiloxane with silicon-oxygen bonds (Si—O) as the main chain. Base silicone oil, part of the methyl group substituted by phenyl is phenyl silicone oil, and vinyl group is substituted by vinyl silicone oil. At present, the most commonly used method for producing silicone oil in industry is: cyclosiloxane and end-blocking agent are reacted under the action of acid catalyst or basic catalyst to prepare, and the cyclosiloxane used is octamethylcyclotetrasiloxane (D4) or Dimethylsiloxane mixed rings (DMC), usually go through a dehydration step before the polymerization reaction to remove the moisture in the cyclosiloxane, and after the polymerization reaction, ...

Examples

preparation example Construction

[0030] see figure 1 , the continuous preparation method of the silicone oil of one embodiment, comprises the following steps:

[0031] S110, dissolving hexamethylcyclotrisiloxane in a dispersant to obtain a mixed solution.

[0032] In one embodiment, the dispersant is at least one of octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane and dimethylsiloxane mixed rings.

[0033] In one embodiment, at least one of tetramethyltetravinylcyclotetrasiloxane, methylphenylcyclosiloxane and diphenylcyclosiloxane may also be added to the dispersant.

[0034] When tetramethyltetravinylcyclotetrasiloxane is added to the dispersant, the product obtained is vinyl silicone oil; when methylphenylcyclosiloxane and diphenylcyclosiloxane are added to the dispersant , the product obtained is phenyl silicone oil.

[0035] In one embodiment, the temperature of the dispersant is heated to 35° C. to 60° C., and then hexamethylcyclotrisiloxane is added therein, and stirred until the hexamethy...

Embodiment 1

[0095] Add 900Kg of dimethylsiloxane mixed rings into the dissolving device, heat to 65°C, then add 400Kg of hexamethylcyclotrisiloxane into the dissolving device and stir until completely dissolved to obtain a mixed solution. Import the above mixed solution into the dehydration equipment, heat it to 95°C, blow nitrogen into the dehydration equipment, and keep the vacuum at -0.09MPa for dehydration treatment for 1 hour. During the dehydration treatment, use a spray tower to dehydrate The overflow is treated by spraying, and the condensate recovered after spraying is introduced into the dissolution equipment for recycling. Add 65Kg of dehydrated hexamethyldisiloxane as an end-capping agent to the dehydrated mixed solution, heat it to 50°C and introduce it into the reaction equipment, and place excess macropores on the fluidized bed of the reaction equipment Cationic exchange resin, the mixed solution undergoes a fluidized bed catalytic reaction for 40 minutes to obtain the reac...

Embodiment 2

[0097] Add 900 Kg of octamethylcyclotetrasiloxane into the dissolving device, heat to 35° C., then add 9 Kg of hexamethylcyclotrisiloxane into the dissolving device and stir until completely dissolved to obtain a mixed solution. Import the above mixed solution into the dehydration equipment, heat it to 95°C, blow nitrogen into the dehydration equipment, and keep the vacuum at -0.08MPa for dehydration treatment for 1.5h. During the dehydration treatment, use a spray tower to dehydrate The treated overflow is sprayed, and the condensate recovered after spraying is introduced into the dissolution equipment for recycling. Add 300Kg of dehydrated tetramethyldivinyldisiloxane to the dehydrated mixed solution as an end-capping agent, heat it to 80°C and introduce it into the reaction equipment, and place an excess amount on the fluidized bed of the reaction equipment macroporous cation exchange resin, and the mixed solution was subjected to a fluidized bed catalytic reaction for 30 m...

technical field

[0001] The invention relates to the technical field of preparation of silicon-containing compounds, in particular to a silicone oil and a continuous preparation method thereof. Background technique

[0002] Silicone oil is one of the most common polysiloxane products on the market. It is a liquid linear polysiloxane with silicon-oxygen bonds (Si—O) as the main chain. Base silicone oil, part of the methyl group substituted by phenyl is phenyl silicone oil, and vinyl group is substituted by vinyl silicone oil. At present, the most commonly used method for producing silicone oil in industry is: cyclosiloxane and end-blocking agent are reacted under the action of acid catalyst or basic catalyst to prepare, and the cyclosiloxane used is octamethylcyclotetrasiloxane (D4) or Dimethylsiloxane mixed rings (DMC), usually go through a dehydration step before the polymerization reaction to remove the moisture in the cyclosiloxane, and after the polymerization reaction, ...

Examples

preparation example Construction

[0030] see figure 1 , the continuous preparation method of the silicone oil of one embodiment, comprises the following steps:

[0031] S110, dissolving hexamethylcyclotrisiloxane in a dispersant to obtain a mixed solution.

[0032] In one embodiment, the dispersant is at least one of octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane and dimethylsiloxane mixed rings.

[0033] In one embodiment, at least one of tetramethyltetravinylcyclotetrasiloxane, methylphenylcyclosiloxane and diphenylcyclosiloxane may also be added to the dispersant.

[0034] When tetramethyltetravinylcyclotetrasiloxane is added to the dispersant, the product obtained is vinyl silicone oil; when methylphenylcyclosiloxane and diphenylcyclosiloxane are added to the dispersant , the product obtained is phenyl silicone oil.

[0035] In one embodiment, the temperature of the dispersant is heated to 35° C. to 60° C., and then hexamethylcyclotrisiloxane is added therein, and stirred until the hexamethy...

Embodiment 1

[0095] Add 900Kg of dimethylsiloxane mixed rings into the dissolving device, heat to 65°C, then add 400Kg of hexamethylcyclotrisiloxane into the dissolving device and stir until completely dissolved to obtain a mixed solution. Import the above mixed solution into the dehydration equipment, heat it to 95°C, blow nitrogen into the dehydration equipment, and keep the vacuum at -0.09MPa for dehydration treatment for 1 hour. During the dehydration treatment, use a spray tower to dehydrate The overflow is treated by spraying, and the condensate recovered after spraying is introduced into the dissolution equipment for recycling. Add 65Kg of dehydrated hexamethyldisiloxane as an end-capping agent to the dehydrated mixed solution, heat it to 50°C and introduce it into the reaction equipment, and place excess macropores on the fluidized bed of the reaction equipment Cationic exchange resin, the mixed solution undergoes a fluidized bed catalytic reaction for 40 minutes to obtain the reac...

Embodiment 2

[0097] Add 900 Kg of octamethylcyclotetrasiloxane into the dissolving device, heat to 35° C., then add 9 Kg of hexamethylcyclotrisiloxane into the dissolving device and stir until completely dissolved to obtain a mixed solution. Import the above mixed solution into the dehydration equipment, heat it to 95°C, blow nitrogen into the dehydration equipment, and keep the vacuum at -0.08MPa for dehydration treatment for 1.5h. During the dehydration treatment, use a spray tower to dehydrate The treated overflow is sprayed, and the condensate recovered after spraying is introduced into the dissolution equipment for recycling. Add 300Kg of dehydrated tetramethyldivinyldisiloxane to the dehydrated mixed solution as an end-capping agent, heat it to 80°C and introduce it into the reaction equipment, and place an excess amount on the fluidized bed of the reaction equipment macroporous cation exchange resin, and the mixed solution was subjected to a fluidized bed catalytic reaction for 30 m...

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