Method for preparing high boiling silicone oil by using organic silicon high boiling substances

Abstract

The invention relates to a method for preparing high boiling silicone oil by using organic silicon high boiling substances, comprising hydrolyzation of alcohol and neutralization, wherein the organic silicon high boiling substances are hydrolyzed in the mixed liquid of alcohol and water and refluxed for 1-4 hours; nitrogen purging is carried out on the reactant, and then the reactant is added with hydrogen chloride dissolved in urea, zinc oxide and ammonium bicarbonate and in the system thereof. The invention integrally uses the organic silicon high boiling substances and lowers the chlorine content in silicon oil products, ensures the molecular weight and viscosity to be controllable and mass to be more stable; the usage of the neutralizing agent and latent solvent is reduced greatly, thus reducing the production cost; the process is simple and the industrial production is easy.

Description

technical field

[0001] The invention relates to a method for preparing silicone oil, in particular to a method for producing high-boiling silicone oil from organosilicon high boilers. Background technique

[0002] In recent years, with the rapid development of the organosilicon industry, the output of methyl chlorosilane monomer is increasing, which leads to the increasing output of by-product organosilicon high boilers. However, organosilicon high boilers cannot be made into useful organosiloxanes by simple methods due to their complex components, containing a large amount of silicon powder impurities, and easily releasing a large amount of corrosive hydrogen chloride gas when exposed to moisture. It has become a prominent problem encountered in the production of organic silicon monomers.

[0003] At present, domestic and foreign researches on the conversion and utilization of organosilicon high boilers are mainly focused on the methods of cracking to produce chlorosilane ...

Examples

Embodiment 1

[0028] Embodiment 1: A kind of method for preparing high boiling silicone oil with organosilicon high boiler, the steps are as follows:

[0029] Pump 100 parts of silicone high-boiler into the enamel kettle, start stirring at room temperature, add dropwise a mixed solution of 55 parts of ethanol and 3 parts of water to the silicone high-boiler, dropwise to half of the total amount of the mixed solution When the dropwise addition was completed, the temperature rose to 70° C., continued to heat up to 80° C. and refluxed for 2 hours, and then purged with nitrogen at 60° C. for 1 hour to obtain acidic silicone oil. The hydrogen chloride gas generated during the dropwise addition is sent to the spray tower through the fan for recovery.

[0030] At a constant temperature of 45°C, add 30 parts of urea from the hand hole of the reaction kettle, then add 3 parts of zinc oxide, and finally add 20 parts of ammonium bicarbonate for neutralization. Ammonium bicarbonate was added in 4 batc...

technical field

[0001] The invention relates to a method for preparing silicone oil, in particular to a method for producing high-boiling silicone oil from organosilicon high boilers. Background technique

[0002] In recent years, with the rapid development of the organosilicon industry, the output of methyl chlorosilane monomer is increasing, which leads to the increasing output of by-product organosilicon high boilers. However, organosilicon high boilers cannot be made into useful organosiloxanes by simple methods due to their complex components, containing a large amount of silicon powder impurities, and easily releasing a large amount of corrosive hydrogen chloride gas when exposed to moisture. It has become a prominent problem encountered in the production of organic silicon monomers.

[0003] At present, domestic and foreign researches on the conversion and utilization of organosilicon high boilers are mainly focused on the methods of cracking to produce chlorosilane ...

Examples

Embodiment 1

[0028] Embodiment 1: A kind of method for preparing high boiling silicone oil with organosilicon high boiler, the steps are as follows:

[0029] Pump 100 parts of silicone high-boiler into the enamel kettle, start stirring at room temperature, add dropwise a mixed solution of 55 parts of ethanol and 3 parts of water to the silicone high-boiler, dropwise to half of the total amount of the mixed solution When the dropwise addition was completed, the temperature rose to 70° C., continued to heat up to 80° C. and refluxed for 2 hours, and then purged with nitrogen at 60° C. for 1 hour to obtain acidic silicone oil. The hydrogen chloride gas generated during the dropwise addition is sent to the spray tower through the fan for recovery.

[0030] At a constant temperature of 45°C, add 30 parts of urea from the hand hole of the reaction kettle, then add 3 parts of zinc oxide, and finally add 20 parts of ammonium bicarbonate for neutralization. Ammonium bicarbonate was added in 4 batc...