Method for producing silicone oil with high hydrogen content by methyldichlorosilae through solvent-free hydrolysis

Abstract

The invention relates to a method for producing silicone oil with high hydrogen content by methyldichlorosilae through solvent-free hydrolysis. The method is characterized by comprising the following steps: adding methyldichlorosilae, trimethylchlorosilane and an organosilicone protecting agent into a reaction kettle, starting stirring and introducing nitrogen gas; continuously feeding domestic water to the reaction kettle, starting a liquid ring compressor, exhausting generated hydrogen chloride away, feeding the hydrogen chloride to a high boiling point cracking device, controlling the temperature in the reaction to be -50 DEG C to 15 DEG C, controlling the temperature of the reaction kettle to be below 15 DEG C after the domestic water is completely fed, reacting for 1 hours, and discharging 21-25% hydrochloric acid at the lower layer after standing and layering; transferring hydrolysate on the upper layer to a deacidification kettle, adding an adsorbent, and stirring for 1 hour to deacidify; taking supernatant liquid and adding into a telomerization kettle, adding activated clay, controlling the temperature to 55-75 DEG C, reacting for 3-6 hours, and filtering to obtain a hydrogen-containing silicone oil; and distilling the hydrogen-containing silicone oil in a distillation kettle, controlling the vacuum degree to -0.09 to 0.01Mpa and the temperature to 115-130 DEG C, and removing low molecules to obtain the hydrogen-containing silicone oil finished-product.

Description

technical field [0001] The invention relates to the field of chemical industry, and relates to a method for producing high hydrogen-containing silicone oil by solvent-free hydrolysis of monomethyldichlorosilane. Background technique [0002] High hydrogen-containing silicone oil is one of the most important products in the silicone oil series. In recent years, it has become a very popular silicone product at home and abroad. Its remarkable feature is that it has good waterproof effect, and it can be cross-linked at low temperature to form a film to form a waterproof layer on the surface of the material. Especially in recent years, it has been widely used in the production of liquid silicone rubber and high-temperature glue anti-yellowing agent. With the increasing development of liquid silicone rubber and high-temperature glue, the demand for high-hydrogen silicone oil will increase. In order to prevent environmental pollution and improve product quality , to meet the needs...

AI Technical Summary

Problems solved by technology

[0006] 1) The hydrogen content is too low, less than 1.55%, and the application field is limited;

[0007] 2) The pollution is serious, using sulfuric acid as a catalyst, the acid water produced by washing after the reaction is a mixed acid water such as hydrochloric acid and sulfuric acid, which cannot be recovered, and a large amount of acid water is produced after washing times, causing environmental pollution and wasting water resources;

[0008] 3. In the current production process of solvent-free hydrogen-containing silicone oil, the hydrolyzate is mostly washed with water, salt water or neutralized with a weak base, and it is difficult to separate the oil and water after washing with water; washing with salt water will leave residual chlorine; neutralization with a weak base will destroy the H bond, resulting in silicone oil storage Hydrogen loss during the process affects stability

But in the end, the volatile content of silicone oil is only 1.5-2%, and the flash point (open cup method) is about 150°C. Continued dehydration will cause the silicone oil to lose hydrogen and return to acid, which restricts its high-level applications.