Method for producing high hydrogen-containing silicone oil by solvent-free hydrolysis of monomethyldichlorosilane

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 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 both at home and abroad. Its notable feature is that it has good waterproof effect, can cross-link at low temperature to form a film, and form a waterproof layer on the surface of the material, which is used for waterproof treatment of fabrics, glass, ceramics, paper, leather, metal, building materials and other industries. Especially in recent years, it has been widely used in the production of liquid silicone rubber and high-temperature rubber anti-yellowing agent. With the increasing development of liquid silicone rubber and high-temperature rubber, the demand for high-hydrogen sil...

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 the storage of silicone oil 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.