The traditional method is to drop the mixed solution of methyl hydrodichlorosilane and trimethyl chlorosilane into the reaction kettle containing solvent and water. After hydrolysis, the acid water is separated and concentrated sulfuric acid is added. After the reaction, the layer was layered, the upper layer was washed to neutral, the low boiling matter was removed, and the product was filtered and decolorized. The solvent is usually hydrocarbon or benzene derivatives, at present the solvent is mostly heptane and toluene. In the above methods, the acid water separated after the reaction is a mixed solution of sulfuric acid and hydrochloric acid, which has many impurities and cannot be recycled. Moreover, it wastes resources by washing for many times and pollutes the environment. Bafeng tang has improved the process by adopting the reverse water solution method, that is, water droplets are added to the reaction kettle containing monomer mixture solution. Since the solubility of HC1 in the organic solvent is far less than that of water, the acid remaining in the hydrolysate will be much less, which is convenient for washing. An-an zhou put forward a method of continuous production of silicone oil, methyl hydrogen dichlorosilane, trimethyl chlorosilane and water according to certain proportion from the bottom of the kettle into the reaction kettle, produce hydrogen chloride gas by absorption equipment processing, products through the layered stratification and gives the lower acid water into concentrated hydrochloric acid storage tank for recycling, the upper hydrolyzed material into alkaline neutralization tank and, neutralizing agent can choose sodium sulfate or sodium bicarbonate, and stratification in the layered device, after get neutral hydrolysis; The neutral hydrolyzed material was polymerized in the polymerization kettle with catalyst, the product was filtered and the low boiling matter was removed in the film evaporator, and the hydrogen-containing silicone oil was obtained. This method avoids the disadvantages of low efficiency and unstable product batch caused by indirect production, and can be controlled automatically, reducing labor cost. T.L indner et al., this paper introduces a improved continuous production process relative to per mole can be hydrolyzed chlorine, reaction monomer with up to 0.5 mol, water generated part of the hydrolysis product, produced by HC1 recycled, applied directly to other reaction processing part of hydrolysate and excess water, ceding the hydrochloric acid can be used as crust source of water, and will get the volatile hydrolysis of methyl hydrogen silicone ring body isolated; At last, the distillation liquid in the distillation stage was added to the equilibrium reactor for refining, and the equilibrium reaction was carried out under the action of strongly acidic ion exchange resin to obtain the low-volatile, straight-chain silicone oil containing hydrogen... In order to increase the yield, the cycloid formed in this process can be mixed with hydrochloric acid solution and quaternary ammonium salt and heated to transform it into linear products. Because the silicon hydrogen bond is more active, the hydrolysis rate is fast, easy to produce gel; Therefore, solvent is usually added to dilute organochlorosilane when it is hydrolyzed to reduce its reaction rate. However, solvent odor is difficult to remove in the product prepared by solvent method, and the product quality is poor, so it cannot be used as a high-end product.






Li xian-qi et al. reacted monomer mixture solution with hydrochloric acid mixture solution by solvent free method. The temperature was controlled at 5-45 ℃. After the reaction, the monomer mixture solution was layered, washed, dried and neutralized. The temperature is controlled at 20 ~ 60℃, the product is balanced with strong acidic cation exchange resin, filtered and distilled to obtain hydrogen-containing silicone oil with good appearance and no peculiar smell 12]. At present, some domestic manufacturers such as jilin changjie siliciology co., LTD., etc. adopt the solvent free method for batch production.






The molar mass distribution of products produced by co-hydrolysis shrinkage method is difficult to control the hydrolysis reaction, and hydroxyl groups will be formed on the main chain to some extent during the reaction process, resulting in crosslinking, thus causing changes in product properties, such as shortened shelf life, etc. However, due to the simple operation and mature technology of this method, most domestic manufacturers still produce all hydrogen-containing silicone oil by this method.