Preparation method of gamma-chloropropyl triethoxysilane coupling agent

Abstract

The invention belongs to the technical field of fine chemical product preparation and relates to a preparation method of a gamma-chloropropyl triethoxysilane coupling agent. The preparation method comprises the following steps: adding a systhesis raw material gamma-chloropropyl trichlorosilane in an overhead tank into a glass lining synthesis kettle through a rotor flow meter so as to carry out one-step synthesis between the synthesis raw material and ethanol, timely discharging a by-product HCl gas produced by the synthesis in vacuum through an exhaust pipeline to enter a hydrochloric acid recovery tank; carrying out secondary synthesis by pumping the one-step synthesis liquid into the bottom of a heater through pipe connection by the use of a matching pump by the utilization of pipeline liquid level difference; adding a synthesis raw material absolute ethyl alcohol in the overhead tank into an absolute ethyl alcohol evaporation container through the rotor flow meter so as to carry out vaporization and then entering a main tower; and carrying out separation of components by the utilization of boiling point gradients of different components while carrying out third synthesis. The preparation method has advantages of reliable principle, low production cost, high conversion rate, large capacity, low energy consumption and high main content, is environmentally friendly, and is suitable for large-scale production.

Description

Technical field: [0001] The invention belongs to the technical field of preparation of fine chemical products, and relates to a new process for continuously preparing γ-chloropropyltriethoxysilane coupling agent by a double-tower method, in particular to a γ-chloropropyltriethoxysilane coupling agent. The preparation method of the joint agent. Background technique: [0002] γ-Chloropropyltriethoxysilane coupling agent is the main raw material for preparing Si-69, Si-75, KH-550 and other silane coupling agents, and it can also be used as a rubber processing aid for Coupling inorganic fillers in various halogenated rubbers such as chloroprene rubber, chlorinated butyl rubber and chlorosulfonated polyethylene to improve various physical and mechanical properties, and can also synthesize organosilicon compounds containing quaternary ammonium salt cations for use as Anti-mold and anti-odor finishing agent has special sterilization, anti-odor, anti-static and surface activity, an...

AI Technical Summary

Problems solved by technology

At present, most γ-chloropropyltriethoxysilane coupling agents adopt batch synthesis technology. Since all synthesis stages of this technology are in one container, no temperature gradient can be formed, and components with different boiling points cannot be effectively separated, let alone continuous. Feeding and continuous product output can only be carried out in stages and steps with temperature changes and synthesis time changes. The reaction time of each batch is long, the production capacity is low, and the content of chloride ions before neutralization reaches more than 0.78%, requiring a large amount of neutralizers, which increases the production capacity. Neutralize the cost, and form a large amount of chloride salts at the same time, the slag is too much to filter slowly, and many products are left in the waste slag, resulting in large loss, low yield, high cost, poor working environment, and serious pollution. The emission policy does not comply with the national environmental protection regulations, and is not suitable for large-scale production; the one-tower continuous synthesis adopted by a few manufacturers, due to the untimely discharge of the reaction by-product HCl, small tower diameter, low height, low temperature, and the temperature gradient is not good Obviously, the component separation effect is poor, resulting in the disadvantages of low product conversion rate, low production capacity, low main content and high chloride ion content, and is not suitable for large-scale production