Method for preparing dibutyl dithiocarbamate by aid of high-gravity reactor

Abstract

The invention discloses a method for preparing dibutyl dithiocarbamate by the aid of a high-gravity reactor. The method includes preparing solution with a molar ratio of 1:0.5-2 from dibutylamine and alkali solution, adding the solution into a mixing tank A, preparing solution with a molar ratio of 1:0.1-1 from carbon disulfide and dichloromethane and adding the solution into a mixing tank B; allowing the temperature of the high-gravity reactor to range from 30 DEG C to 95 DEG C under the control, continuously pumping the solution in the tank A at the flow rate of 1-200 ml / min, simultaneously continuously pumping the solution in the tank B into a vaporizing tube at the speed of 1-200 ml / min, vaporizing the solution, then feeding the solution into the high-gravity reactor and carrying out gas-liquid counter-current reaction on the solution and the vaporized solution; condensing unreacted gas phases, feeding the unreacted gas phases into the tank B to be reused and allowing serous fluid with the dibutylamine and alkali to flow into the tank A to participate in cycling; pumping the serous fluid into a separator when the decreasing speed of the content of the dibutylamine in the tank A tends to be gentle, removing water phases, washing oil phases until the oil phases are neutral and then carrying out reduced pressure distillation under the condition of the vacuum degree ranging from -0.01 Mpa to -0.5 Mpa at the temperature of 50-90 DEG C to obtain the clear and transparent dibutyl dithiocarbamate.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and specifically relates to the preparation of dibutyl dibutylamine from a mixed gas formed of di-n-butylamine, carbon disulfide and dichloromethane under alkaline conditions by using a high-gravity reactor for gas-liquid countercurrent reaction. Thiocarbamate method. The method relates to a preparation method which can be used for anti-oxidation, extreme pressure and anti-wear lubricating oil additives. Background technique [0002] During use, the lubricating oil contacts with the oxygen in the air and the metal surface to undergo an oxidation reaction and deteriorate, which increases the viscosity of the oil, increases the acid value, generates sludge and precipitation, and causes corrosion and wear to the metal parts. Dibutyl dithiocarbamate is a phosphorus-free, ash-free, low-sulfur, anti-oxidation additive. When added to oil, it can slowly form a dense sulfide protective film wit...

AI Technical Summary

Problems solved by technology

[0005] The traditional kettle reaction needs to add additional solvent, and the yield is about 80%. The process is labor-intensive, high energy consumption, serious pollution, poor product quality, dark color, and is an obsolete process.

At present, the domestic product adopts the kettle-type two-step reaction method, which has various disadvantages, and needs to be improved by adopting more efficient, fast, high-quality, high-yield, low-energy-consumption, and less-polluting methods.

Images