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Di-n-butylamine is an organic synthesis of raw materials
Jan 10, 2018

Di-n-butylamine is an organic synthesis of raw materials for petroleum additives, rubber vulcanization accelerators, mineral flotation agents, corrosion inhibitors, emulsifiers, pesticides, polymerization inhibitor and dye production. For example, the pesticides can be used to synthesize carbosulfan, rubber vulcanization accelerator (BZ, TP), anti-aging agent (NBC), POP polymerization catalyst, anti-corrosion agent, and oil additive dibutyl dithiocarbamic acid Salt (molybdenum, lead, antimony, zinc) and other production.

(1) Butanol method: derived from the role of n-butanol and ammonia. In the presence of copper-nickel acid clay catalyst near hydrogen, the reaction temperature is 200 ℃. The reaction gas is condensed, and the crude product obtained from the separation contains 2% -4.82% of butylamine, 17% -26% of dibutylamine and 31% -61% of tributylamine, and can be obtained by rectification to obtain monobutylamine and dibutyl amine Amine and tributylamine three products. Adjust ammonia and n-butanol molar ratio, you can adjust the proportion of three products. The reaction equation is as follows:

nC4H9OH + NH3 + H2 → n-C4H9NH2 + (n-C4H9) 2NH + (n-C4H9) 3N

(2) Calcium cyanide (calcium cyanamide) process: The process is as follows: the n-butanol, ammonia and hydrogen are controlled by a flow meter, and the mixture is fed into a stainless steel reaction tower in proportion to lime nitrogen (calcium cyanamide) , The lime nitrogen suspended in ice water, slowly added to the cooled sodium hydroxide solution, the temperature was maintained below 25 ℃, stirring vigorously 1h, to give sodium cyanamide solution. To this solution was added bromobutane - ethanol solution, stirred at reflux 2.5h, then distillation, the residue was cooled suction filtration, the filter cake was washed with ethanol, the filtrate and lotion combined with benzene extraction, the extract was washed with no Calcium sulfate is dried, and the residue is distilled under reduced pressure after distillation to remove benzene, and the distillate is collected at 147-151 DEG C (4.66kPa) to obtain dibutylcyanamide. Water and concentrated sulfuric acid and dibutylcyanamide were successively added to the reactor, refluxed slowly for 6h, cooled, and poured into cooled sodium hydroxide solution along the wall of the reactor (flowing to the bottom of the reactor without being mixed with the reaction material) to make the free amine Separated; then heated to remove the amine and water together. To the distillate was added granular potassium hydroxide, and cooled with ice, amine layer separation, drying, distillation, collecting 157 ~ 160 ° C distillate products. Process is:

Ammonia, Butanol, Bromobutane, Mono-Butylamine, Di-n-butylamine, Tri-n-butylamine, Pesticide Butyrate, Rubber vulcanization accelerator (BZ, TP), Antioxidant ), POP polymerization catalysts, anti-corrosion agents, and oil additives dibutyl dithiocarbamate

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