Process for manufacturing 4,4'-methylene-bis-(dibutyl-dithiocarbamate)

• Main Authors: PETRO JOZSEF, FOSTNER JANOS, SZOBOSZLAY SZABOLCS, JOVER BELA, FEKETE IMRE, CSERGO KAROLY
• Format: Patent
• Language: English; Spanish
• Published: 01.08.1998
• Edition: 6
• Subjects: ACYCLIC OR CARBOCYCLIC COMPOUNDS; CHEMISTRY; FUELS; LUBRICANTS; LUBRICATING COMPOSITIONS; METALLURGY; ORGANIC CHEMISTRY; PEAT; PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATINGINGREDIENTS IN A LUBRICATING COMPOSITION

The subject-matter of the invention is a process for manufacturing 4,4'-methylene-bis-(dibutyl-dithiocarbamate) with ASTM colour less than 2, by reacting aqueous solutions of dibutyl amine and sodium hydroxide with carbon disulfide at a temperature below 42 DEG C, treating the obtained reaction product with methylene dichloride followed by vacuum stripping at a temperature below 122 DEG C and a pressure above 5 kPa, phase separation and filtration of the precipitated sodium chloride, characterized by keeping the temperature of the mixture during the reaction with carbon disulfide at or below 15 DEG C and performing the vacuum stripping in 2 steps, first at a temperature of from 45 DEG C to 100 DEG C and at a pressure of from 5 to 50 kPa, then carrying out the phase separation at 35 DEG C to 50 DEG C, and thereafter performing the second vacuum stripping of the separated organic phase also at a temperature of from 45 DEG C to 100 DEG C and at a pressure of from 5 to 50 kPa. PROCEDIMIENTO PERFECCIONADO PARA LA FABRICACION DE METILENO-BIS-(DIBUTIL-DITIOCARBAMATO) CON COLOR ASTM INFERIOR A 2. LA INVENCION SE REFIERE A LA FABRICACION MEJORADA DE METILENO-BIS-(DIBUTIL-DITIOCARBAMATO) CON COLOR ASTM INFERIOR A 2, MEDIANTE REACCION DE SOLUCIONES ACUOSAS DE DIBUTIL-AMINA E HIDROXIDO SODICO CON DISULFURO DE CARBONO, TRATAMIENTO DEL PRODUCTO DE REACCION OBTENIDO CON DICLORURO DE METILENO, SEGUIDO POR ESTABILIZACION AL VACIO, SEPARACION DE FASES Y FILTRADO DEL CLORURO SODICO PRECIPITADO. DURANTE LA REACCION CON DISULFURO DE CARBONO LA TEMPERATURA DE LA MEZCLA SE MANTIENE A 15C O MENOS Y LA ESTABILIZACION AL VACIO SE EFECTUA EN DOS PASOS, PRIMERO A TEMPERATURA ENTRE 45C Y 100C Y PRESION DE 5-50 KPA, DESPUES SE LLEVA A CABO LA SEPARACION DE FASES A TEMPERATURA ENTRE 35C Y 50C, Y A CONTINUACION SE EFECTUA UNA ESTABILIZACION AL VACIO DE LA FASE ORGANICA SEPARADA TAMBIEN A TEMPERATURA ENTRE 45C Y 100C Y A UNA PRESION DE 5-50 KPA.