DIPHENYLAMINE-4-SULFONIC ACID BARIUM SALT synthesis

Yield:-

Reaction Conditions:

Stage #1:diphenylamine with sulfuric acid at 160; for 1 h;Large scale;
Stage #2: with water at 125; for 0.333333 h;Large scale;
Stage #3: with barium hydroxideHeating;Large scale;Temperature;

Steps:

2 Example 2: A method for preparation of barium diphenylaminesulfonate
(1) In a 20L Erlenmeyer flask, 8 Kg of diphenylamine was added. Add 5-10L concentrated sulfuric acid. Heated to 160°C. 550 ml of water was distilled off in 1 hour under reduced pressure. Sampling samples. The degree of sulfonation was examined. If sulfonation is not complete, 200-300 ml of water was distilled off under reduced pressure; (2) After completion of sulfonation, 5L of water was added to carry out hydrolysis transposition reaction. After incubation at 125°C for 20 minutes, poured into 50-60Kg of water. Heated to boiling. 80 - 100 Kg of a 20 wt% barium hydroxide solution was added. Filter. Separate residue and filtrate, respectively. (3) The filter cake with 10L of water, heating and stirring 20min, suction filtration. The filtrate was combined with the pre-filtrate. Leaching in the 10L water leaching 20min, then suction filtration. The three filtrates were combined, Heated to 80-90°C. pH 6-7 was adjusted with 10 wt% sodium carbonate. While hot filter. The precipitate was removed. 8 Kg of solid barium chloride was added. Cooled to 5-10°C Filtration, precipitation with cold water. Washed twice, Cl- is removed, dried in a vacuum oven at 80-100°C.

References:

Tianjin Guangfu Technology Development Co., Ltd.;Zhao, Peng;Li, Qian CN105566177, 2016, A Location in patent:Paragraph 0022; 0023; 0024; 0025; 0026

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