(1) Air oxidation method using kettle reactor condensation reaction. First the solid alkali aqueous solution at 15% in the kettle, and add carbon disulfide and dimethylamine (because of low boiling point, 40% water solution), stirring, a little heat, control temperature in 40 ~ 45 ℃, condensation reaction of 1 h above, to the material liquid PH up to 9 ~ 10, yellowish green or amber liquid, the condensation of dimethyl disulfide hydrogen generation of sodium formate. The sodium nitrite is prepared into 10% aqueous solution, and is added to the condensation product at room temperature and agitation, and then filtered to remove the slag, and the filtrate is transferred to the oxidation reactor. Oxidation reactor can be stirred tank type, from the jacket through the cooling medium cooling; Also available tower, tower body with jacket for heat exchange. The use of air bubble stirring, forming a good mass transfer. Sulfuric acid is slowly dropped into the oxidation reactor, the temperature is controlled at about 8℃, and at the same time through air, oxidation reaction, to generate accelerator TMTD. In the reaction, hydrogen monoxide is carried out with the air, which is yellow because it is oxidized to NO2 in the air. It should be absorbed, and then transferred to post-treatment after the oxidation reaction is completed. The generated tetramethylchulam disulfide was insoluble in water, and was separated out as a solid particle. The product was first absorbed and filtered, then washed with water, dried after dehydration, crushed and sieved, and the accelerant TMTD was obtained.
(2) chlorine - air oxidation method in the condensation reactor, the concentration of 40% dimethylamine solution and concentration of 15% sodium hydroxide aqueous solution, and the concentration of 98% carbon disulfide reaction at 40~45℃ for 1h, reaction terminal pH value between 9-10, the light yellow liquid is formic sodium. Flumex sodium is added to the top of the oxidation tower by pump metering, air is imported from the bottom of the oxidation tower through the rotor flowmeter, and chlorine gas is imported from each layer of the tower. Chlorine gas diluted by air moves in the opposite direction to the 50% formic sodium. The generated accelerator TMTD suspension was separated, washed, dried, crushed, screened and packed to get the finished product.
(3) Laboratory method: Add 52G 40% dimethylamine solution, 47G 15% NaOH solution and 73G 98% carbon disulphide into 100ml three-mouth flask with agitator, stir, control the temperature at 40~45℃ reaction for 1h. The pH value at the end point was between 9 and 10. 17g of chlorine gas (measured in cylinder weightlessness) is slowly introduced under agitation. The resulting accelerator TMTD was separated, washed and dried to obtain the finished product.
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