zinc;N,N-氨基二硫代二乙酯

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The sequence of addition of the zinc compound and carbon disulfide is changed to conform to the method of Example 1 of U.S. Pat. No. 6,534,675, and zinc diethyldithiocarbamate (ZDEC-C) is prepared. Add 73 grams of diethylamine to 150 grams of water with temperature controlled at 25° C., then add 900 grams of solution with 3.4% ammonium hydroxide and 1% carbon dioxide which prevents the premature precipitation of the zinc content. Further add 346 grams of zinc ammonia complex solution A as in Example 1 containing 9.56% zinc to the solution and 1.7 grams of emulsifier Tanemul 1203. Lower the solution temperature to 15° C., add 78.5 grams of carbon disulfide slowly into the mixture under heavy agitation over 1 hour while keeping the temperature at or below 20° C. Yellowish white precipitates appear with the addition, and vapor comes out from the mixture. Continue the agitation for 3 hours, then heat the solution gradually to 40° C. Boil the solution, continue agitation for another 2 hours, then vacuum filter the precipitates. The filtrate has a pH of 8.45, and is substantially free of zinc and ammonia. The filtration is finished in 5 minutes. Wash the solid at the filter with 500 ml of 80° C. distilled water four times. Then dry the precipitate at 110° C. for 2 hours to obtain 172 grams of zinc diethyldithiocarbamate with 0.1% moisture content. We call this sample ZDEC-C. 6,534,675, and zinc diethyldithiocarbamate (ZDEC-C) is prepared controlled at 25° C. the premature precipitation of the zinc content Lower the solution temperature to 15° C., add 78.5 grams of carbon disulfide slowly into the mixture under heavy agitation over 1 hour below 20° C Yellowish white precipitates appear with the addition, and vapor for 3 hours for another 2 hours vacuum filter the precipitates The filtration Wash the solid at the filter with 500 ml of 80° C. distilled water four times Then dry the precipitate at 110° C. for 2 hours

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The sequence of addition of the zinc compound and carbon disulfide is changed to conform to the method of Example 1 of U.S. Pat. No. 6,534,675, and zinc diethyldithiocarbamate (ZDEC-C) is prepared. Add 73 grams of diethylamine to 150 grams of water with temperature controlled at 25° C., then add 900 grams of solution with 3.4% ammonium hydroxide and 1% carbon dioxide which prevents the premature precipitation of the zinc content. Further add 346 grams of zinc ammonia complex solution A as in Example 1 containing 9.56% zinc to the solution and 1.7 grams of emulsifier Tanemul 1203. Lower the solution temperature to 15° C., add 78.5 grams of carbon disulfide slowly into the mixture under heavy agitation over 1 hour while keeping the temperature at or below 20° C. Yellowish white precipitates appear with the addition, and vapor comes out from the mixture. Continue the agitation for 3 hours, then heat the solution gradually to 40° C. Boil the solution, continue agitation for another 2 hours, then vacuum filter the precipitates. The filtrate has a pH of 8.45, and is substantially free of zinc and ammonia. The filtration is finished in 5 minutes. Wash the solid at the filter with 500 ml of 80° C. distilled water four times. Then dry the precipitate at 110° C. for 2 hours to obtain 172 grams of zinc diethyldithiocarbamate with 0.1% moisture content. We call this sample ZDEC-C. 6,534,675, and zinc diethyldithiocarbamate (ZDEC-C) is prepared controlled at 25° C. the premature precipitation of the zinc content Lower the solution temperature to 15° C., add 78.5 grams of carbon disulfide slowly into the mixture under heavy agitation over 1 hour below 20° C Yellowish white precipitates appear with the addition, and vapor for 3 hours for another 2 hours vacuum filter the precipitates The filtration Wash the solid at the filter with 500 ml of 80° C. distilled water four times Then dry the precipitate at 110° C. for 2 hours