Sulfide heavy metal trapping agent and preparation method thereof
A heavy metal trapping agent and sulfide technology, which is applied in the fields of mercaptan preparation, chemical instruments and methods, organic chemistry, etc., can solve the problems of low yield, long synthesis route, and low zinc removal rate, and achieve short settling time, Easy to operate, not easy to secondary pollution effect
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Embodiment 1
[0028] A kind of sulfide heavy metal trapping agent N,N'-bis(2-mercaptoethyl)-1,3-benzenedicarboxamide, its preparation method is as follows:
[0029] At -5°C, in a 150mL three-necked flask, dissolve mercaptoethylamine hydrochloride to isophthaloyl chloride at a molar ratio of 2.9, that is, 4.94g of mercaptoethylamine hydrochloride and 3.05g of isophthaloyl chloride are dissolved in 65mL of chloroform, Add 5mL triethylamine, and react under stirring for 5 hours to obtain the heavy metal chelating agent N,N'-bis(2-mercaptoethyl)-1,3-benzenedicarboxamide (NBMIPA for short), and the reaction yield is 78.6%.
[0030] Infrared IR and nuclear magnetic NMR characterization results are as follows:
[0031] IR(KBr disk, cm -1 ): 3281.28 s(V NH), 3066.99 m{V C-H(Ar)}, 2932.02 m{V C-H(methylene)}, 2533.41 w (V SH), 1629.86 ss (V CO), 1529.32 ss (δ NH), 1290.56 m (V C-N), 1081.27 m (V C-S), 689.45 m {out-of-plane expansion C-H(Ar)}.
[0032] 1 H NMR (CDCl 3 , 300 MHz) δ(ppm): 1.445 ...
Embodiment 2
[0035] A kind of sulfide heavy metal trapping agent N,N'-bis(2-mercaptoethyl)-1,3-benzenedicarboxamide, its preparation method is as follows:
[0036] At 5°C, in a 150mL three-necked flask, dissolve mercaptoethylamine hydrochloride to isophthaloyl chloride at a molar ratio of 2.7, that is, dissolve 4.60 g of mercaptoethylamine hydrochloride and 3.05 g of isophthaloyl chloride in 65 mL of chloroform, and add 5mL of triethylamine was reacted for 4 hours under stirring to obtain the heavy metal chelating agent N,N'-bis(2-mercaptoethyl)-1,3-benzenedicarboxamide (NBMIPA for short), and the reaction yield was 54.9 %.
[0037]
Embodiment 3
[0039] A kind of sulfide heavy metal trapping agent N,N'-bis(2-mercaptoethyl)-1,3-benzenedicarboxamide, its preparation method is as follows:
[0040] At 20°C, in a 150 mL three-necked flask, dissolve mercaptoethylamine hydrochloride to isophthaloyl dichloride in a molar ratio of 1:2.3, that is, 3.92 g mercaptoethylamine hydrochloride and 3.05 g isophthaloyl chloride are dissolved in 65 mL of chloroform , add 5mL triethylamine, and react under stirring for 3 hours to obtain heavy metal chelating agent N,N'-bis(2-mercaptoethyl)-1,3-benzenedicarboxamide (NBMIPA for short), and the reaction yield was 25.3%.
[0041]
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