3-sulfoglutaramide type extraction agent and application thereof in extraction of gold
A technology of sulfur glutaramide and extraction agent, which is applied in the field of precious metal extraction, can solve the problems of acid resistance and long extraction equilibrium time, and achieve the effects of low cost, superior extraction performance, and simple synthesis method
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[0028] The preparation method of above-mentioned 3-thioglutaramide class extraction agent comprises the steps:
[0029] (1) Preparation of dimethyl 2,2'-thiodiglycolic acid: Dissolve 2,2'-thiodiglycolic acid in methanol to obtain a methanol solution of 2,2'-thiodiglycolic acid, 2,2'- The material molar ratio of thiodiglycolic acid to methanol is 1:(2~3), heated and kept at 5~100°C, stirred for 3~15h, placed and cooled to room temperature, removed methanol by rotary evaporation, and then vacuumed to remove residual methanol to obtain crude 2,2'-dimethyl thiodiglycolate;
[0030] (2) Preparation of 2,2'-3-thioglutaramide: Prepare the chloroform solution of amine and the chloroform solution of dimethyl thiodiglycolate crude product respectively, and then dimethyl thiodiglycolate The chloroform solution of the crude product is added dropwise to the chloroform solution of the amine, the molar ratio of dimethyl 2,2'-thiodiglycolate to the amine is 1:(2~3), at 20~100℃ After the dro...
Embodiment 1
[0034] Example 1 Preparation of N,N'-dimethyl-N,N'-diphenyl-3-thioglutaramide.
[0035] Add 2,2'-thiodiglycic acid into a three-necked flask and dissolve it in methanol; stir and react at 50°C for 5 hours; let it cool to room temperature, transfer the reaction solution into an eggplant-shaped flask, and remove excess methanol with a rotary evaporator. Then, the residual methanol was removed by vacuum suction to obtain dimethyl 2,2'-thiodiglycolic acid with a yield of 85%.
[0036] Add methylaniline into a three-necked flask with a constant pressure funnel and dissolve it with chloroform, and dissolve dimethyl 2,2'-thiodiglycolic acid with chloroform and transfer it to a constant pressure funnel; place the three-necked flask at 40 In a water bath at ℃, drop thiodiglycolyl chloride in chloroform at a rate of 1 drop per second. After completion of the dropwise addition, the reaction was stirred at 140° C. for 3 hours.
[0037] Cool the obtained reaction solution to room tempera...
Embodiment 2
[0049] Example 2 The test of the equilibration time of extractant extracting precious metal gold.
[0050] The reaction product prepared in Example 1 is dissolved in the chloroform system to form a chloroform solution with a concentration of 0.02mol / L of the extractant, and as an organic phase, prepare an aqueous solution of gold chloride so that the concentration of gold is 50mg / L, as the aqueous phase, the extraction test was carried out. Among them, the volume of the organic phase and the aqueous phase are each 5 mL in the Erlenmeyer flask and oscillated in the constant temperature oscillator in the water bath until the extraction equilibrium is reached. During the extraction process, the concentration of hydrochloric acid is controlled at 3 mol / L, the amplitude is 160 ± 2 spm, and the extraction temperature is controlled at 25 ± 0.5 °C, after shaking, transfer to a centrifuge tube for centrifugal phase separation, and the metal ion concentration of the aqueous phase after...
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