3-thioglutaramide extractant and its application in palladium extraction

The technology of thioglutaramide and extraction agent is applied in the field of precious metal extraction, which can solve the problems of long extraction equilibrium time and acid insufficiency, and achieve the effects of superior extraction performance, low cost and good radiation stability.

Active Publication Date: 2016-06-08
SOUTHEAST UNIV
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  • Abstract
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Problems solved by technology

[0004] Purpose of the invention: In order to avoid the problems of acid resistance and long extraction equilibrium time when the two types of extractants of sulfides and sulfoxides are used to recover precious metals, the present invention provides 3-thioglutaramide extractants, which is a technology to be solved in the present invention The problem is to provide the preparation method and application of the above extractant

Method used

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  • 3-thioglutaramide extractant and its application in palladium extraction
  • 3-thioglutaramide extractant and its application in palladium extraction
  • 3-thioglutaramide extractant and its application in palladium extraction

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preparation example Construction

[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 temper...

Embodiment 2

[0049] Example 2 The test of the equilibration time of extractant extracting noble metal palladium.

[0050] The reaction product prepared in Example 1 is dissolved in the chloroform system, and the concentration of the extractant is formed as a chloroform solution of 0.02mol / L, and as the organic phase, the aqueous solution of palladium chloride is prepared so that the concentration of palladium 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 o...

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Abstract

The invention discloses a 3-sulfoglutaramide type extraction agent. The invention simultaneously provides a preparation method and application of the extraction agent. The preparation method comprises the following steps: firstly reacting methanol with thiodiacetic acid to obtain dimethyl thiodiacetate, and finally reacting corresponding amine with dimethyl thiodiacetate to obtain corresponding 3-sulfoglutaramide. The extraction efficiency of the extraction agent against a precious metal, namely palladium, is 98.16%-99.22%. The extraction agent can be simultaneously applied to a mixed solution containing palladium, platinum, copper, iron, zinc and other base metals for recovering palladium. The preparation method disclosed by the invention is simple and easy to operate, and the extraction agent has excellent extraction performance against palladium ions in a high-acid solution; and furthermore, the extraction agent is stable to a strong acid and good in radiation stability, the synthesis method is simple, and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of precious metal extraction, and in particular relates to a 3-thioglutaramide extractant and its application in extracting palladium. Background technique [0002] my country produces a large amount of electronic waste every year. With the upgrading of electronic products, the amount of electronic waste continues to increase. The unreasonable disposal of a large amount of electronic waste not only pollutes the environment, but also causes a huge waste of resources. The metal purity of some parts or components coated with palladium in electronic waste is very high. For example, the purity of some palladium components can reach 99.999%, so it is a general trend to recover precious metals from electronic waste. Precipitation and displacement methods are traditional processes for separating and recovering precious metals, which are tedious and consume a lot of energy. Solvent extraction is considered to be the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D11/00B01D11/04C22B3/34C22B11/00
CPCY02P10/20
Inventor 黄瑛武剑李泳华李尚华
Owner SOUTHEAST UNIV
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