Electrochemical synthesis method of ultra-high-purity noble metal compound

Abstract

The invention discloses an electrochemical synthesis method of an ultra-high-purity precious metal compound, which comprises the following steps: dissolving precious metal powder in a high-purity acid solution system by adopting an electrochemical dissolution process in a clean environment to form an ionic precious metal, selectively removing impurities through acid-resistant chelating resin, and carrying out reduced pressure distillation and concentration to obtain the ultra-high-purity precious metal compound. In the process, introduction of other impurity ions is avoided, the efficiency is high, and industrial batch production is easy. The purity of the obtained precious metal compound can reach 99.999% or above, and the obtained precious metal compound can be used as a raw material in the fields of chips, electrons, catalysts and the like.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of noble metal compounds and electrochemical synthesis, and particularly relates to an electrochemical synthesis method of super-high-purity noble metal compounds. BACKGROUND

[0002] Super-high-purity noble metal chlorides (such as chloroauric acid, chloroplatinic acid, palladium chloride, ruthenium trichloride, rhodium trichloride, etc.) are indispensable key basic raw materials for modern high-tech industries, and the purity thereof directly determines the performance and reliability of downstream products. These compounds are widely used in: (1) semiconductor industry: as precursors for chemical vapor deposition (CVD) and atomic layer deposition (ALD), used for preparing noble metal thin film electrodes, barrier layers, etc., and the purity is usually higher than 99.999% (5N), and the content of specific impurity elements needs to be controlled at the ppb (parts per billion) level. (2) High-end catalysis: as active precursors for homogeneous catalysis (such as cross-coupling reaction) and heterogeneous catalysis (such as automobile exhaust purification catalyst), impurities will poison the catalytic active center, resulting in catalyst deactivation. (3) Biological medicine and electronic plating: used for synthesizing anticancer drugs (such as cisplatin), preparing conductive paste and noble metal plating of precision electronic components, and any harmful impurities will seriously affect the safety and electrical performance of the products.

[0003] Currently, the traditional methods for preparing noble metal chlorides in industry and laboratories mainly include aqua regia dissolution method and direct chlorination method, but these methods have obvious limitations when pursuing ultra-high purity (≥5N): (1) aqua regia dissolution method: this method is to dissolve high-purity noble metal raw materials in aqua regia (a mixture of concentrated nitric acid and concentrated hydrochloric acid), and then evaporate and dissolve repeatedly to remove nitrate ions, and finally crystallize to obtain the target chloride. However, it is difficult to completely remove nitrate ions in this method, even after multiple evaporation and repeated hydrochloric acid leaching, trace amounts of nitrate ions may still remain in the product. Nitrate is a very strong non-metallic impurity, which can seriously damage the film quality in semiconductor precursor applications, and its detection and removal are extremely difficult. Moreover, aqua regia has strong corrosive properties, which may dissolve metal impurities such as silicon, sodium, and calcium from the reactor vessels (such as glass and quartz), causing secondary pollution. In addition, this method has a long process flow, complex operation, time-consuming and energy-consuming evaporation, and increases the risk of environmental pollution during production. (2) Direct chlorination method: this method is to directly chlorinate noble metal powder under the atmosphere of chlorine or hydrogen chloride gas to generate the corresponding chloride. The defects of this method are: for some noble metals (such as iridium and ruthenium), direct chlorination often has a slow reaction rate, and it is easy to generate a mixture of chlorides with different valence states, resulting in unstable product composition and low purity; this method cannot purify impurities in the raw metal, if the initial metal raw material contains other refractory metal impurities, they will remain in the final product in the form of chlorides or unreacted; the operation involves high temperature and toxic chlorine gas, which requires strict gas tightness and corrosion resistance of the equipment, increasing the cost and safety risk of the equipment.

[0004] In addition, in order to purify noble metal chlorides in the prior art, methods such as recrystallization or solvent extraction are often used. However, the recrystallization method has limited separation effect on impurities with similar chemical properties, low efficiency, and the solvent itself may also introduce organic impurities; the solvent extraction method has a complex process flow, is prone to emulsification and solvent residue problems, and is difficult to meet the requirements of electronic-grade ultra-high purity.

[0005] In summary, the existing methods for preparing noble metal chlorides have the problems of long process flow, easy introduction of specific impurities (such as nitrate, alkali metal, alkaline earth metal, etc.) that are difficult to remove, poor batch stability of the product, and difficulty in stably obtaining ≥5N ultra-high purity products. Therefore, there is an urgent need in the art to develop a new method for preparing ultra-high purity noble metal chlorides with simple process flow, strong controllability, high purification efficiency, and stable production of ultra-high purity noble metal chlorides. SUMMARY

[0006] The purpose of the present application is to provide an electrochemical synthesis method for ultra-high purity noble metal compounds, which does not involve the introduction of impurity metal ions, and has high efficiency and is easy to be industrialized for batch production.

[0007] In order to achieve the above purpose, the electrochemical synthesis method of the ultra-high purity noble metal compound provided by the application comprises the following steps: Step 1: passing an acid solution through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 1.0-10.0 mol / L; adding the acid aqueous solution into an electrolytic tank with stirring function, adding noble metal powder into the electrolytic tank, installing corresponding noble metal electrode sheets at the positive and negative electrodes of the electrolytic tank, connecting electrode wires, starting stirring and connecting power supply, and performing electrolysis at a redox electrode potential, so that the noble metal powder starts to dissolve, the solution gradually changes color from colorless to colored, and the noble metal powder is completely dissolved. The acid solution is any one of hydrochloric acid, sulfuric acid and acetic acid.

[0008] Step 2: passing the solution in the electrolytic tank after electrolysis in step 1 through an acid-resistant resin column to remove metal impurities, and then performing vacuum distillation to concentrate the solution to precipitate solids, so that the obtained solids are the ultra-high purity noble metal compound crystals, and the purity of the obtained solids is more than 99.995% after sampling ICP-MS analysis and detection.

[0009] The above steps are all operated in a clean environment. The clean environment is provided by a glove box, and the glove box is internally ventilated with air filtered by a fresh air filtering system.

[0010] Further, in step 1, the acid solution is preferably passed through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 1.0-10.0 mol / L; the acid aqueous solution is added into an electrolytic tank with stirring function, palladium powder is added into the electrolytic tank, palladium electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started and power supply is connected, and electrolysis is performed at a voltage of 3.5-18.0 V and a current of 1.0-10.0 A until the palladium powder is completely dissolved.

[0011] Further, in step 1, the acid solution is passed through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 2.0-10.0 mol / L; the acid aqueous solution is added into an electrolytic tank with stirring function, rhodium powder is added into the electrolytic tank, rhodium electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started and power supply is connected, and electrolysis is performed at a voltage of 6.0-24.0 V and a current of 5.0-10.0 A until the rhodium powder is completely dissolved.

[0012] Further, in step 1, the acid solution is preferably passed through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 3.0-8.0 mol / L; the acid aqueous solution is added into an electrolytic tank with stirring function, platinum powder is added into the electrolytic tank, platinum electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started and power supply is connected, and electrolysis is performed at a voltage of 3.0-15.0 V and a current of 2.0-8.0 A until the platinum powder is completely dissolved.

[0013] Further, in the step 1, the acid solution is preferably passed through an acid-resistant resin column to obtain a 6.0-10.0 mol / L acid aqueous solution; the acid aqueous solution is added to an electrolytic tank with stirring function, and iridium powder is added to the electrolytic tank; iridium electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started, and power is turned on; electrolysis is carried out at a voltage of 5.0-20.0 V and a current of 4.0-10.0 A until the iridium powder is completely dissolved.

[0014] Further, in the step 1, the acid solution is preferably passed through an acid-resistant resin column to obtain a 3.0-10.0 mol / L acid aqueous solution; the acid aqueous solution is added to an electrolytic tank with stirring function, and ruthenium powder is added to the electrolytic tank; ruthenium electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started, and power is turned on; electrolysis is carried out at a voltage of 6.0-24.0 V and a current of 3.0-9.0 A until the ruthenium powder is completely dissolved.

[0015] Further, in the step 1, the acid solution is preferably passed through an acid-resistant resin column to obtain a 1.0-10.0 mol / L acid aqueous solution; the acid aqueous solution is added to an electrolytic tank with stirring function, and gold powder is added to the electrolytic tank; gold electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started, and power is turned on; electrolysis is carried out at a voltage of 3.0-7.5 V and a current of 2.0-6.0 A until the gold powder is completely dissolved.

[0016] Further, the acid-resistant resin in the step 1 is selected from any one of a chelating resin (such as Seplite® LSC series chelating resin of Lanxiao Technology) and a complex adsorption resin (such as Seplite® LX series complex adsorption resin of Lanxiao Technology).

[0017] Further, in the step 1, the purity of the noble metal powder is preferably greater than 99.95%, and the particle size is 150-800 mesh, accounting for ≥95%.

[0018] The beneficial effects of the present application are as follows: The present application utilizes the specific redox electrode potential principle of noble metals, and uses an electrochemical dissolution process in a clean environment to dissolve noble metal powder in a high-purity acid solution system to form ionic noble metal. After selective impurity removal by acid-resistant chelating resin, vacuum distillation and concentration are performed to obtain ultra-high purity noble metal compounds. This process does not involve the introduction of other impurity metal ions, realizes efficient dissolution of platinum group metals and gold, has high efficiency, and is easy to industrialize for batch production. The purity of the obtained noble metal compounds can reach more than 99.999%, which can be used as raw materials in the fields of chips, electronics, catalysts, etc. DETAILED DESCRIPTION

[0019] The application will be further described in detail in connection with the following examples, but the scope of protection of the application is not limited to these examples.

[0020] In the following examples, the LSD396 complex adsorption resin, LX-935 complex adsorption resin, LSC-495 chelate resin, LSC800 chelate resin, LSC-600 chelate resin used are provided by Lanxiao Technology. Example 1

[0021] Step 1: The concentrated hydrochloric acid with a mass concentration of 36% is passed through the LSD396 complex adsorption resin column, then deionized water is added for dilution to obtain a 5.5 mol / L hydrochloric acid aqueous solution; the hydrochloric acid aqueous solution is added to an electrolytic cell with a stirrer, and the electrolytic cell is added with palladium powder with a purity of more than 99.95% and a particle size of 200-400 mesh, palladium electrode sheets with a purity of more than 99.95% are inserted at the positive and negative electrodes of the electrolytic cell, the electrode leads are connected, the stirring is started and the power is turned on, the voltage is controlled at 6.5V and the current is controlled at 7.2A, electrolysis is carried out, bubbles are generated on the surface of the palladium electrode sheet, the palladium powder starts to dissolve, and the solution gradually changes from colorless to deep red until the palladium powder is completely dissolved.

[0022] Step 2: The above deep red solution is passed through the LSC-495 chelate resin column for secondary impurity removal, and then concentrated to the target concentration to obtain an ultra-high purity palladium chloride hydrochloride solution, or concentrated to dryness to obtain an ultra-high purity reddish-brown palladium chloride crystal.

[0023] The above steps are all operated in a glove box clean and dust-free environment formed by fresh air filtration.

[0024] The purity of the palladium chloride crystal reaches 99.9997% through sampling ICP-MS analysis and detection. Example 2

[0025] Step 1: The glacial acetic acid solution with a mass concentration of 45% is passed through the LSD396 complex adsorption resin column, then deionized water is added for dilution to obtain a 2.5 mol / L acetic acid aqueous solution; the acetic acid aqueous solution is added to an electrolytic cell with a stirrer, and the electrolytic cell is added with palladium powder with a purity of more than 99.95% and a particle size of 200-400 mesh, palladium electrode sheets with a purity of more than 99.95% are inserted at the positive and negative electrodes of the electrolytic cell, the electrode leads are connected, the stirring is started and the power is turned on, the voltage is controlled at 12.5V and the current is controlled at 7.5A, electrolysis is carried out, bubbles are generated on the surface of the palladium electrode sheet, the palladium powder starts to dissolve, and the solution gradually changes from colorless to deep red until the palladium powder is completely dissolved.

[0026] Step 2: The above deep red solution is subjected to secondary impurity removal by passing through a LSC-495 chelating resin column to remove metal impurities, and then concentrated to a target concentration to obtain an ultrahigh-purity palladium acetate solution, or concentrated to dryness to obtain ultrahigh-purity brown palladium acetate crystals.

[0027] The above steps are all operated in a glove box clean dust-free environment formed by filtered fresh air.

[0028] The purity of the palladium acetate crystals reaches 99.9997% through sampling ICP-MS analysis and detection. Example 3

[0029] Step 1: A 36% mass concentration of concentrated hydrochloric acid is subjected to a LSD396 complex adsorption resin column, and then diluted with deionized water to obtain a 9.0 mol / L hydrochloric acid aqueous solution; the hydrochloric acid aqueous solution is added to an electrolytic cell with a stirrer, and rhodium powder with a purity of more than 99.95% and a particle size of 325-600 mesh is added to the electrolytic cell; rhodium electrode sheets with a purity of more than 99.95% are inserted into the positive and negative electrodes of the electrolytic cell, the electrode leads are connected, the stirring is started, and the power is turned on; the voltage is controlled at 7.5 V, and the current is controlled at 8.0 A to perform electrolysis; bubbles are generated on the surface of the rhodium electrode sheet, the rhodium powder starts to dissolve, the solution gradually changes from colorless to wine red, and the rhodium powder is completely dissolved.

[0030] Step 2: The above wine red solution is subjected to secondary impurity removal by passing through a LSC800 chelating resin column to remove metal impurities, and then concentrated to a target concentration to obtain an ultrahigh-purity rhodium chloroacetate solution, or concentrated to dryness to obtain ultrahigh-purity reddish-brown rhodium trichlorohydrate crystals.

[0031] The above steps are all operated in a glove box clean dust-free environment formed by filtered fresh air.

[0032] The purity of the rhodium trichlorohydrate crystals reaches 99.9992% through sampling ICP-MS analysis and detection. Example 4

[0033] Step 1: A 30% mass concentration of sulfuric acid solution is subjected to a LSD396 complex adsorption resin column, and then diluted with deionized water to obtain a 2.0 mol / L sulfuric acid aqueous solution; the sulfuric acid aqueous solution is added to an electrolytic cell with a stirrer, and rhodium powder with a purity of more than 99.95% and a particle size of 325-600 mesh is added to the electrolytic cell; rhodium electrode sheets with a purity of more than 99.95% are inserted into the positive and negative electrodes of the electrolytic cell, the electrode leads are connected, the stirring is started, and the power is turned on; the voltage is controlled at 8.5 V, and the current is controlled at 7.5 A to perform electrolysis; bubbles are generated on the surface of the rhodium electrode sheet, the rhodium powder starts to dissolve, the solution gradually changes from colorless to deep red, and the rhodium powder is completely dissolved.

[0034] Step 2: The above dark red solution is subjected to secondary impurity removal by passing through a LX-935 complex adsorption resin column to remove metal impurities, and then concentrated to a target concentration to obtain a rhodium sulfate solution with ultra-high purity, or concentrated to dryness to obtain red-brown rhodium sulfate crystals with ultra-high purity.

[0035] The above steps are all operated in a glove box clean dust-free environment formed by filtered fresh air.

[0036] The purity of the rhodium sulfate crystals reaches 99.9993% as detected by sampling ICP-MS analysis. Example 5

[0037] Step 1: Concentrated hydrochloric acid with a mass concentration of 36% is subjected to a LX-935 complex adsorption resin column, and then diluted with deionized water to obtain a 7.2 mol / L hydrochloric acid aqueous solution; the hydrochloric acid aqueous solution is added to an electrolytic cell with a stirrer, and platinum powder with a purity of more than 99.95% and a particle size of 200-400 mesh is added to the electrolytic cell; platinum electrode sheets with a purity of more than 99.95% are inserted into the positive and negative electrodes of the electrolytic cell, and the electrode leads are connected; the stirring is started and the power is turned on, and the voltage is controlled at 6.5V and the current is controlled at 6.5A for electrolysis; bubbles are generated on the surface of the platinum electrode sheet, the platinum powder starts to dissolve, and the solution gradually changes from colorless to dark red until the platinum powder is completely dissolved.

[0038] Step 2: The above dark red solution is subjected to secondary impurity removal by passing through a LX-935 complex adsorption resin column to remove metal impurities, and then concentrated to a target concentration to obtain a rhodium sulfate solution with ultra-high purity, or concentrated to dryness to obtain red-brown rhodium sulfate crystals with ultra-high purity.

[0039] The above steps are all operated in a glove box clean dust-free environment formed by filtered fresh air.

[0040] The purity of the rhodium sulfate crystals reaches 99.9993% as detected by sampling ICP-MS analysis. Example 6

[0041] Step 1: Concentrated hydrochloric acid with a mass concentration of 36% is subjected to a LX-935 complex adsorption resin column, and then diluted with deionized water to obtain a 7.2 mol / L hydrochloric acid aqueous solution; the hydrochloric acid aqueous solution is added to an electrolytic cell with a stirrer, and platinum powder with a purity of more than 99.95% and a particle size of 200-400 mesh is added to the electrolytic cell; platinum electrode sheets with a purity of more than 99.95% are inserted into the positive and negative electrodes of the electrolytic cell, and the electrode leads are connected; the stirring is started and the power is turned on, and the voltage is controlled at 6.5V and the current is controlled at 6.5A for electrolysis; bubbles are generated on the surface of the platinum electrode sheet, the platinum powder starts to dissolve, and the solution gradually changes from colorless to dark red until the platinum powder is completely dissolved.

[0042] Step 2: The above reddish-brown solution is subjected to a second impurity removal by passing through a LSC-600 chelating resin column, and then concentrated to a target concentration to obtain an ultrahigh-purity iridium trichloride hydrochloride solution, or concentrated to dryness to obtain ultrahigh-purity dark green iridium trichloride hydrate crystals.

[0043] The above steps are all operated in a glove box clean dust-free environment formed by filtered fresh air.

[0044] The purity of the iridium trichloride hydrate crystals reaches 99.9991% as detected by sampling ICP-MS analysis. Example 7

[0045] Step 1: Concentrated hydrochloric acid with a mass concentration of 36% is subjected to a LSD396 complex adsorption resin column, and then diluted with deionized water to obtain a 10.0 mol / L hydrochloric acid aqueous solution; the hydrochloric acid aqueous solution is added to an electrolytic cell with a stirrer, and ruthenium powder with a purity of more than 99.95% and a particle size of 300-500 mesh is added to the electrolytic cell; a ruthenium electrode sheet with a purity of more than 99.95% is inserted into the positive and negative electrodes of the electrolytic cell, the electrode leads are connected, the stirring is started, and the power is turned on; the voltage is controlled at 12.0 V, and the current is controlled at 9.0 A to perform electrolysis; bubbles are generated on the surface of the ruthenium electrode sheet, the ruthenium powder starts to dissolve, and the solution gradually changes from colorless to dark brown until the ruthenium powder is completely dissolved.

[0046] Step 2: The above dark brown solution is subjected to a second impurity removal by passing through a LSC800 chelating resin column, and then concentrated to a target concentration to obtain an ultrahigh-purity chlororuthenic acid solution, or concentrated to dryness to obtain ultrahigh-purity brown ruthenium trichloride hydrate crystals.

[0047] The above steps are all operated in a glove box clean dust-free environment formed by filtered fresh air.

[0048] The purity of the ruthenium trichloride hydrate crystals reaches 99.9992% as detected by sampling ICP-MS analysis. Example 8

[0049] Step 1: Concentrated hydrochloric acid with a mass concentration of 36% is subjected to a LSD396 complex adsorption resin column, and then diluted with deionized water to obtain a 3.0 mol / L hydrochloric acid aqueous solution; the hydrochloric acid aqueous solution is added to an electrolytic cell with a stirrer, and gold powder with a purity of more than 99.95% and a particle size of 150-300 mesh is added to the electrolytic cell; a gold electrode sheet with a purity of more than 99.95% is inserted into the positive and negative electrodes of the electrolytic cell, the electrode leads are connected, the stirring is started, and the power is turned on; the voltage is controlled at 5.5 V, and the current is controlled at 6.0 A to perform electrolysis; bubbles are generated on the surface of the gold electrode sheet, the gold powder starts to dissolve, and the solution gradually changes from colorless to dark yellow until the gold powder is completely dissolved.

[0050] Step 2: The above deep yellow solution is subjected to a LSC-600 chelating resin column for secondary impurity removal, and then concentrated to a target concentration to obtain an ultrahigh-purity chloroauric acid solution, or concentrated to dryness to obtain ultrahigh-purity yellow gold trichloride crystals.

[0051] The above steps are all operated in a glove box clean and dust-free environment formed by filtered air.

[0052] Through sampling ICP-MS analysis and detection, the purity of the gold trichloride crystals reaches 99.9996%.

[0053] In the above examples, the instruments involved all use containers made of glass, quartz, polytetrafluoroethylene, etc. There is a risk of chlorine gas generation and overflow during the experiment, so measures such as tail gas collection and alkali absorption elimination should be taken in advance.

Claims

1. An electrochemical synthesis method of ultra-high purity noble metal compounds, characterized by: The method comprises the following steps: Step 1: passing an acid solution through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 1.0-10.0 mol / L; adding the acid aqueous solution into an electrolytic tank with stirring function, adding noble metal powder into the electrolytic tank, installing corresponding noble metal electrode sheets at the positive and negative electrodes of the electrolytic tank, connecting electrode wires, starting stirring and connecting power supply, and electrolyzing under a redox electrode potential until the noble metal powder is completely dissolved; the acid solution is any one of hydrochloric acid, sulfuric acid and acetic acid; Step 2: passing the solution in the electrolytic tank after electrolysis in step 1 through an acid-resistant resin column, and then performing vacuum distillation to concentrate to precipitate solids, so as to obtain a noble metal compound crystal with a purity of more than 99.999%. The above steps are all operated in a clean environment.

2. The electrochemical synthesis of ultrahigh purity noble metal compounds according to claim 1, characterized in that: In step 1, an acid solution is passed through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 1.0-10.0 mol / L; The acid aqueous solution is added into an electrolytic tank with stirring function, and palladium powder is added into the electrolytic tank; palladium electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started and power supply is connected; electrolysis is performed under a voltage of 3.5-18.0 V and a current of 1.0-10.0 A until the palladium powder is completely dissolved.

3. The method of electrochemical synthesis of ultrahigh purity noble metal compounds according to claim 1, characterized by the fact that: In step 1, an acid solution is passed through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 2.0-10.0 mol / L; The acid aqueous solution is added into an electrolytic tank with stirring function, and rhodium powder is added into the electrolytic tank; rhodium electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started and power supply is connected; electrolysis is performed under a voltage of 6.0-24.0 V and a current of 5.0-10.0 A until the rhodium powder is completely dissolved.

4. The electrochemical synthesis of ultrahigh purity noble metal compounds according to claim 1, characterized in that: In step 1, an acid solution is passed through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 3.0-8.0 mol / L; the acid aqueous solution is added into an electrolytic tank with stirring function, and platinum powder is added into the electrolytic tank; platinum electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started and power supply is connected; electrolysis is performed under a voltage of 3.0-15.0 V and a current of 2.0-8.0 A until the platinum powder is completely dissolved.

5. The method of electrochemical synthesis of ultrahigh purity noble metal compounds according to claim 1, characterized by that: In step 1, an acid solution is passed through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 6.0-10.0 mol / L; The acid aqueous solution is added into an electrolytic tank with stirring function, and iridium powder is added into the electrolytic tank; iridium electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started and power supply is connected; electrolysis is performed under a voltage of 5.0-20.0 V and a current of 4.0-10.0 A until the iridium powder is completely dissolved.

6. The method of electrochemical synthesis of ultrahigh purity noble metal compounds according to claim 1, characterized by that: In step 1, an acid solution is passed through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 3.0-10.0 mol / L; The acid aqueous solution is added into an electrolytic tank with stirring function, and ruthenium powder is added into the electrolytic tank; ruthenium electrode sheets are installed at the positive and negative electrodes of the electrolytic tank, electrode wires are connected, stirring is started and power supply is connected; electrolysis is performed under a voltage of 6.0-24.0 V and a current of 3.0-9.0 A until the ruthenium powder is completely dissolved.

7. The electrochemical synthesis of ultrahigh purity noble metal compounds according to claim 1, characterized by the fact that: In step 1, the acid solution is passed through an acid-resistant resin column to obtain an acid aqueous solution with a concentration of 1.0-10.0 mol / L; the acid aqueous solution is added into an electrolytic cell with stirring function, and gold powder is added into the electrolytic cell; gold electrode sheets are installed at the positive and negative electrodes of the electrolytic cell, electrode wires are connected, stirring is started, and power is turned on; electrolysis is carried out at a voltage of 3.0-7.5 V and a current of 2.0-6.0 A until the gold powder is completely dissolved.

8. The electrochemical synthesis of ultrahigh purity noble metal compounds according to any one of claims 1 to 7, characterized in that: The clean environment is provided by a glove box, and the glove box is internally ventilated with air filtered by a fresh air filtering system.

9. The electrochemical synthesis of ultrahigh purity noble metal compounds according to any one of claims 1 to 7, characterized in that: The acid-resistant resin is selected from any one of chelating resins and complex adsorption resins.

10. The electrochemical synthesis of ultrahigh purity noble metal compounds according to any one of claims 1 to 7, characterized in that: In step 1, the purity of the noble metal powder is greater than 99.95%, and the particle size is 150-800 mesh, accounting for greater than or equal to 95%.