Method for preparing cupric tungstate via electrolysis of cation membrane

A technology of cationic membrane and copper tungstate, applied in the direction of electrolysis process, electrolysis components, organic diaphragm, etc., can solve the problems of reaction time of additives, etc., and achieve the effect of short reaction time, large synthesis amount and simple process

Inactive Publication Date: 2014-10-01
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solid-state metathesis method has a lot of metal oxide impurities due to the uniform mixing of raw materials; the disadvantages of the sol-gel method, aqueous phase precipitation method, hydrothermal method, microwave method, etc. are the presence of additives or the long reaction time

Method used

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  • Method for preparing cupric tungstate via electrolysis of cation membrane
  • Method for preparing cupric tungstate via electrolysis of cation membrane
  • Method for preparing cupric tungstate via electrolysis of cation membrane

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Using 95ml of 0.01mol / L sodium tungstate solution as anolyte, 90ml of 0.01mol / L sodium hydroxide solution as catholyte, copper sheet as anode and titanium mesh as cathode, electrolyze at a constant voltage of 50V for 10min. The electrolyzed product was washed three times with deionized water, and then dried in a blast drying oven at a constant temperature of 60°C for 2 hours. The temperature was raised to 500°C at a heating rate of 1 min, then roasted at a constant temperature for 1 h, and cooled to room temperature naturally. The obtained product is tested for EDS and XRD, such as figure 1 with figure 2 .

[0029] By observing figure 1 From the EDS diagram, it can be obtained that there are only three elements of Cu, W and O in the product. By observing figure 2 In the XRD pattern, it can be determined that the obtained product is CuWO 4 .

Embodiment 2

[0031] With 95ml of 0.01mol / L sodium tungstate solution as anolyte, 90ml of 0.01mol / L sodium hydroxide solution as catholyte, copper sheet as anode and titanium mesh as cathode, electrolyze 306S with a constant current of 0.6A (Electrolysis time is based on Na + The theoretical electricity consumed by all the ions transferred to the cathode chamber is calculated, that is, ). The electrolyzed product was washed three times with deionized water, and then dried in a blast drying oven at a constant temperature of 60°C for 2 hours. Raise the temperature to 500°C at a heating rate of min, then roast at constant temperature for 1h, and cool to room temperature naturally. The obtained product is tested for EDS and XRD, such as image 3 .

[0032] By observing image 3 From the EDS diagram of (a), it can be obtained that there are only three elements of Cu, W, and O in the product. By observing image 3 The XRD pattern in (b), it can be confirmed that the obtained product is Cu...

Embodiment 3

[0034] With 95ml of 0.01mol / L sodium tungstate solution as anolyte, 90ml of 0.01mol / L sodium chloride solution as catholyte, copper sheet as anode and titanium mesh as cathode, electrolyze 306S with a constant current of 0.6A . The electrolyzed product was washed three times with deionized water, and then dried in a blast drying oven at a constant temperature of 60°C for 2 hours. Raise the temperature to 500°C at a heating rate of min, then roast at constant temperature for 1h, and cool to room temperature naturally. The obtained product is tested for EDS and XRD, such as Figure 4 .

[0035] By observing Figure 4 From the EDS diagram of (a), it can be obtained that there are only three elements of Cu, W, and O in the product. By observing Figure 4 The XRD pattern in (b), it can be confirmed that the obtained product is CuWO 4 .

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Abstract

The invention relates to a method for preparing cupric tungstate via a cation membrane electrolysis method. The method comprises the following steps: carrying out constant-current electrolysis or constant-voltage electrolysis on a sodium tungstate solution by utilizing a cation membrane for 3 to 30 minutes by taking a copper sheet as an anode, a noble electrode as a cathode, a sodium tungstate solution as an anolyte and a solution with pH between 0 and 14 as a catholyte under the condition that the temperature of the electrolytes is raised from room temperature to 90 DEG C; then cleaning an obtained product and drying; carrying out high-temperature roasting on the dried product, namely putting the product into a container under an air atmosphere, heating to 450 DEG C to 600 DEG C under a heating rate of 2.5 to 10 DEG C/min and roasting at a constant temperature for 1 to 5 hours; and naturally cooling to the room temperature, thereby obtaining a pure cupric tungstate crystal. According to the method, the Na<+> is transferred into a cathode chamber under the action of the electrolysis of the cation membrane; the reaction time is short and any additives are not used, so that the pure cupric tungstate can be obtained; and any impurities and impurity ions are not generated, so that the subsequent treatment is simple. In addition, the method is simple in process, easy to operate, small in investment and large in synthesis quantity. Thus, the method can be directly applied to industrial production.

Description

technical field [0001] The invention belongs to the field of inorganic materials, and in particular relates to copper tungstate, in particular to a method for preparing copper tungstate by cationic membrane electrolysis. technical background [0002] Metal tungstate (M(Ⅱ)WO 4 ) is a class of inorganic materials with many potential applications in different fields, such as: photoluminescence, microwave applications, optical fiber materials, scintillator materials, humidity sensors, magnetic properties, catalysts, etc. [0003] Copper tungstate has two crystal forms, one is the metastable form of octahedral structure, and the other is the stable form of tetrahedral structure. The metastable form of copper tungstate will change into the stable form of copper tungstate, which requires high temperature calcination. [0004] At present, the main methods of synthesizing metal tungstates include solid-state double decomposition method, sol-gel method, aqueous phase precipitation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/00C25B13/08
Inventor 张全生闵凡奇王淼李硕李细方党国举王昭勍李海燕
Owner SHANGHAI INST OF TECH
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