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Method for preparing and purifying cuprous halide

A cuprous halide and purification method technology, applied in the direction of copper halide, copper chloride, etc., can solve the problems of complex equipment and process, small product particles, pollution of the environment, etc., and achieve the effect of economical reaction process, high purity and low price

Inactive Publication Date: 2010-09-29
ANHUI INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Each of the above methods has its shortcomings, for example: the direct reaction method needs to be completed under high temperature conditions, the equipment and process are more complicated, and the energy consumption is large; the monovalent copper salt hydrolysis method and the replacement method have a large amount of waste water in the reaction process, It not only pollutes the environment but also causes waste; some hydrolysis processes need to be completed under high temperature and high pressure, the equipment is complex, energy-consuming, and unsafe
The divalent copper salt reduction process is relatively simple, but the cost is high, and the prepared product has small particles, which are easily oxidized during post-processing and use.

Method used

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  • Method for preparing and purifying cuprous halide
  • Method for preparing and purifying cuprous halide
  • Method for preparing and purifying cuprous halide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment one: the preparation of cuprous chloride

[0023] Weigh 2.50g copper chloride hydrate (CuCl 2 2H 2 O) put into 50mL glass test tube, then add 40mL of ethylene glycol solvent, dissolve copper chloride hydrate (CuCl 2 2H 2 O) A grass-green solution is obtained. Close the mouth of the test tube with a rubber stopper with an open hole (diameter of the small hole is about 1 mm). Heat and maintain the temperature of the ethylene glycol solvent at around 160°C. After one day, the color of the solution becomes light, and there is a white precipitate at the bottom of the test tube. The white precipitate was washed twice with deionized water, and then dried in a vacuum oven at 60° C. for 8 hours.

[0024] Adopt X-ray powder diffraction technique to carry out phase analysis to product, the result is as follows figure 2 shown. The positions of all diffraction peaks are consistent with the standard spectrum, indicating that the obtained product is cuprous chloride...

Embodiment 2

[0025] Embodiment two: the purification of cuprous bromide

[0026] Put 4.0g of cuprous bromide (purity less than 95%) and 2.0g of potassium bromide (analytical pure) into the bottom of a glass container with a capacity of 100mL, and place a partition at the bottom and upper 1 / 5 of the container . Pour 90ml of ethylene glycol solvent (analytical grade), and seal the mouth of the glass container with a perforated rubber stopper. Heating the bottom of the glass container, keeping the temperature at the bottom at around 170°C, and the temperature near the upper partition at around 150°C, after 12 hours, a large amount of white cuprous bromide polycrystalline particles were deposited on the surface of the upper partition. The cuprous bromide was taken out, washed twice with deionized water, and then dried in a vacuum oven at 60° C. for 8 hours.

[0027] The phase analysis of the product was carried out by X-ray powder diffraction technique, and the result showed that the obtaine...

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Abstract

The invention discloses a method for preparing and purifying cuprous halide. The method comprises the following steps of: placing copper halide in a reaction vessel, adding a glycol solvent into the vessel, and keeping the constant temperature of between 130 and 180 DEG C for 24 to 48 hours to produce white cuprous halide grains; and purifying the cuprous halide by a special purifying device; placing the cuprous halide serving as raw materials on the bottom of the purifying device; adding the glycol solvent and a small amount of corresponding alkali halate into the vessel to make the vessel achieve about 90 percent of the degree of filling, and sealing the opening of the vessel by a plug or a cover which is provided with a pore; heating the vessel, keeping the temperature of a lower clapboard on the bottom of the vessel at about 170 DEG C, and keeping the temperature of an upper clapboard on the top of the vessel at about 150 DEG C; and depositing the purified cuprous halide on the surfaces of the clapboards, and washing and drying the cuprous halide deposited on the surface of the upper clapboard to obtain analytically pure cuprous halide. The method has the characteristics of simple equipment and method for synthesis and purification, mild condition, and environmental protection; and the obtained cuprous halide has complete crystalline form, large grain size, high purity, and strong oxidation resistance.

Description

technical field [0001] The patent of the invention belongs to the technical field of inorganic non-metallic materials, and specifically relates to a preparation and purification method of cuprous halide. Background technique [0002] Common cuprous halides include cuprous chloride (CuCl), cuprous bromide (CuBr) and cuprous iodide (CuI), which are an important class of chemical raw materials. Cuprous chloride can be used as the precursor of the insecticide cupric oxychloride; in the presence of aluminum chloride, cuprous chloride can absorb carbon monoxide, and this reaction is widely used in the ammonia synthesis industry; cuprous chloride can also be used as an organic reaction Catalysts, for example: (1) it can carry out 1,4-addition to α, β-unsaturated ketone together with Grignard reagent; (2) in the Sandmeyer reaction, use cuprous chloride (or bromide Cuprous) treatment of aromatic diazonium salts can give chlorinated aromatics (or brominated aromatics). Cuprous bromi...

Claims

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Application Information

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IPC IPC(8): C01G3/04C01G3/05
Inventor 万松明苗凤秀王宜申吕宪顺顾桂新张庆礼殷绍唐
Owner ANHUI INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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