Preparation method of hydrogen selenide

A technology of hydrogen selenide and zinc selenide, applied in the direction of binary selenium/tellurium compounds, etc., can solve problems such as environmental pollution and large equipment investment

Active Publication Date: 2010-08-25
中昊光明化工研究设计院有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0015] The purpose of the present invention is to provide a new method for preparing hydrogen selenide, which can be prepared conveniently at any time, especially can meet the needs of selenium in organic and inorganic synthesis, is safe and simple, and overcomes the existing active selenide The shortcomings of environmental pollution caused by the process of hydrolysis and synthesis of hydrogen selenide, and the shortcomings of relatively large equipment investment required to overcome the direct reaction of selenium and hydrogen to synthesize hydrogen selenide

Method used

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Embodiment 1

[0034] 10 grams of zinc selenide is added in the reactor 2, and the whole system is purged with high-purity nitrogen to remove the air in the system; the reactor 2 is heated to 80°C with the heater 3, and 20 milliliters of 30% concentrated hydrochloric acid is added dropwise, one After hours of dropwise addition, the gas enters the receiving bottle 7 after being processed by the washer 4, the water washer 5 and the dryer 6, and the receiving bottle 7 is soaked in the cold well 8, and the temperature of the cold well is controlled at -110°C. The purity of hydrogen selenide was 95% (volume fraction) by gas chromatography, and the yield was 76%. After the reaction was finished, 5 milliliters of hydrogen peroxide was added dropwise to the liquid in the reactor 2 to remove hydrogen selenide in the liquid.

Embodiment 2

[0036] 10 grams of zinc selenide was added to reactor 2, and the whole system was purged with high-purity nitrogen to remove the air in the system; reactor 2 was heated to 80°C with heater 3, and 30 ml of 30% sulfuric acid was added dropwise for one hour After the dropwise addition, the gas is processed by the washer 4, the water washer 5 and the drier 6 and enters the receiving bottle 7. The receiving bottle 7 is soaked in the cold well 8, and the temperature of the cold well is controlled at -100°C. The purity of hydrogen selenide was 95% (volume fraction) as checked by gas chromatography, and the yield was 70%. After the reaction was finished, 5 milliliters of hydrogen peroxide was added dropwise to the liquid in the reactor 2 to remove hydrogen selenide in the liquid.

Embodiment 3

[0038] 500 grams of zinc selenide was added to reactor 2, and the air in the system was removed with high-purity nitrogen. Heat the reactor 2 to 80°C with the heater 3, start to drop 1000 milliliters of 30% concentrated hydrochloric acid, control the reaction process, the dropwise addition is completed in about 3 hours, and the generated gas passes through the washer 4, the water washer 5 and the drier 6 After the treatment, it enters the receiving bottle 7, and the receiving bottle 7 is soaked in the cold well 8, and the temperature of the cold well is controlled at -80°C. Obtain 205 grams of hydrogen selenide, the purity is greater than 95% (volume fraction), and the yield is 80%. After the reaction was finished, 20 milliliters of hydrogen peroxide was added dropwise to the liquid in the reactor 2 to remove hydrogen selenide in the liquid.

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Abstract

The invention discloses a preparation method of hydrogen selenide, which is synthesized by reacting zinc selenide and acid at the reaction temperature of 50-200DEG C and the mol ratio of the zinc selenide to the acid being 10:(1-0.1):1. The equipment has simple operation; the method for synthesizing the hydrogen selenide by reacting the zinc selenide and the acid has mild operation condition, well controls the synthesizing process as well as solves the problems that a method for synthesizing the hydrogen selenide by reacting the zinc selenide and water causes the pollution to the environment in the process of synthesizing aluminum selenide and in the process of using the aluminum selenide and extremely-high equipment investment is required by other methods.

Description

technical field [0001] The invention belongs to the technical field of organic chemical production, and in particular relates to a method for preparing hydrogen selenide gas. Background technique [0002] Hydrogen selenide gas is mainly used in the synthesis of inorganic or organic selenium-containing compounds to provide selenium. As we all know, selenium has special activity on the human body, especially the substances containing selenium compounds have activity on cancer cells, so they have a wide range of medical and medicinal prospects. In addition, high-purity hydrogen selenide can be used as semiconductor doping gas and production. [0003] The general method for preparing hydrogen selenide has: [0004] Synthesis of Hydrogen Selenide by Direct Reaction of Selenium and Hydrogen [0005] h 2 +Se→H 2 Se [0006] Selenide reacts with water to obtain hydrogen selenide, such as the hydrolysis of aluminum selenide [0007] 2Al+3Se→Al 2 Se 3 [0008] Al 2 Se 3 +H...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04
Inventor 徐永峰宋喜东梁肃臣岳成君
Owner 中昊光明化工研究设计院有限公司
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