Preparation method of arsine

[0020] As described in the background art, the preparation method of arsine in the prior art uses a large amount of water, the reaction is not complete, and the resulting arsenic-containing waste liquid causes damage to the environment. In order to solve the above technical problems, the present invention provides a method for preparing arsine, which includes the following steps: mixing and reacting raw materials including calcium hydride and arsenic trichloride in a vacuum environment with a water content of less than 100 ppm to obtain arsine.

[0021] The preparation process of arsine in the prior art makes it difficult to remove the water in arsine, and the present invention can effectively solve the above problems by using anhydrous n-hexane as the medium; and, the present invention uses calcium hydride and arsenic trichloride. The reaction can also effectively solve the problem of incomplete arsine generation in the arsine production process in the prior art. Further, in ord...

[0033] The preparation method of arsine in this embodiment includes the following steps:

[0034] Add 1300g calcium hydride to the reaction kettle and vacuum process the reaction kettle. When the vacuum degree of the reaction kettle is 1kpa, the pressure of the reaction kettle is reduced to 10pa by a molecular pump to ensure that a very small amount of air remains in the reaction kettle. Add 3000g n-hexane (moisture is less than 100ppm, no air treatment). The temperature of the reaction kettle is set to 30°C, and the condenser is set to 0°C. When the temperature of the reaction kettle and the condenser reach the set temperature, turn on the stirring and start to add 1815g of arsenic trichloride dropwise. After the dropwise addition is completed in 2 hours, the reaction kettle is adjusted. At a temperature of 50°C, calcium hydride reacts with arsenic trichloride to obtain arsine. The n-hexane and arsine evaporated in the reactor enter the condenser for cooling. The liquefied n-hex...

[0036] The preparation method of arsine in this embodiment includes the following steps:

[0037] Add 1300g calcium hydride to the reactor, and treat the reactor with vacuum. When the vacuum of the reactor is 1kpa, the pressure of the reactor is reduced to 10pa by a molecular pump to ensure that a very small amount of air remains in the reactor. 3500g n-heptane (moisture less than 100ppm, no air treatment) The temperature of the reaction kettle is set to 30°C, and the condenser is set to 0°C. When the temperature of the reaction kettle and the condenser reach the set temperature, turn on the stirring and start to add 1815g of arsenic trichloride dropwise. After the dropwise addition is completed in 2 hours, the reaction kettle is adjusted. At a temperature of 50°C, calcium hydride reacts with arsenic trichloride to obtain arsine. The n-hexane and arsine evaporated in the reactor enter the condenser for cooling. The liquefied n-hexane is refluxed to the reactor, and the reflux con...