A preparation method and device for a stable arsenic trioxide standard gas

A technology of arsenic trioxide and a flow control device, which is applied in the field of flue gas purification, can solve the problems of low efficiency of arsenic hydrogen, etc., and achieve the effects of improved generation and oxidation efficiency and high stability

Active Publication Date: 2022-05-17
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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Problems solved by technology

[0004] In order to overcome the disadvantages of the prior art, the present invention provides a stable preparation method and device for diarsenic trioxide standard gas, and proposes the optimal conditions for the use of instrument reagents on the basis of comprehensively considering the efficient and stable operation of each part of the system to solve the problem of arsenic hydrogen The problem of low efficiency; the atomization unit is installed after the arsine hydrogen generation unit, so that the arsenic hydrogen atomization reaction generates atomic arsenic, and the atomic arsenic is combined with oxygen to generate arsenic trioxide gas, which improves the oxidation efficiency

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  • A preparation method and device for a stable arsenic trioxide standard gas

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Embodiment 1

[0029] When sodium arsenite with a concentration of 30 ppm is mixed with 10% (V / V) hydrochloric acid in the three-way reaction block I, it is further reacted with 0.3% (V / V) potassium borohydride in the three-way reaction block II , the generated arsine and hydrogen gas are mixed with 200 mL / min argon gas through the gas-liquid separator, and then brought into the atomization reactor (400 ℃) for atomization, and the generated atomic arsenic is mixed with 400 mL / min nitrogen and oxygen mixed gas (oxygen is 60 mL / min) for mixed oxidation, and finally arsenic trioxide gas is generated. The determination of the arsenic content in the separated mother liquor showed that the content was less than 1.5 ppm (<5%), which proved that the arsenic in the sodium arsenite device basically formed arsenic hydride and participated in the subsequent reaction. After cleaning the arsenic in the reaction tube, tail gas absorption liquid and connecting tube, it was found that the recovery rate of to...

Embodiment 2

[0031] When sodium arsenite with a concentration of 60 ppm is mixed with 10% (V / V) hydrochloric acid in the three-way reaction block I, it is further reacted with 0.5% (V / V) potassium borohydride in the three-way reaction block II, The generated arsine and hydrogen gas are mixed with 300mL / min argon gas through the gas-liquid separator, and then brought into the atomization reactor (500°C) for atomization, and the generated atomic arsenic is mixed with 500mL / min min nitrogen and oxygen mixed gas (oxygen is 100 mL / min) for mixed oxidation, and finally arsenic trioxide gas is generated. Determination of the arsenic content in the separated mother liquor showed that the content was less than 2.4 ppm (<5%). The recovery rate of total gaseous arsenic was higher than 95%, the concentration of formed arsenic was 0.047 mL / min, and the standard deviation of multiple determinations was less than 9%.

Embodiment 3

[0033] When sodium arsenite with a concentration of 120 ppm is mixed with 15% (V / V) hydrochloric acid in the three-way reaction block I, it is further reacted with 0.8% (V / V) potassium borohydride in the three-way reaction block II, The generated arsine and hydrogen gas are mixed with 600mL / min argon through the gas-liquid separator, and then brought into the atomization reactor (600°C) for atomization, and the generated atomic arsenic is mixed with 600mL / min at 750°C min nitrogen and oxygen mixed gas (oxygen is 200 mL / min) for mixed oxidation, and finally arsenic trioxide gas is generated. Determination of the arsenic content in the separated mother liquor showed that the content was less than 3.6 ppm (<5%). The recovery rate of total gaseous arsenic was higher than 94%, the concentration of formed arsenic was 0.088 mL / min, and the standard deviation of multiple determinations was less than 7%.

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Abstract

A stable method for preparing arsenic trioxide standard gas, comprising the following steps: generation of arsenic hydride: sodium arsenite reacts with hydrochloric acid and potassium borohydride to generate arsine gas and hydrogen gas, which are then separated by a gas-liquid separator; arsenic Atomization: The separated arsine gas and hydrogen gas enter the atomization reactor through the carrier gas, preheat at a certain temperature, and atomize the arsine gas into arsenic atoms through the flame at the furnace mouth of the atomizer ;Arsenic atomic oxidation: atomic arsenic is mixed with nitrogen and oxygen gas in the gas mixing chamber and brought into a high-temperature electric heating furnace, and fully combined with oxygen at a certain temperature to form arsenic trioxide; tail gas absorption. The present invention solves the problem of low generation efficiency of arsine by adjusting the ratio parameter of solution supply; an atomization unit is arranged after the arsenic hydride generation unit, so that arsine is pyrolyzed into atomic arsenic, and atomic arsenic is then combined with oxygen Combined with the generation of arsenic trioxide gas, the oxidation efficiency of arsenic hydrogen is greatly improved.

Description

technical field [0001] The invention relates to a preparation method and device of a stable arsenic trioxide standard gas, belonging to the technical field of flue gas purification. Background technique [0002] Exposure to excessive arsenic in the atmosphere can cause irreversible damage to human body functions. Arsenic in the flue gas of coal-fired power plants is one of the main sources of atmospheric arsenic, and the main form of occurrence is arsenic trioxide, which is highly toxic and easy to diffuse. However, in the past, most of the attention on heavy metals in flue gas has focused on the monitoring and control of mercury, and there is a lack of monitoring methods for the more toxic gaseous arsenic. Due to the huge workload, high cost and many uncontrollable effects of field experiments, it is very urgent to monitor arsenic trioxide in flue gas on a laboratory scale. [0003] The control of arsenic trioxide first requires a stable source. At present, there are few d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28C01G28/00
CPCG01N1/28C01G28/005
Inventor 苑春刚何楷强蒋洋红段雪雷黎燕史孟丹
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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