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Copper salt absorption liquid for desorbing arsenic hydride from ethane and propene in gas phase and application thereof

An arsine and absorbing liquid technology, applied in absorption purification/separation, organic chemistry, material separation, etc., can solve the problems of imperfect monitoring system, loss of purification production equipment, unsatisfactory dearsenic removal efficiency, etc., and achieve the cost of use Low, easy-to-obtain, high-sensitivity effects

Active Publication Date: 2012-01-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this arsenic removal agent is not specially developed for ethylene and propylene raw materials, and its arsenic removal efficiency cannot meet the requirements of polyolefin catalysts for raw materials (the new generation of high-efficiency polyolefin catalysts does not require arsine content in olefin raw materials. Greater than 30ppb (volume fraction))
In addition, the monitoring system of domestic olefin purification equipment is not perfect, and most of them rely on experience to calculate the use of purification systems
When the purification system fails or the purification effect decreases and is not replaced in time, it will bring great losses to the production equipment

Method used

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  • Copper salt absorption liquid for desorbing arsenic hydride from ethane and propene in gas phase and application thereof
  • Copper salt absorption liquid for desorbing arsenic hydride from ethane and propene in gas phase and application thereof
  • Copper salt absorption liquid for desorbing arsenic hydride from ethane and propene in gas phase and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0014] The arsine content of propylene in the refinery is 910ppb (volume fraction) after preliminary purification, and 0.26mol / L bromine aqueous solution: 30%H 2 o 2 Solution: 0.2mol / L copper chloride solution is mixed according to the volume ratio of 3:3:1, the concentration of bromine water in the mixed solution is 0.11mol / L, the concentration of hydrogen peroxide is 3.7mol / L, and the concentration of copper chloride is 0.03mol / L L, then adjust the pH value to 3 with 1:1 concentrated hydrochloric acid and concentrated nitric acid, and then pack it into a 60mm in diameter and 250mm long airtight purification absorber, and keep the temperature of the mixed solution at 70°C. Propylene containing 910ppb (volume fraction) of arsine passes through the first-stage absorption liquid (1) at a flow rate of 100mL / min and is directly connected to the six-way valve (3) for sampling of the monitoring system. The six-way valve is equipped with a quantitative loop Continuous quantitative s...

Embodiment 2

[0016] 0.26mol / L bromine aqueous solution: 30% H 2 o 2 Solution: 0.2mol / L copper chloride solution is mixed according to the volume ratio of 3:3:1, the concentration of bromine water in the mixed solution is 0.11mol / L, the concentration of hydrogen peroxide is 3.7mol / L, and the concentration of copper chloride is 0.03mol / L L, then use 1:1 concentrated hydrochloric acid and concentrated nitric acid to adjust the pH value to 3, then put it into three purification adsorbers with a diameter of 0.1m and a length of 1m, and keep the temperature of the mixed solution at 30°C. Refinery propylene containing arsine 910ppb (volume fraction) is purified and absorbed through the three-stage series absorption solution (1) at a flow rate of 1.2L / min, and then connected to the sampling six-way valve of the monitoring system through the bypass dryer (2) (3), the six-way valve is equipped with a quantitative loop to realize continuous quantitative sampling, and the sampling interval is 20 minu...

Embodiment 3

[0018] The refinery propylene monitors after preliminary purification and finds that the arsine content is 910ppb (volume fraction), and 0.26mol / L bromine aqueous solution: 30%H 2 o 2 Solution: 0.2mol / L copper sulfate solution is mixed in a volume ratio of 4:4:1, the concentration of bromine water in the mixed solution is 0.12mol / L, the concentration of hydrogen peroxide is 3.9mol / L, and the concentration of copper sulfate is 0.02mol / L. Then use 1:1 concentrated hydrochloric acid and concentrated nitric acid to adjust the pH value to 2 and then pack it into a purification adsorber with a diameter of 60 mm and a length of 250 mm, and the temperature of the mixed solution is kept at 70°C. Propylene containing trace arsine 910ppb (volume fraction) is purified and absorbed through the primary absorption liquid (1) at a flow rate of 80mL / min, and then directly connected to the six-way valve (3) for sampling of the monitoring system. The six-way valve is equipped with The quantitat...

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Abstract

The invention relates to a copper salt absorption liquid for desorbing arsenic hydride from ethane and propene in gas phase and an online monitoring system. The absorption liquid is composed of the mixed liquid of bromine water, hydrogen peroxide, copper salt and inorganic acid. The online monitoring system comprises a sampling system, a gas-phase chromatographic separation system and a mass spectrum analysis system, wherein a six-way valve of the sampling system is used for sampling continuously; and the gas-phase chromatographic separation system is used for separating the arsenic hydride from the ethane and the propene, and then the mass spectrum analysis system is used for monitoring quantitatively. The absorption liquid provided by the invention has the advantages of simple ingredient and low cost. The arsenic hydride in the ethane and the propene can be desorbed to a content of smaller than 30ppb. The online monitoring system has the advantages of high sensitivity, low limit of detection and capability of rapidly reflecting the absorbing and purifying effect of the absorption liquid.

Description

technical field [0001] The invention relates to a solution for purifying arsine gas in gaseous ethylene and propylene through a catalytic oxidation method, and monitors the purification effect of the absorption solution through an online monitoring system to ensure that the content of arsine after purification is less than 30ppb. Background technique [0002] Ethylene and propylene gas are raw material gases for the production of polyolefins, so the performance of polyethylene and polypropylene depends on the polymerization process and also on the purity of raw materials and impurity content. Arsenide is a typical polyolefin catalyst poison. Many catalysts used in industry are very sensitive to arsenide. A very small amount (a few tenths of a million) of arsenide can poison and deactivate the catalyst. Changes in domestic refinery crude oil, improvements in deep processing technology, and continuous improvement in processing capacity have resulted in the presence of arsenic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/11C07C11/04C07C11/06G01N30/02
Inventor 陈松宋阳李思睿张颖
Owner CHINA PETROLEUM & CHEM CORP
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