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Method for jointly removing phosphine by aid of complexation systems and jet flow by means of oxidizing

A phosphine and system technology, applied in chemical instruments and methods, separation methods, gas treatment, etc., can solve the problems of potential safety hazards, blackening of waste acid, blackening of sulfuric acid, etc., to improve safety and corrosion Low, cost-saving effect

Active Publication Date: 2018-11-13
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the concentrated sulfuric acid purification process can well achieve the expected treatment purpose, there are still many problems in the operation process: (1) the concentration of concentrated sulfuric acid is very strict, because the concentrated sulfuric acid will play the dual role of oxidation and dehydration, Therefore, the requirements for its concentration are very strict. The mass fraction of sulfuric acid entering the concentrated sulfuric acid cleaning tower must be greater than 98%. When the mass fraction of sulfuric acid drops to 80%, it is sent to the waste acid tank, which requires frequent detection of concentrated sulfuric acid concentration to ensure efficient operation of the entire process; (2) carbonization causes sulfuric acid to turn black, making it difficult to treat waste acid
Concentrated sulfuric acid dehydrates and carbonizes long-chain olefins and unsaturated long-chain alkynes in acetylene gas, so the waste acid produced by the sulfuric acid cleaning system is black in color and contains various impurities, including sulfurous acid, phosphoric acid, etc.; (3) Carbide causes serious equipment damage
The nature of concentrated sulfuric acid itself determines that it has high requirements on the operating equipment to ensure no corrosion, no leakage and long-term operation, but the accumulation of some carbides during the treatment process will damage the equipment, posing a safety hazard

Method used

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  • Method for jointly removing phosphine by aid of complexation systems and jet flow by means of oxidizing
  • Method for jointly removing phosphine by aid of complexation systems and jet flow by means of oxidizing
  • Method for jointly removing phosphine by aid of complexation systems and jet flow by means of oxidizing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] Weigh 1.76g Fe 2 (SO 4 ) 3 , 2.57g EDTA is added to 14.83mL 85% H 3 PO 4 After stirring to dissolve, dilute with pure water to 51mL(nEDTA:nFe 3+ =1:1); After mixing, pour it into a glass reaction device, and finally add 9mL of freshly produced nano-microbubble water, control the reaction temperature to maintain at 40°C, and after sealing, open the phosphine hydrogen bottle with a concentration of 1000ppm to start ventilation. And adjust the gas flow to stabilize at 20mL / min.

[0091] Such as image 3 As shown, the reaction liquid can react with phosphine, and the removal rate reaches the highest when the dephosphorization starts, which can reach about 45%. The reaction solution has an obvious effect on the removal of high-content phosphine, indicating that it can be applied to the removal of phosphine in the form of impurities in acetylene gas. Among them, the removal rate η is obtained by the following formula:

[0092]

[0093] C 0 Is the concentration of phosphine in ppm...

Embodiment 2

[0095] Weigh 1.76g Fe 2 (SO 4 ) 3 , 2.57g EDTA is added to 14.83mL 85% H 3 PO 4 After stirring to dissolve, dilute with pure water to 51mL(nEDTA:nFe 3+ =1:1), mix well and pour it into a glass reaction device, and finally add 9mL of freshly produced nanobubble water, control the reaction temperature at 40℃, 45℃ and 50℃ respectively, after sealing, open the phosphorus with a concentration of 1000ppm The hydrogen gas cylinder was ventilated, and the gas flow rate was adjusted to stabilize at 20 mL / min.

[0096] Such as Figure 4 As shown, as the temperature increases, the initial dephosphorization rate of the complexed iron and jet combined system also increases. The maximum dephosphorization rate of the system can reach 60% at 50℃, and the dephosphorization rate is faster than 40℃ and 45℃ over time; at 40℃, the dephosphorization rate can be maintained at a better level for a longer time (43% ~33%).

Embodiment 3

[0098] Weigh 1.76g Fe 2 (SO 4 ) 3 , 2.57g EDTA is added to 14.83mL 85% H 3 PO 4 After stirring to dissolve, dilute with pure water to 51mL(nEDTA:nFe 3+ =1:1), mix well and pour into a glass reaction device, and finally add 9mL, 18mL and 27mL of freshly produced nanobubble water respectively, control the reaction temperature at 40℃, 45℃ and 50℃, after sealing, open the concentration Start to ventilate the 1000 ppm phosphine hydrogen cylinder, and adjust the gas flow rate to stabilize at 20 mL / min.

[0099] Such as Figure 5 As shown, as the amount of nanobubble water added increases, the initial dephosphorization rate of the complexed iron and jet combined system also increases. The maximum dephosphorization rate of the system can reach more than 50% at 27mL.

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Abstract

The invention provides a method for jointly removing phosphine by the aid of complexation systems and jet flow by means of oxidizing. The method includes filling iron complex systems with gas containing phosphine impurities; adding nano-micro bubble water generated by the jet flow into the iron complex systems; oxidizing the phosphine by intermediate-state active species with strong oxidizing properties under catalytic effects of iron complexes to obtain phosphoric acid so as to achieve the purpose of removing the phosphine. The intermediate-state active species are generated by the nano-microbubble water. The method has the advantages that reaction conditions include the low temperatures and the normal pressure, operation can be facilitated, oxidized phosphine is transformed into the phosphoric acid, and the method is free of other byproducts and is a clean process convenient to industrially popularize and utilize.

Description

Technical field [0001] The invention belongs to the field of exhaust gas purification and relates to a method for removing phosphine. In particular, it relates to a safe and reliable green purification method that can directly oxidize phosphine gas under normal pressure and low temperature, has no by-product production, has no potential explosion hazard, and is safe and reliable. Background technique [0002] In the production of PVC by calcium carbide method, acetylene cleaning is an important process. In the industrial calcium carbide acetylene production process, the crude acetylene gas mainly contains impurity gases such as phosphine, which has a greater impact on subsequent industrial production. The impurity gas in the calcium carbide gas not only affects the purity of the acetylene gas, but also affects the purity of the final product. More importantly, the presence of impurity gases, especially phosphine, will have a toxic effect on a series of catalysts involved in indu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D53/78B01D53/46
CPCB01D53/46B01D53/78B01D2251/10B01D2255/20738B01D2257/55
Inventor 余江肖祥陈鹏
Owner BEIJING UNIV OF CHEM TECH
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