Purification for separating feed gas in stabilized isotope 13C by low-temperature CO rectifying method

A low-temperature rectification and purification process technology, applied in the field of chemical production process, can solve the problems of inconvenient operation, complex equipment, high requirements for equipment conditions, etc., and achieve the effect of high purification efficiency, simple device and convenient use

Active Publication Date: 2007-04-04
SHANGHAI RES INST OF CHEM IND
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AI Technical Summary

Problems solved by technology

[0004] However, most of the above methods cannot achieve the detection of H in CO feed gas. 2 O.CO 2 , O 2 In-depth purification requirements, using palladium / metal oxide catalytic reaction to remove O 2 , artificially increased H 2 components, and the precious metal catalyst has short life and high price
The use of pressure swing adsorption is complicated in equipment, high in energy consumption, and low in gas purity, so it can only be used as a means of preliminary purification.
Low temperature distillation method is difficult to operate, high energy consumption, high requirements for equipment conditions, and high cost
The United States uses alkaline asbestos membrane adsorption, which can only absorb CO 2 , and have to be replaced regularly, inconvenient to operate
None of the above methods can satisfy CO low temperature rectification to produce stable isotope 13 C and 18 O Requirements for Raw Gas

Method used

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  • Purification for separating feed gas in stabilized isotope 13C by low-temperature CO rectifying method

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Experimental program
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Effect test

Embodiment 1

[0028] Cylinder CO feed gas contains O 2 50ppm, H 2 O 30ppm, CO 2 10ppm, N 2 500ppm, with a flow rate of 100L / h and a pressure of 0.15MPa, after passing through a molecular sieve normal temperature adsorber (the size of the adsorber is Φ50×1000, with 5A molecular sieve inside), the H 2 O≤1ppm, CO 2 ≤4ppm; then enter the chemical purification column (column size is Φ25×220, filled with Φ3mm sponge Ti particles), the purification column is heated to 700C to remove O in the raw gas 2 and further remove H 2 O and CO 2 , so that the O in the outlet gas 2 down to 0.1ppm, H 2O.CO 2 down to 0.1ppm; then enter the molecular sieve low-temperature adsorber (filled with 5A molecular sieve, particle size 4mm), deep purification at -190°C to obtain H 2 O.CO 2 , O 2 All≤0.01ppm; N 2 , Ar, and organic impurity gases are all ≤ 1ppm product gas.

Embodiment 2

[0030] O in industrial CO feed gas 2 ≤5%, H 2 O≤3%, CO 2 ≤1%, the rest is N 2 , Ar and organic impurity gas, with a flow rate of 140L / h and a pressure of 0.5MPa, after passing through a molecular sieve normal temperature adsorber (filled with 4A molecular sieve, particle size Φ4mm, adsorber is Φ500×5000), the H in the outlet gas 2 O≤4ppm, CO 2 ≤5ppm; then enter the chemical purification column (filled with Φ3mm manganese oxide particles, filling size Φ50×500), the purification column is heated to 200°C, O 2 The gas can be removed to 0.1ppm; then the gas enters the molecular sieve cryogenic adsorber (filled with 5A molecular sieve, particle size Φ4mm), and is deeply purified at -100°C to obtain H 2 O.CO 2 , O 2 All≤0.01ppm, while N 2 , Ar and organic impurities are all lower than 1ppm product gas.

Embodiment 3

[0032] O in industrial CO feed gas 2 ≤5%, H 2 O≤3%, CO 2 ≤1%, the rest is N 2 , Ar and organic impurity gas, with a flow rate of 120L / h and a pressure of 0.3MPa, after passing through the molecular sieve normal temperature adsorber 3 (filled with 13X molecular sieve, particle size Φ4mm, and the adsorber is Φ500×5000), the H in the outlet gas 2 O≤4ppm, CO 2 ≤5ppm; then enter the chemical purification column (filled with Φ3mm manganese oxide particles, filling size Φ50×500), the purification column is heated to 500°C, O 2 The gas can be removed to 0.1ppm; then the gas enters the molecular sieve cryogenic adsorber (filled with 5A molecular sieve, particle size Φ4mm), and is deeply purified at -150°C to obtain H 2 O.CO 2 , O 2 All≤0.01ppm, while N 2 , Ar and organic impurities are all lower than 1ppm product gas.

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Abstract

Purification for separating charge gas of 13C stable isotope by CO low-temperature rectifying method is carried out by taking CO as charge gas, normal-temperature adsorbing, chemical purifying and low-temperature adsorbing. The content of O2 is <=0.01ppm, the content of H20 is <=0.01ppm and the content of CO2 is <=0.01ppm, they accord with technology requirement. It is simple and cheap, has advanced technology and high purifying efficiency and can be used to separate stable isotope 13C and 180 by CO low-temperature rectifying method.

Description

technical field [0001] The invention relates to a chemical production process, in particular to a CO low-temperature rectification separation method 13 Purification process of raw material gas in C stable isotope. Background technique [0002] CO cryogenic rectification method is the current method to produce stable isotope 13 The main method of C, the purity of CO feed gas is the key to CO cryogenic rectification. The cryogenic distillation process requires O in the CO feed gas 2 ≤0.1ppm, H 2 O≤0.1ppm, CO 2 ≤0.1ppm; while industrial CO feed gas, CO>90%, O 2 ≤5%, H 2 O≤3%, CO 2 ≤1%. Even electronic grade high-purity CO gas still contains H 2 O about 30ppm, CO 2 About 10ppm, O 2 About 50ppm, much higher than the process requirements. If the concentration of the above three components is too high, it is easy to crystallize in the rectification tower to block the pipeline, or even explode. Therefore, the deep purification technology of CO raw material gas determi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/18B01D53/04B01D59/04C01B32/40
Inventor 李虎林李良君陈仙送杜晓宁于国庆刘建亮杨继群
Owner SHANGHAI RES INST OF CHEM IND
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