CN102937627B - Online analysis method for gas components in natural gas hydrogen production process - Google Patents
Online analysis method for gas components in natural gas hydrogen production process Download PDFInfo
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- CN102937627B CN102937627B CN201210399166.6A CN201210399166A CN102937627B CN 102937627 B CN102937627 B CN 102937627B CN 201210399166 A CN201210399166 A CN 201210399166A CN 102937627 B CN102937627 B CN 102937627B
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Abstract
The invention discloses an online analysis method for gas components in a natural gas hydrogen production process. According to the method, four valve, six columns, three quantitative pipes, double gas paths, double detectors (PDD and TCD), double channels and a host machine of a chromatograph are adopted, front end switch three way sampling is adopted, and merging-into-two way in the instrument is adopted to concurrently carry out trace detection and constant detection on 5N high purity hydrogen, conversion gas and shift gas, and monitor product quality and catalyst performances. According to the present invention, the method for determining five key impurities in the high purity hydrogen and contents of CO, CO2 and CH4 affecting catalyst performances in the conversion gas and the shift gas by using the single instrument has the following characteristics that: sensitivity meets testing requirements, and the two systems are adopted, such that rapid switch and accurate quantification can be achieved so as to effectively reduce an analysis time.
Description
Technical field
The present invention relates to a kind of analytical approach of gas composition, is particularly the analytical approach of major constituents in microcomponent and reformed gas in rock gas high purity hydrogen, conversion gas.
Background technology
Hydrogen is one of clean and the most eternal energy of the mankind.The formation of world energy sources has experienced from solidifying (bavin, coal, nucleon), liquefaction (oil), to the process of (rock gas, hydrogen) of vaporization, hydrocarbon proportion is wherein on the way down: 90% (bavin), 60% (coal) 30% (oil), 20% (rock gas), 0% (hydrogen), the content of hydrogen is more and more higher, and the content of carbon is more and more lower.As everyone knows, carbon dioxide is to pollute the chief culprit who causes global greenhouse effect, and the minimizing of carbon content means the clean energy.Hydrogen, due to its special character, is widely used in the industries such as petrochemical complex, aviation, metallurgy, electronics, electric power, building materials, gas manufacture.Along with the in short supply of world energy sources and the attention to environmental issue, hydrogen, as high-octane carrier, more and more receives the concern in the world.Due to the development of solar electrical energy generation, electrolysis hydrogen, fuel cell, hydrogen storage technology, the substitute that it is petroleum-based energy from general industrial gas transition that the status of hydrogen is about to.Direct-current discharge helium ionization detector (DID) is detecting device non-selective, that versatility is very strong, except carrier gas He, any gas is had to very sensitive response, and lowest detectable limit can be to 10
-9(ppb level) is to measure at present trace gas impurity detecting device with the most use.
In process for making hydrogen on-line analysis, most important is to make the analytic system of design can trace and constant impurity be analyzed simultaneously, be designed should be able to detect very soon impurity concentration and change, and can provide in a short period of time (steady state (SS)) assay value of balance and quantitatively accurately, the feature such as the low and analytical cycle of detectability is short.
The shortcomings such as traditional analytical approach is to adopt FID and TCD detecting device dehydration plant in addition, and regeneration rapidly that its shortcoming is that sensitivity is not high, the complicated unfavorable operation of gas circuit and dehydration column lost efficacy is complicated.
Summary of the invention
Goal of the invention of the present invention is the weak point in order to overcome prior art, the technique research and development of matched gas hydrogen manufacturing and the needs of production, according to the physicochemical property of hydrogen and each composition impurity, by being different from the innovation of three aspects of conventional method of analysis, trace and constant gas composition on-line analysis in a kind of natural gas hydrogen preparation technique are provided.
Goal of the invention of the present invention is achieved by the following technical solution: gas composition on-line analysis in a kind of natural gas hydrogen preparation technique, comprise high-purity hydrogen analysis and reformed gas, the analysis of variation gas, and its analytical procedure is:
(1), the analysis of 5N high-purity hydrogen
1. sampling: the input modes that adopt equipressure, two quantity tubes with chromatograph, follow large flow to purge displacement sampling, quantity tube 1min by 5N high-purity hydrogen with the flow displcement chromatography instrument of 0.1MPa, 300mL/min, guarantee that Rapid Detection impurity concentration changes, and can provide in a short period of time the assay value of balance;
2. separate trace impurity: the carrier gas of the testing sample gas 30mL/min flow after above-mentioned sampling is sent into the piece-rate system of processing through cleaning and separate trace impurity;
3. detect: the above-mentioned testing sample gas through separation trace impurity is inputted to chromatographic PDD detecting device and draw analysis result.
Above-mentioned steps 2. middle piece-rate system is chromatographic pair of quantity tube, three valve three rod structures, comprising: two 0.5mL quantity tubes, a pre-separation post, two analytical columns, a ten-way valve, two six-way valves.By operated pneumatic valve I, cut emptying sample gas in quantity tube 1 is sent into Q post CO wherein
2impurity is sent into the quantitative test of chromatographic PDD detecting device, and all the other components are by needle-valve emptying.By operated pneumatic valve I, the sample gas in quantity tube 2 is sent into 5A post I it is carried out to pre-separation, and pass through needle-valve 1 by most of major constituent hydrogen emptying, then by operated pneumatic valve II, remaining component is sent into 5A post II, and by O wherein
2, N
2, CH
4, CO impurity sends into the quantitative test of chromatographic PDD detecting device.
" stainless steel pipeline prevents the Adsorption Effect quantitative test of tube wall to pipe valve system: in above-mentioned analytical approach, all pipelines that contact with sample gas all adopt at 316L EP 1/8.All valves that contact with sample gas are selected blowing and sweeping type valve, in the protection in high-purity helium all the time of valve plane, while guaranteeing to switch, without air leaks, sneak among sample.
Chromatographic chromatographic condition: quantity tube 0.5mL, nebulizer gas pressure 0.4MPa, driving atmospheric pressure 0.4MPa, carrier gas flux 30mL/min, 60 ℃ of column temperatures, 120 ℃ of detector temperatures.
Q post: long 3m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 object Haysep Q.
5A post I: long 2m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 object 5A molecular sieve;
5A post II: long 2m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 order 5A molecular sieve;
Detection system: select imported from America pulsed discharge helium ionization detector (PDD) to detect the impurity content separating through piece-rate system, the average detected limit 10 × 10
-9.
(2) analysis of reformed gas, conversion gas
4. sampling: the input mode that adopts equipressure, single quantity tube with chromatograph, follow large flow to purge displacement sampling, quantity tube 1min by reformed gas, conversion gas with the flow displcement chromatography instrument of 0.1MPa, 300mL/min, guarantee that Rapid Detection impurity concentration changes, and can provide in a short period of time the assay value of balance;
5. separate constant impurity: the carrier gas of the testing sample gas 30mL/min flow after above-mentioned sampling is sent into the piece-rate system of processing through cleaning and separate constant impurity;
6. detect: the above-mentioned testing sample gas through separation constant impurity is inputted to chromatographic TCD detecting device and draw analysis result.
Above-mentioned piece-rate system is chromatographic single quantity tube, single valve three rod structures, comprising: a 0.5mL quantity tube, a blowback post, two analytical columns, a ten-way valve.By operated pneumatic valve, cut just to blow sample gas in quantity tube 1 is sent into Q post, treat CO, CO
2and CH
4by Q post, send into after analytical column, valve switching just blows the moisture remaining in Q post off.Finally pass through R post by CO
2impurity is sent into the quantitative test of chromatographic TCD detecting device, by 5A post by CO, CH
4impurity is sent into the quantitative test of chromatographic TCD detecting device.
" stainless steel pipeline prevents the Adsorption Effect quantitative test of tube wall to pipe valve system: in above-mentioned analytical approach, all pipelines that contact with sample gas all adopt at 316L EP 1/8.All valves that contact with sample gas are selected blowing and sweeping type valve, in the protection in high-purity helium all the time of valve plane, while guaranteeing to switch, without air leaks, sneak among sample.
Chromatographic chromatographic condition: quantity tube 0.5mL, nebulizer gas pressure 0.4MPa, driving atmospheric pressure 0.4MPa, carrier gas flux 30mL/min, 60 ℃ of column temperatures, 120 ℃ of detector temperatures.
Q post: long 3m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 object Haysep Q.
R post: long 2m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 object Haysep R;
5A post: long 2m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 order 5A molecular sieve;
Detection system: select domestic thermal conductivity detector (TCD) (TCD) to detect the impurity content separating through piece-rate system, the average detected limit 50 × 10
-6.The combination gas H of operation
2, CO, CO
2hts catalyst Fe is being housed
2o
3variation stove in carry out water gas reaction, CO further with steam reaction, most of CO is converted into CO
2and H
2.Its process using high temperature shift, the gas after conversion is after cooling after separating technology condensed fluid, and gas is sent into hydrogen purification operation.
4. hydrogen purification: adopt general hydrogen section and purification section two-stage purifying process.General hydrogen section adopts 8-2-5/PSA technique, and this operation is comprised of 8 adsorption towers, and normal pressure desorption mode is all pressed in 2 adsorption tower chargings simultaneously for 5 times; Purification section adopts 6-2-3/PSA technique, and this operation is comprised of 6 adsorption towers, and normal pressure desorption mode is all pressed in 2 adsorption tower chargings simultaneously for 3 times.
The invention has the beneficial effects as follows: and the present invention adopt PDD to trace impurity analyze advantage be highly sensitive, all components is had to corresponding genus common detector, the analytical error that when adopting TCD to analyze constant impurity and design the saturation water adopting in back-flushing technique emptying reformed gas, conversion gas and eliminated that shortcoming improves analysis efficiency frequently to deoxidation column regeneration by gas circuit, the loaded down with trivial details optional equipment of optimization brings.Use in single Instrument measuring high-purity hydrogen the CO, the CO that in 5 kinds of critical impurities and reformed gas, conversion gas, affect catalyst performance
2, CH
4the method of content, its sensitivity meets test request, uses one or two kind of system, can switch fast accurate quantitative analysis, thereby effectively reduces the time of analysis.
Accompanying drawing explanation
Accompanying drawing 1 has represented a kind of process chart of natural gas hydrogen preparation method of the present invention.
Accompanying drawing 1 is the structural drawing of piece-rate system of the present invention;
In figure: 1. quantity tube; 2. quantity tube; 3. ten-way valve; 4. six-way valve; 5. six-way valve; 6.Q post; 7.5A post I; 8. 5A post II; 9.PDD detecting device.
Embodiment
Below, with reference to accompanying drawing 1, the present invention will be described.
One, the analysis of 5N high-purity hydrogen
Use 5N high-purity hydrogen as sample, this sample enters quantity tube 1, the quantity tube 2 of chromatograph displcement chromatography instrument with the flow of 0.1MPa, 300mL/min.After displacement 1min, start-up operation program.Sample gas in quantity tube 1, quantity tube 2 is sent into respectively to chromatographic Q post and 5A post I, in Q post, by needle-valve 3 emptying, remove CO
2all components, then enter chromatographic PDD detecting device Analysis for CO
2impurity content.5A post I plays pre-separation effect, and passes through needle-valve 1 by major constituent H
2most of emptying, but to guarantee the O in sample gas
2loss, is not then sent into remaining ingredient in chromatographic 5A post II and separates by switch valve 2, finally by chromatographic PDD detecting device quantitative test impurity content.
Two, the analysis of reformed gas, conversion gas
Use reformed gas, conversion gas as sample, this sample enters the quantity tube 1 of chromatograph displcement chromatography instrument with the flow of 0.1MPa, 300mL/min.After displacement 1min, start-up operation program.Sample pneumatic transmission in quantity tube 1 is entered to chromatographic Q post, wait component CO to be measured, CO
2, CH
4enter after 5A post and R post, switch ten-way valve the moisture remaining in chromatographic Q post is just blown off.And CO, CO
2, CH
4after Fen Li with R post by chromatographic 5A post respectively, enter respectively chromatographic TCD detecting device and carry out quantitative test.
Peak area and calibrating gas by each spectrum peak in analysis of spectra compare, and draw O in high-purity hydrogen
2, N
2, CH
4, CO impurity content, and in reformed gas, conversion gas, affect CO, the CO of catalyst performance
2, CH
4the method of content.
Claims (5)
1. an on-line analysis for gas composition in natural gas hydrogen preparation technique, comprises high-purity hydrogen analysis and reformed gas, the analysis of variation gas, it is characterized in that its analytical procedure is:
(1) analysis of 5N high-purity hydrogen
1. sampling: the input modes that adopt equipressure, two quantity tubes with chromatograph, follow large flow to purge displacement sampling, flow displacement quantity tube 1min by 5N high-purity hydrogen with 0.1MPa, 300mL/min, guarantee that Rapid Detection impurity concentration changes, and can provide in a short period of time the assay value of balance;
2. separate trace impurity: this piece-rate system is chromatographic pair of quantity tube, three valve three rod structures, comprise: two 0.5mL quantity tubes, a pre-separation post, two analytical columns, a ten-way valve, two six-way valves, cut emptying by operated pneumatic valve I sample gas in quantity tube I sent into Q post CO wherein
2impurity is sent into the quantitative test of chromatographic PDD detecting device, all the other components are by needle-valve emptying, by operated pneumatic valve I, the sample gas in quantity tube II is sent into 5A post I it is carried out to pre-separation, and pass through needle-valve 1 by most of major constituent hydrogen emptying, then by operated pneumatic valve II, remaining component is sent into 5A post II, and by O wherein
2, N
2, CH
4, CO impurity sends into the quantitative test of chromatographic PDD detecting device;
3. detect: the above-mentioned testing sample gas through separation trace impurity is inputted to chromatographic PDD detecting device and draw analysis result;
(2) analysis of reformed gas, conversion gas
1. sampling: the input mode that adopts equipressure, single quantity tube with chromatograph, follow large flow to purge displacement sampling, reformed gas, conversion gas are replaced to quantity tube 1min with the flow of 0.1MPa, 300mL/min, guarantee that Rapid Detection impurity concentration changes, and can provide in a short period of time the assay value of balance;
2. separate constant impurity: this piece-rate system is chromatographic single quantity tube, single valve three rod structures, comprise: a 0.5mL quantity tube, a blowback post, two analytical columns, a ten-way valve, by operated pneumatic valve, cut just to blow sample gas in quantity tube I is sent into Q post, treat CO, CO
2and CH
4by Q post, send into after analytical column, valve switching just blows the moisture remaining in Q post off, finally passes through R post by CO
2impurity is sent into the quantitative test of chromatographic TCD detecting device, by 5A post by CO, CH
4impurity is sent into the quantitative test of chromatographic TCD detecting device;
3. detect: the above-mentioned testing sample gas through separation constant impurity is inputted to chromatographic TCD detecting device and draw analysis result.
2. the on-line analysis of gas composition in natural gas hydrogen preparation technique as claimed in claim 1; it is characterized in that all pipelines that contact with sample gas in the analysis of above-mentioned 5N high-purity hydrogen all adopt at 316L EP 1/8 " stainless steel pipeline; prevent the Adsorption Effect quantitative test of tube wall; all valves that contact with sample gas are selected blowing and sweeping type valve; in the protection in high-purity helium all the time of valve plane, sneak among sample while guaranteeing to switch without air leaks.
3. gas composition on-line analysis in natural gas hydrogen preparation technique as claimed in claim 2, is characterized in that the chromatograph condition in its analytical approach: quantity tube 0.5mL, nebulizer gas pressure 0.4MPa, driving atmospheric pressure 0.4MPa, carrier gas flux 30mL/min, 60 ℃ of column temperatures, 120 ℃ of detector temperatures;
Q post: long 3m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 object Haysep Q;
5A post I: long 2m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 object 5A molecular sieve;
5A post II: long 2m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 order 5A molecular sieve;
Detection system: select imported from America pulsed discharge helium ionization detector (PDD) to detect the impurity content separating through piece-rate system, the average detected limit 10 × 10
-9.
4. the on-line analysis of gas composition in natural gas hydrogen preparation technique as claimed in claim 1; in it is characterized in that in the analysis of described reformed gas, conversion gas, all pipelines that contact with sample gas all adopt at 316L EP 1/8 " stainless steel pipeline; prevent the Adsorption Effect quantitative test of tube wall; all valves that contact with sample gas are selected blowing and sweeping type valve; in the protection in high-purity helium all the time of valve plane, sneak among sample while guaranteeing to switch without air leaks.
5. the on-line analysis of gas composition in natural gas hydrogen preparation technique as claimed in claim 5, is characterized in that the chromatographic chromatographic condition in its analytical approach: quantity tube 0.5mL, nebulizer gas pressure 0.4MPa, driving atmospheric pressure 0.4MPa, carrier gas flux 30mL/min, 60 ℃ of column temperatures, 120 ℃ of detector temperatures;
Q post: long 3m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 object Haysep Q;
R post: long 2m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 object Haysep R;
5A post: long 2m, internal diameter 1/8 " stainless-steel tube, in-built 80～100 order 5A molecular sieve;
Detection system: select domestic thermal conductivity detector (TCD) (TCD) to detect the impurity content separating through piece-rate system, the average detected limit 50 × 10
-6.
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| CN201689079U (en) * | 2010-03-24 | 2010-12-29 | 上海宝钢工业检测公司 | Gas chromatography analysis device of natural gas compositions |
| CN201886002U (en) * | 2010-12-16 | 2011-06-29 | 大连中汇达科学仪器有限公司 | Gas analysis system |
| CN102621251A (en) * | 2011-01-31 | 2012-08-01 | 中国石油化工股份有限公司 | Trace helium, neon and hydrogen gas analysis method and device |
| CN102183610B (en) * | 2011-03-11 | 2013-06-05 | 苏州金宏气体股份有限公司 | Method for analyzing 7N electronic grade ultrapure ammonia |
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Address after: 215152 Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Jinhong Gas Co.,Ltd. Address before: 215143 No. 6 Anmin Road, Panyang Industrial Park, Huangduo Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee before: SUZHOU JINHONG GAS Co.,Ltd. |