CN212514443U - Gas chromatography detection system for analyzing hydrocarbon impurities and trace gas in propylene - Google Patents
Gas chromatography detection system for analyzing hydrocarbon impurities and trace gas in propylene Download PDFInfo
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- CN212514443U CN212514443U CN202021329599.0U CN202021329599U CN212514443U CN 212514443 U CN212514443 U CN 212514443U CN 202021329599 U CN202021329599 U CN 202021329599U CN 212514443 U CN212514443 U CN 212514443U
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Abstract
The utility model belongs to the technical field of gaseous detection, concretely relates to a gas chromatography detecting system for hydrocarbon impurity and trace gas in analysis propylene, including hydrogen cylinder, nitrogen cylinder, first quantitative pipe, six-way valve, first ten logical valve, second quantitative pipe, first chromatographic column, second chromatographic column, third chromatographic column, twenty-way valve, third quantitative pipe, fourth chromatographic column, fifth chromatographic column, nickel reborner, thermal conductivity cell detector, back hydrogen flame ionization detector and preceding hydrogen flame ionization detector. The utility model discloses can realize once advancing analysis analyses such as hydrocarbon impurity and trace carbon monoxide, carbon dioxide and oxygen in the appearance analysis propylene, easy operation, the expense is low, and the analysis is quick, and the accuracy is high, and good repeatability adopts the blowback device simultaneously, has improved the life of chromatographic column, has avoided the carbon deposit of nickel reborner.
Description
Technical Field
The utility model belongs to the technical field of gaseous detection, concretely relates to a gas chromatography detecting system for hydrocarbon impurity and trace gas in analysis propylene.
Background
The polypropylene production industry puts high requirements on the purity of propylene monomers, trace impurities have great influence on polymerization reaction, wherein when carbon monoxide, carbon dioxide, oxygen and the like exceed standards, the activity and the orientation capability of a catalyst are influenced, the yield of polypropylene is reduced, and the quality is poor. Usually, three chromatographs are needed to detect hydrocarbon impurities, carbon monoxide, carbon dioxide and oxygen in propylene respectively, the detection is time-consuming and labor-consuming, and errors are easily introduced.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is: the gas chromatography detection system for analyzing the hydrocarbon impurities and trace gas in the propylene can analyze the hydrocarbon impurities and trace carbon monoxide, carbon dioxide and oxygen in the propylene by one-time sample injection, and has the advantages of simple operation, low cost, quick analysis, high accuracy and good repeatability.
The utility model discloses an adopt following technical scheme to realize:
the gas chromatography detection system for analyzing hydrocarbon impurities and trace gases in propylene comprises a hydrogen cylinder, a nitrogen cylinder, a first quantitative tube, a six-way valve, a first ten-way valve, a second quantitative tube, a first chromatographic column, a second chromatographic column, a third chromatographic column, an twenty-way valve, a third quantitative tube, a fourth chromatographic column, a fifth chromatographic column, a nickel conversion furnace, a thermal conductivity cell detector, a rear hydrogen flame ionization detector and a front hydrogen flame ionization detector;
the 1 st interface of the six-way valve is a sample inlet, the two ends of the first quantitative tube are respectively connected with the 3 rd interface and the 6 th interface of the six-way valve, the 4 th interface of the six-way valve is connected with the nitrogen cylinder, one end of the first chromatographic column is connected with the 5 th interface of the six-way valve, and the other end of the first chromatographic column is connected with the front hydrogen flame ionization detector;
the 2 nd interface of the six-way valve is connected with the 9 th interface of the first ten-way valve, the two ends of the second quantitative tube are respectively connected with the 8 th interface and the 1 st interface of the first ten-way valve, the hydrogen cylinder is respectively connected with the 7 th interface and the 4 th interface of the first ten-way valve, the two ends of the second chromatographic column are respectively connected with the 2 nd interface and the 5 th interface of the first ten-way valve, the 3 rd interface of the first ten-way valve is a back flushing port, one end of the third chromatographic column is connected with the 6 th interface of the first ten-way valve, and the other end of the third chromatographic column is connected with the thermal conductivity cell detector;
the 10 th interface of first ten logical valves and the 9 th interface connection of twentieth valve, the 8 th interface and the 1 st interface of twentieth valve are connected respectively to the both ends of third ration pipe, and the 10 th interface of twentieth valve is the air release, the 2 nd interface and the 5 th interface of twentieth valve are connected respectively to the both ends of fourth chromatographic column, the nitrogen cylinder respectively with the 7 th interface and the 4 th interface connection of twentieth valve, the 3 rd interface position blowback mouth of twentieth valve, the 6 th interface of twentieth valve is connected to the one end of fifth chromatographic column, the other end passes through the nickel reborner and is connected with back hydrogen flame ionization detector.
The first chromatographic column is an aluminum oxide capillary chromatographic column.
The second chromatographic column is a pre-column of a third chromatographic column, and the third chromatographic column is a molecular sieve packed column, preferably a 13X molecular sieve packed column.
The fourth chromatographic column is a pre-column of a fifth chromatographic column, and the fifth chromatographic column is a Porapak Q packed column.
The nickel converter is internally filled with hydrogen.
Compared with the prior art, the beneficial effects of the utility model are as follows:
the utility model discloses can realize once advancing analysis analyses such as hydrocarbon impurity and trace carbon monoxide, carbon dioxide and oxygen in the appearance analysis propylene, easy operation, the expense is low, and the analysis is quick, and the accuracy is high, and good repeatability adopts the blowback device simultaneously, has improved the life of chromatographic column, has avoided the carbon deposit of nickel reborner.
Drawings
FIG. 1 is a schematic view of the sampling process of the present invention;
FIG. 2 is a schematic view of the sample injection process of the present invention;
in the figure: 1. a hydrogen gas cylinder; 2. a nitrogen gas cylinder; 3. a first dosing tube; 4. a six-way valve; 5. a first ten-way valve; 6. a second dosing tube; 7. a first chromatographic column; 8. a third chromatographic column; 9. a second chromatography column; 10. a thermal conductivity cell detector; 11. a post-hydrogen flame ionization detector; 12. a nickel reformer; 13. a pre-hydrogen flame ionization detector; 14. a fifth chromatographic column; 15. a fourth chromatographic column; 16. a twentieth valve; 17. a third dosing tube.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
As shown in fig. 1-2, the gas chromatography detection system for analyzing hydrocarbon impurities and trace gases in propylene includes a hydrogen cylinder 1, a nitrogen cylinder 2, a first quantitative tube 3, a six-way valve 4, a first ten-way valve 5, a second quantitative tube 6, a first chromatographic column 7, a second chromatographic column 9, a third chromatographic column 8, a twentieth-way valve 16, a third quantitative tube 17, a fourth chromatographic column 15, a fifth chromatographic column 14, a nickel conversion furnace 12, a thermal conductivity cell detector 10, a rear hydrogen flame ionization detector 11, and a front hydrogen flame ionization detector 13;
the 1 st interface of the six-way valve 4 is a sample inlet, the two ends of the first quantitative pipe 3 are respectively connected with the 3 rd interface and the 6 th interface of the six-way valve 4, the 4 th interface of the six-way valve 4 is connected with the nitrogen cylinder 2, one end of the first chromatographic column 7 is connected with the 5 th interface of the six-way valve 4, and the other end is connected with the front hydrogen flame ionization detector 13;
a 2 nd interface of the six-way valve 4 is connected with a 9 th interface of the first ten-way valve 5, two ends of the second quantitative tube 6 are respectively connected with an 8 th interface and a 1 st interface of the first ten-way valve 5, the hydrogen cylinder 1 is respectively connected with a 7 th interface and a 4 th interface of the first ten-way valve 5, two ends of the second chromatographic column 9 are respectively connected with the 2 nd interface and the 5 th interface of the first ten-way valve 5, a 3 rd interface of the first ten-way valve 5 is a back flushing port, one end of the third chromatographic column 8 is connected with a 6 th interface of the first ten-way valve 5, and the other end of the third chromatographic column is connected with the thermal conductivity cell detector 10;
the 10 th interface of first ten logical valve 5 and the 9 th interface connection of twentieth logical valve 16, the 8 th interface and the 1 st interface of twentieth logical valve 16 are connected respectively to the both ends of third ration pipe 17, and the 10 th interface of twentieth logical valve 16 is the drain, the 2 nd interface and the 5 th interface of twentieth logical valve 16 are connected respectively to the both ends of fourth chromatographic column 15, nitrogen cylinder 2 respectively with the 7 th interface and the 4 th interface connection of twentieth logical valve 16, the 3 rd interface position blowback mouth of twentieth logical valve 16, the 6 th interface of twentieth logical valve 16 is connected to the one end of fifth chromatographic column 14, the other end passes through nickel converting furnace 12 and is connected with back hydrogen flame ionization detector 11.
The first chromatographic column 7 is an aluminum oxide capillary chromatographic column.
The second chromatographic column 9 is a pre-column of the third chromatographic column 8, and the third chromatographic column 8 is a molecular sieve packed column.
The fourth chromatographic column 15 is a pre-column of the fifth chromatographic column 14, and the fifth chromatographic column 14 is a Porapak Q packed column.
The nickel converter 12 is internally filled with hydrogen.
The analysis principle and the process are as follows:
as shown in fig. 1, the six-way valve 4, the first ten-way valve 5 and the twenty-way valve 16 are all in a sampling state, a gas sample is introduced through a sample inlet of a 1 st interface of the six-way valve 4, the gas sample sequentially enters the first quantitative tube 3, the second quantitative tube 5 and the third quantitative tube 17, after sampling, as shown in fig. 2, sample introduction analysis is performed, and an analysis flow is as follows:
flow path A: the gas sample is switched by the six-way valve 4, and the gas sample is carried into the first chromatographic column 7 by the nitrogen carrier gas2O3) The capillary column is used for detecting the hydrocarbon impurities in the propylene by a hydrogen flame ionization detector 13 (FID).
Flow path B: the gas sample is switched through the twentieth valve 16, the gas sample is carried into the fourth chromatographic column 15 chromatographic column pre-column by nitrogen carrier gas, firstly, carbon monoxide and carbon dioxide are separated from other components and then enter the fifth chromatographic column 14Porapak Q packed column, then the gas sample is switched through the twentieth valve 16, the carbon monoxide and the carbon dioxide are separated through the fifth chromatographic column 14, the carbon monoxide and the carbon dioxide are converted into methane through catalytic hydrogenation of the nickel converter 12, and then the contents of the carbon monoxide and the carbon dioxide in propylene are detected through the hydrogen flame ionization detector 11 (FID). Meanwhile, the impurities such as hydrocarbon and the like are blown out from the fourth chromatographic column 15 chromatographic column pre-column through the 3 rd interface blowback port of the twenty-first valve 16 through blowback, so that carbon deposition caused by entering the nickel converter 12 is avoided.
Flow path C: the gas sample is switched by the first ten-way valve 5, the gas sample is carried into the second chromatographic column 9 by hydrogen carrier gas, firstly, oxygen is separated from other hydrocarbon components and then enters the third chromatographic column 813X molecular sieve chromatographic column, then the gas sample is switched by the first ten-way valve 5, the oxygen is separated by the 13X molecular sieve chromatographic column, and the content of the oxygen in the propylene is detected by the thermal conductivity cell detector 10 (TCD). Meanwhile, the impurities such as hydrocarbon and the like are blown out from the second chromatographic column 9 chromatographic column pre-column through the 3 rd interface blowback port of the first ten-way valve 5 through blowback so as to prevent the permanent inactivation of the molecular sieve.
Of course, the above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the embodiments of the present invention. The present invention is not limited to the above examples, and the technical field of the present invention is equivalent to the changes and improvements made in the actual range of the present invention, which should be attributed to the patent coverage of the present invention.
Claims (5)
1. A gas chromatography detecting system for analyzing hydrocarbon impurities and trace gas in propylene is characterized in that: the device comprises a hydrogen cylinder (1), a nitrogen cylinder (2), a first quantitative tube (3), a six-way valve (4), a first ten-way valve (5), a second quantitative tube (6), a first chromatographic column (7), a second chromatographic column (9), a third chromatographic column (8), a twenty-way valve (16), a third quantitative tube (17), a fourth chromatographic column (15), a fifth chromatographic column (14), a nickel converter (12), a thermal conductivity cell detector (10), a rear hydrogen flame ionization detector (11) and a front hydrogen flame ionization detector (13);
the 1 st interface of the six-way valve (4) is a sample inlet, the two ends of the first quantitative tube (3) are respectively connected with the 3 rd interface and the 6 th interface of the six-way valve (4), the 4 th interface of the six-way valve (4) is connected with the nitrogen gas cylinder (2), one end of the first chromatographic column (7) is connected with the 5 th interface of the six-way valve (4), and the other end of the first chromatographic column is connected with the front hydrogen flame ionization detector (13);
a 2 nd interface of the six-way valve (4) is connected with a 9 th interface of the first ten-way valve (5), two ends of the second quantitative tube (6) are respectively connected with an 8 th interface and a 1 st interface of the first ten-way valve (5), the hydrogen cylinder (1) is respectively connected with a 7 th interface and a 4 th interface of the first ten-way valve (5), two ends of the second chromatographic column (9) are respectively connected with a 2 nd interface and a 5 th interface of the first ten-way valve (5), a 3 rd interface of the first ten-way valve (5) is a back flushing port, one end of the third chromatographic column (8) is connected with the 6 th interface of the first ten-way valve (5), and the other end of the third chromatographic column is connected with the thermal conductivity cell detector (10);
the 10 th interface of first ten logical valve (5) and the 9 th interface connection of twentieth valve (16), the 8 th interface and the 1 st interface of twentieth valve (16) are connected respectively to the both ends of third ration pipe (17), the 10 th interface of twentieth valve (16) is the drain, the 2 nd interface and the 5 th interface of twentieth valve (16) are connected respectively to the both ends of fourth chromatographic column (15), nitrogen gas bottle (2) are respectively with the 7 th interface and the 4 th interface connection of twentieth valve (16), the 3 rd interface position blowback mouth of twentieth valve (16), the 6 th interface of twentieth valve (16) is connected to the one end of fifth chromatographic column (14), the other end passes through nickel converter (12) and is connected with back hydrogen flame ionization detector (11).
2. The gas chromatography detection system for analyzing hydrocarbon impurities and trace gases in propylene as claimed in claim 1, wherein: the first chromatographic column (7) is an aluminum oxide capillary chromatographic column.
3. The gas chromatography detection system for analyzing hydrocarbon impurities and trace gases in propylene as claimed in claim 1, wherein: the second chromatographic column (9) is a pre-column of a third chromatographic column (8), and the third chromatographic column (8) is a molecular sieve packed column.
4. The gas chromatography detection system for analyzing hydrocarbon impurities and trace gases in propylene as claimed in claim 1, wherein: the fourth chromatographic column (15) is a pre-column of a fifth chromatographic column (14), and the fifth chromatographic column (14) is a Porapak Q packed column.
5. The gas chromatography detection system for analyzing hydrocarbon impurities and trace gases in propylene as claimed in claim 1, wherein: hydrogen is introduced into the nickel converter (12).
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112986447A (en) * | 2021-04-23 | 2021-06-18 | 中国原子能科学研究院 | Gas chromatography device |
CN115201386A (en) * | 2022-07-08 | 2022-10-18 | 昆明摩创科技有限公司 | Gas chromatography catalytic combustion ionization and hot wire detection system and method |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112986447A (en) * | 2021-04-23 | 2021-06-18 | 中国原子能科学研究院 | Gas chromatography device |
CN115201386A (en) * | 2022-07-08 | 2022-10-18 | 昆明摩创科技有限公司 | Gas chromatography catalytic combustion ionization and hot wire detection system and method |
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