CN100578215C - Open type natural gas generating kinetics research device and use method thereof - Google Patents
Open type natural gas generating kinetics research device and use method thereof Download PDFInfo
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- CN100578215C CN100578215C CN200710028545A CN200710028545A CN100578215C CN 100578215 C CN100578215 C CN 100578215C CN 200710028545 A CN200710028545 A CN 200710028545A CN 200710028545 A CN200710028545 A CN 200710028545A CN 100578215 C CN100578215 C CN 100578215C
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Abstract
The invention discloses a open-type natural gas generating dynamics research device and method, aims at providing a experiment device that structure is easy, reliability is high, operation is convenient, cost of analysis is low, the technique scheme includes high-pressure gas source, flow controller, sample pyrolyzer, several air vessels, vacuumized device and main controller, it controls hydrocarbon gas generated by sample in different temperature interval via valve transforming controller controlled by main controller to enter different air vessels, when course of storing gas of the first air vessel is over, gas phase chromatogram can be used to analyze component of gas on-line, and component of gas can be analyzed to determine the nature and quantitative analysis and carbon isotope and hydrogen/ deuterium isotope analysis, dynamics parameter generated by natural gas can obtained based on temperature heat simulating and corresponding gas stored in air vessels; the invention can be used in single constituent natural gas generating dynamics research.
Description
Technical field
The present invention relates to a kind of analysis of experiments technology, refer in particular to a kind of open type natural gas generating kinetics research device of single component rock gas hydrocarbon-generating dynamics research, the invention still further relates to the using method of said apparatus.
Background technology
At present, the home and abroad is not used in the commercialization instrument of single component rock gas hydrocarbon-generating dynamics research and sells, and a few studies mechanism utilizes homemade research device to study.The known online pyrolysis-isotope analysis method that has German geoscience research centre to be adopted.The principle of this method is, the hydrocarbon gas that pyrolysis produces is under the carrying of carrier gas, conversion by six-way valve, intermittently enter isotope mass spectrometry analysis, its advantage is to have omitted cold-trap, and shortcoming is that structure is comparatively complicated, the switching of each valve needs programmed control, the peripherals of pyrolysis and the gas circuit of isotope mass spectrometry are connected as a single entity, and need necessarily transform isotope mass spectrometry, have influenced the versatility of isotope mass spectrometry to a certain extent.In addition, because in different pyrolysis phase, the quantity and the composition of the hydro carbons that pyrolysis produces have very big difference, for the hydrocarbon gas to variable concentrations can both reach the desired concentration of on-line analysis, require isotope mass spectrometry to have the stability and the very wide range of linearity of height.It is reported that because the methane concentration of on-line analysis is low excessively, analytical error is up to 1.5 ‰.And the concentration of ethane and propane does not reach and analyzes the least concentration that requires far below the concentration of methane, in fact can't do the isotope of ethane and propane.In addition, thermal simulation is carried out under normal pressure, differ greatly with natural geologic condition, thereby its effect is restricted.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of simple in structure, reliability is high, easy for operation, open type natural gas generating kinetics research device that analysis cost is low.
Another technical matters that the present invention will solve provides the using method of said apparatus.
Last technical scheme of the present invention is such: a kind of open type natural gas generating kinetics research device, comprise high-pressure air source, flow controller, sample pyrolysis apparatus, a plurality of gas-holder, vacuum extractor and primary controller, high-pressure air source pipeline connection traffic controller, the flow controller pipeline connects the sample pyrolysis apparatus, wherein said sample pyrolysis apparatus is connected with a plurality of gas-holder by air inlet pipeline respectively, gas-holder is connected by the gas chromatography of outlet pipe with the analytical gas composition respectively, and each gas-holder is equipped with air intake control valve and leaving air control valve; Vacuum extractor connects sample pyrolysis apparatus and gas-holder by pipeline; Primary controller connects the sample pyrolysis apparatus by heating and temperature control device circuit, and primary controller connects each air intake control valve and leaving air control valve by valve switching controller circuit, and primary controller connects vacuum extractor by vacuum display controller circuit.
Back of the present invention one technical scheme is such: a kind of using method of open type natural gas generating kinetics research device is characterized in that comprising the steps: that (1) is placed on kerogen sample to be analyzed in the sample pyrolysis apparatus; (2) starting vacuum extractor vacuumizes system; (3) start heating and temperature control control sample pyrolysis apparatus and rise to 650 ℃ from room temperature with the heating rate of 2 ℃ of per minutes and 20 ℃, open high-pressure air source simultaneously, and the hydrocarbon gas in different temperatures stage is carried by carrier gas enter successively in the different gas-holder; (4) after the gas storage process of first gas-holder finishes, promptly begin to carry out the gas componant on-line analysis, or take out gas with gastight syringe and carry out the carbon isotope and the hydrogen/deuterium isotope analysis and the isotope analysis of the qualitative and quantitative analysis and the gas of gas componant by gas chromatography; (5) the gas storage process of all the other gas-holder is proceeded, and finishes until pyrolytic process; (6) output of hydrocarbon gas in the gas that is preserved in the temperature by thermal simulation and corresponding each gas-holder at last draws the kinetic parameter that rock gas generates.
Air pressure in the step described in the using method of above-mentioned open type natural gas generating kinetics research device (3) in the gas-holder is lower than an atmospheric pressure all the time.
The present invention is the pressing open type natural gas generating kinetics research device, under major part nature geologic condition, the generation of rock gas is under the open or semi-open condition, the present invention is the simulating nature geologic condition farthest, draw rational natural gas generating kinetics parameter, and be used for the generation forecast assessment of rock gas, be the production active service.Compared with prior art, have following advantage:
(1) adopt gases at high pressure both as carrier gas and pressure source that sample is exerted pressure, simulating nature geologic condition as much as possible, make experimental data more accurately, have more actual reference.
(2) Zhuan Zhi good reliability, the automaticity height behind the sample of packing into, can be finished the dynamic analysis of gas componant automatically.
(3) can analyze all hydrocarbon gas and H
2, H
2The kinetic parameter of inorganic gas such as S by the gas concentration unit of off-line, can be analyzed the isotopic power mathematic(al) parameter of the methane of protolith of low organic carbon and ethane, propane.
(4) need not to use liquid nitrogen under the general condition, use cost reduces, simplified control.
(5) cooperate the isotope instrument, once experiment can be done the isotope analysis of the hydrocarbon-generating dynamics of all components and carbon, hydrogen/deuterium simultaneously.
Description of drawings
Below in conjunction with the specific embodiment in the accompanying drawing the present invention is described in further detail, but does not constitute any limitation of the invention.
Fig. 1 is the structural representation of a kind of specific embodiment of the present invention;
Among the figure: high-pressure air source 1, flow controller 2, sample pyrolysis apparatus 3, gas-holder 4, vacuum extractor 5, primary controller 6, gas chromatography 7, air intake control valve 8, leaving air control valve 9, heating and temperature control device 10, valve switching controller 11, vacuum display controller 12.
Embodiment
Consult shown in Figure 1, a kind of open type natural gas generating kinetics research device of the present invention, comprise high-pressure air source 1, flow controller 2, sample pyrolysis apparatus 3, ten gas-holder 4, vacuum extractor 5 and primary controllers 6, high-pressure air source 1 pipeline connection traffic controller 2, flow controller 2 pipelines connect sample pyrolysis apparatus 3, high-pressure air source 1 is to reach the pressure source that sample is exerted pressure, simulating nature geologic condition as much as possible as carrier gas; Sample pyrolysis apparatus 3 is connected with ten gas-holder 4 by air inlet pipeline respectively, and gas-holder 4 is connected with the gas chromatography 7 of analytical gas composition by outlet pipe respectively, and each gas-holder 4 is equipped with air intake control valve 8 and leaving air control valve 9; Vacuum extractor 5 connects sample pyrolysis apparatus 3 and gas-holder 4 by pipeline; Primary controller 6 connects sample pyrolysis apparatus 3 by heating and temperature control device 10 circuit, and primary controller 6 connects each air intake control valve 8 and leaving air control valve 9 by valve switching controller 11 circuit, and primary controller 6 connects vacuum extractor 5 by vacuum display controller 12 circuit.
Principle of work of the present invention and using method are as follows:
(1) the kerogen sample is placed in the sample pyrolysis apparatus 3.
(2) starting 5 pairs of systems of vacuum extractor vacuumizes.
(3) start heating and temperature control device 10 control sample pyrolysis apparatus 3 and rise to 650 ℃ from room temperature, open high-pressure air source 1 simultaneously with the heating rate of 2 ℃ of per minutes and 20 ℃; The kerogen sample is subjected to thermogenetic hydrocarbon gas, carried by carrier gas and to enter gas-holder 4, switch by valve switching controller 11, the air intake control valve of controlling on the different gas-holder 48 (solenoid valve) opens or closes, the hydrocarbon gas in different temperatures stage is entered in the different gas-holder 4 successively, the air-flow of a time sample pyrolysis apparatus 3 in office only is communicated with a gas-holder 4; By suitable calculating carrier gas flux and pyrolysis time, make the air pressure in the gas-holder 4 be lower than an atmospheric pressure all the time.
(4) after the gas storage process of first gas-holder finishes, can carry out gas componant and isotope analysis, the gas chromatography 7 of analytical gas composition and gas-holder 4 switch by valve switching controller 11, leaving air control valve 9 (solenoid valve) on the gas-holder 4 is opened, directly be communicated with, carry out the on-line analysis of gas componant automatically with gas chromatography 7; Take out gas with the air hatch of gastight syringe by gas-holder 4 tops then and carry out the carbon isotope and the hydrogen/deuterium isotope analysis of the qualitative and quantitative analysis and the gas of gas componant.。
(5) the gas storage process of all the other gas-holder 4 is proceeded, and finishes until pyrolytic process; The total system procedure auto-control, the experiment of finishing a sample needs 10 hours approximately.
(6) output of hydrocarbon gas in the gas that is preserved in the temperature by thermal simulation and corresponding each gas-holder 4 at last calculates the kinetic parameter that rock gas generates by specific program.
Claims (3)
1. open type natural gas generating kinetics research device, comprise high-pressure air source (1), flow controller (2), sample pyrolysis apparatus (3), a plurality of gas-holder (4), vacuum extractor (5) and primary controller (6), high-pressure air source (1) pipeline connection traffic controller (2), flow controller (2) pipeline connects sample pyrolysis apparatus (3), it is characterized in that described sample pyrolysis apparatus (3) is connected with a plurality of gas-holder (4) by air inlet pipeline respectively, gas-holder (4) is connected with the gas chromatography (7) of analytical gas composition by outlet pipe respectively, and each gas-holder (4) is equipped with air intake control valve (8) and leaving air control valve (9); Vacuum extractor (5) connects sample pyrolysis apparatus (3) and gas-holder (4) by pipeline; Primary controller (6) connects sample pyrolysis apparatus (3) by heating and temperature control device (10) circuit, primary controller (6) connects each air intake control valve (8) and leaving air control valve (9) by valve switching controller (11) circuit, and primary controller (6) connects vacuum extractor (5) by vacuum display controller (12) circuit.
2. the using method of the described open type natural gas generating kinetics research device of claim 1 is characterized in that comprising the steps: that (1) is placed on kerogen sample to be analyzed in the sample pyrolysis apparatus; (2) starting vacuum extractor vacuumizes system; (3) start heating and temperature control control sample pyrolysis apparatus and rise to 650 ℃ from room temperature with the heating rate of 2 ℃ of per minutes or 20 ℃, open high-pressure air source simultaneously, and the hydrocarbon gas in different temperatures stage is carried by carrier gas enter successively in the different gas-holder; (4) after the gas storage process of first gas-holder finishes, promptly begin to carry out the gas componant on-line analysis, or take out gas with gastight syringe and carry out the carbon isotope and the hydrogen/deuterium isotope analysis and the isotope analysis of the qualitative and quantitative analysis and the gas of gas componant by gas chromatography; (5) the gas storage process of all the other gas-holder is proceeded, and finishes until pyrolytic process; (6) output of hydrocarbon gas in the gas that is preserved in the temperature by thermal simulation and corresponding each gas-holder at last draws the kinetic parameter that rock gas generates.
3. the using method of open type natural gas generating kinetics research device according to claim 2 is characterized in that the air pressure in the gas-holder is lower than an atmospheric pressure all the time in the described step (3).
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| CN200710028545A CN100578215C (en) | 2007-06-12 | 2007-06-12 | Open type natural gas generating kinetics research device and use method thereof |
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| CN200710028545A CN100578215C (en) | 2007-06-12 | 2007-06-12 | Open type natural gas generating kinetics research device and use method thereof |
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| CN100578215C true CN100578215C (en) | 2010-01-06 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101270295B (en) * | 2008-04-29 | 2011-11-09 | 中国科学院广州地球化学研究所 | Accurate temperature control thermal decomposition apparatus for open type hydrocarbon producing kinetics research |
| CN102139193B (en) * | 2011-01-19 | 2014-02-26 | 中国科学院广州地球化学研究所 | Full automatic high-pressure hydrogenation thermal cracking device for geochemistry research |
| CN107178789B (en) * | 2016-03-09 | 2020-06-09 | 西门子公司 | Combustion monitoring method, device and system of natural gas combustor |
| CN108469490B (en) * | 2018-03-20 | 2020-05-15 | 中国科学院广州地球化学研究所 | Automatic analysis device for components and carbon isotopes of gas in thermal simulation gold tube of hydrocarbon source rock |
| CN109374367A (en) * | 2018-12-21 | 2019-02-22 | 中国人民解放军空军工程大学 | Multichannel large capacity high-temperature vacuum sampler |
| CN113777177B (en) * | 2020-06-09 | 2024-03-26 | 中国石油天然气股份有限公司 | System and method for detecting sulfur compounds in gas |
| CN114487228B (en) * | 2022-02-08 | 2024-01-23 | 河南省科学院 | Pyrolysis gas or gasification gas automatic storage and detection system and method |
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| JP2000162369A (en) * | 1998-11-30 | 2000-06-16 | Hitachi Ltd | Neutron irradiation material inspection system |
| CN1301346A (en) * | 1998-05-15 | 2001-06-27 | 福特姆石油天然气有限公司 | Arrangement equipment and method for testing heterogeneous catalyst for short contact time reactions |
| CN1335499A (en) * | 2000-07-25 | 2002-02-13 | 海城市石油化工仪器厂 | Quantitative analysis device for oil bearing component generated through rock pyrolysis |
| CN1735676A (en) * | 2002-12-23 | 2006-02-15 | 国际壳牌研究有限公司 | Apparatus and method for determining and controlling the hydrogen-to-carbon ratio of a pyrolysis |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1301346A (en) * | 1998-05-15 | 2001-06-27 | 福特姆石油天然气有限公司 | Arrangement equipment and method for testing heterogeneous catalyst for short contact time reactions |
| JP2000162369A (en) * | 1998-11-30 | 2000-06-16 | Hitachi Ltd | Neutron irradiation material inspection system |
| CN1335499A (en) * | 2000-07-25 | 2002-02-13 | 海城市石油化工仪器厂 | Quantitative analysis device for oil bearing component generated through rock pyrolysis |
| CN1735676A (en) * | 2002-12-23 | 2006-02-15 | 国际壳牌研究有限公司 | Apparatus and method for determining and controlling the hydrogen-to-carbon ratio of a pyrolysis |
Non-Patent Citations (1)
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| 天然气生成动力学模拟及其地质应用. 张海祖，耿安松，熊永强，王铜山，刘金钟.天然气工业，第26卷第2期. 2006 * |
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