CN206832715U - A kind of hydrocarbon source rock organic carbon pyrolysis analysis device - Google Patents

A kind of hydrocarbon source rock organic carbon pyrolysis analysis device Download PDF

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CN206832715U
CN206832715U CN201720603290.8U CN201720603290U CN206832715U CN 206832715 U CN206832715 U CN 206832715U CN 201720603290 U CN201720603290 U CN 201720603290U CN 206832715 U CN206832715 U CN 206832715U
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gas
pyrolysis
unit
oxidation
component
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张小涛
汪双清
沈斌
秦婧
孙玮琳
徐学敏
黄春华
杨佳佳
芦苒
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STATE GEOLOGY EXPERIMENT AND TEST CENTER
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Abstract

A kind of hydrocarbon source rock organic carbon pyrolysis analysis device, including pyrolysis unit, oxidation unit, clean unit, detection unit, control process unit;Pyrolysis unit includes the first temperature control chamber and pyrolysis oven, oxidation unit includes the second temperature control chamber and oxidation tube, moisture of the clean unit including gas cooling chamber and series connection dispels component, solid particle dispels component, and detection unit includes detector and is resident chamber and the infrared detector of inside;First temperature control chamber one end is connected by gas pipeline with gas circuit change-over switch, and the other end is connected by the inlet end of gas path pipe and oxidation tube;Gas circuit change-over switch connects helium pipeline and oxygen channel respectively;Oxygen channel is additionally provided with the oxygen manifold with air circuit breaker, and oxygen manifold is also connected to the inlet end of oxidation tube;The inlet end that the outlet side of oxidation tube dispels component by gas pipeline with moisture is connected;Solid particle dispels the outlet side of component and the inlet end of infrared detector connects, the outlet side of infrared detector and atmosphere.

Description

A kind of hydrocarbon source rock organic carbon pyrolysis analysis device
Technical field
The utility model belongs to oil-gas exploration and development technical field, and in particular to organic matter abundance in hydrocarbon source rock determines, and is one Kind forms the device for implementing analysis test to the organic carbon content (TOC) and its organic matter of hydrocarbon source rock, suitable for general thermal evolution Degree to the rock pyrolysis Parameter analysis of high evolution level mud shale determines with TOC.
Background technology
The organic carbon content of hydrocarbon source rock is the basic Geochemical Parameters for evaluating its petroleum geologic conditions.Rock pyrolysis point Analysis is to obtain the basic fundamental means of hydrocarbon primary rock producing hydrocarbon potentiality parameter, while is also a kind of fast of acquisition content of organic carbon of hydrocarbon source rock Speed, economic method, for working well for general maturity hydrocarbon source rock.For source rocks in high maturity, it is necessary to 750 DEG C- 800 DEG C of pyrolysis temperature could realize its kerogenic complete thermal cracking, therefore measured by traditional 600 DEG C of highest pyrolysis temperatures Rock pyrolysis analysis data can not reflect its real hydrocarbon potentiality, pyrolysed hydrocarbon (S2) parameter value is seriously less than normal while also straight Connecing causes organic carbon content and direct measured value deviation that empirically formula pyrolysis parameters of rock calculates serious.However, current The highest pyrolysis temperature of domestic rock pyrolysis analysis instrument can only achieve 600 DEG C, for high maturity hydrocarbon source rock France can only be used raw The external instrument such as the rock pyrolysis analysis instrument of Rock-Eval VI of production carries out pyrolysis analysis.Foreign rock pyrolysis instrument not only hold high by price It is expensive, and poor durability, parts are fragile, specificity is very strong, made troubles to maintenance, and maintenance promptness rate is very poor.China's page The main object of rock gas exploration exploitation is that evolution level reaches the high ripe mud shale to the post-mature stage, however, it is current this Kind of equipment and technology status prevent rock pyrolysis analysis, and this is economical, efficiently technological means is from effectively serving in China's shale The work of exploration and development of the contour evolution petroleum resources of gas, have impact on operating efficiency.
Utility model content
In view of the above problems, the purpose of this utility model is to provide a kind of hydrocarbon source rock organic carbon pyrolysis analysis device, and it is most High pyrolysis temperature is high, can be applied to general evolution level to the organic carbon analysis of high evolution level mud shale.
To achieve the above object, the utility model takes following technical scheme:
A kind of hydrocarbon source rock organic carbon pyrolysis analysis device, the pyrolysis unit, oxidation unit, purification that it includes being sequentially connected are single Member, detection unit, and the operation for device and control, the control process unit of data acquisition and procession;
The pyrolysis unit includes the first temperature control chamber and internal pyrolysis oven, and the armouring that the pyrolysis oven includes 1000 DEG C of heatproof adds Heated filament;The oxidation unit includes the second temperature control chamber and internal oxidation tube, and the second temperature control chamber includes the armouring of 1000 DEG C of heatproof Heater strip;The clean unit includes gas cooling chamber and internal moisture dispels component and solid particle dispels component, the moisture Dispel component and solid particle dispels component series connection and is placed in gas cooling intracavitary;The detection unit include detector be resident chamber and Internal infrared detector;
The first temperature control chamber one end is connected by gas pipeline with gas circuit change-over switch, and the other end is by gas path pipe with being somebody's turn to do The inlet end connection of oxidation tube;The gas circuit change-over switch connects helium pipeline and oxygen channel respectively;The oxygen channel is additionally provided with Oxygen manifold with air circuit breaker, the oxygen manifold are also connected to the inlet end of the oxidation tube;The outlet side of the oxidation tube passes through The inlet end that gas pipeline dispels component with the moisture is connected;The solid particle dispels outlet side and infrared detector of component Inlet end connection, the outlet side of the infrared detector and atmosphere.
Further, the control process unit passes through sensor and digital communications ports and the pyrolysis unit, oxidation Unit, clean unit, detection unit connection.
Further, it is equipped with flow stabilizing valve on oxygen channel and the helium pipeline.
Further, the oxygen channel connects source of oxygen or air-source, and the helium pipeline connects helium gas source.
Further, the control process unit is computer.
The beneficial effects of the utility model are:The highest pyrolysis temperature of the utility model device reaches 850 DEG C, it is possible to achieve The kerogenic complete thermal cracking of source rocks in high maturity, and by the way that conventional rock pyrolysis instrument is pyrolyzed for each pyrolysis temperature stage The hydrogen flame ion signal detection (FID) of product is changed into the detection for its carbon signal so that test data directly embodies hydrocarbon The organic carbon content (TOC) of source rock, without being calculated by empirical equation, avoid because the mistake that properties of samples difference is brought Difference;Meanwhile the philosophy and technique method based on hydrocarbon source rock rock pyrolysis analysis, the rock pyrolysis parameter of the utility model device can To be corresponded with the rock pyrolysis parameter of conventional rock pyrolysis instrument, possess the analysis test function of conventional rock pyrolysis instrument, because And hydrocarbon primary rock producing hydrocarbon potentiality parameter can be obtained.
Brief description of the drawings
Fig. 1 is the structural framing schematic diagram of the utility model hydrocarbon source rock organic carbon pyrolysis analysis device.
Embodiment
Specific embodiment of the present utility model is further illustrated below in conjunction with the accompanying drawings.
As shown in figure 1, the utility model provides a kind of hydrocarbon source rock organic carbon pyrolysis analysis device, it includes what is be sequentially connected Pyrolysis unit, oxidation unit, clean unit, detection unit, and operation for device and control, data acquisition and procession Control process unit 15.The control process unit 15 passes through sensor and the pyrolysis unit, oxidation unit, clean unit, detection Unit connects.
The pyrolysis unit, which includes the first temperature control chamber 1 and internal pyrolysis oven 2, the pyrolysis oven 2, includes the armour of 1000 DEG C of heatproof Fill heater strip.The oxidation unit, which includes the second temperature control chamber 3 and internal oxidation tube 4, the second temperature control chamber 3, includes 1000 DEG C of heatproof Armouring heater strip.The clean unit includes gas cooling chamber 5 and internal moisture dispels component 6 and solid particle dispels component 7, the moisture dispels component 6 and solid particle is dispelled the series connection of component 7 and is placed in gas cooling chamber 5.The detection unit includes inspection Survey device and be resident chamber 8 and the infrared detector 9 of inside.
The one end of first temperature control chamber 1 is connected by gas pipeline with gas circuit change-over switch 10, and the other end passes through gas path pipe It is connected with the inlet end of the oxidation tube 4.The gas circuit change-over switch 10 connects helium pipeline 11 and oxygen channel 12, the oxygen respectively Pipeline 12 connects source of oxygen or air-source, and the helium pipeline 11 connects helium gas source, distinguishes on helium pipeline 11 and the oxygen channel 12 Provided with flow stabilizing valve A, flow stabilizing valve B.The oxygen channel 12 is additionally provided with the oxygen manifold 14 with air circuit breaker 13, the oxygen manifold 14 It is connected to the inlet end of the oxidation tube 4.The air inlet of component 6 is dispelled by gas pipeline and the moisture in the outlet side of the oxidation tube 4 End connection.The outlet side that the solid particle dispels component 7 is connected with the inlet end of the infrared detector 9, the infrared detector 9 Outlet side and atmosphere.
Rock sample is in pyrolysis oven 2 as volatilization, evaporation and thermal cracking, life occur for the rising of the temperature of the first temperature control chamber 1 Into some gaseous states, the hydro carbons of liquid.Meanwhile the helium of fixed flow rate is under flow stabilizing valve A control, via gas circuit change-over switch 10, pyrolysis oven 2 is entered by gas pipeline;After maximum temperature of the temperature stabilization in setting of pyrolysis oven 2, switching gas circuit conversion Switch 10, cut-out helium supply, allows oxygen (or air) to enter under flow stabilizing valve B control to set flow velocity by gas pipeline Enter pyrolysis oven 2, remnant organic matter is flowed down complete oxidation in air (or oxygen);So simultaneously, air circuit breaker 13 is closed.In heat The gaseous hydrocarbon that generates and liquefied hydrocarbon enter oxidation tube 4 under the drive of helium stream by gas pipeline in solution stove 2, with via Flow stabilizing valve B, air circuit breaker 13, setting flow velocity oxygen (or air) the stream mixing of oxygen manifold 14, provided in the second temperature control chamber 3 CO is oxidized at a temperature of 600 DEG C to 800 DEG C2.The CO generated in oxidation tube 4 and pyrolysis oven 22With water under the drive of helium stream, Enter gas by gas pipeline to cool chamber 5, pass sequentially through that moisture dispels component 6 and solid particle dispels component 7, dispel wherein Solid particle and water.Contain CO after purified2Gas enters detector by gas pipeline and is resident chamber 8, by infrared detector 9 Detection.Standard substance is analyzed, sample is carried out on the basis of being calibrated with the parameter value of standard substance to test data The integrated treatment of product data, obtain the value of its S0, S1, S2, S4, TOC indices parameter.
The utility model also provides a kind of method that hydrocarbon source rock organic carbon pyrolysis analysis is carried out using above-mentioned analytical equipment, tool For body, it comprises the following steps:
(1) organic matter is pyrolyzed
Open helium pipeline 11 and oxygen channel 12, the output pressure in the helium pipeline 11 and oxygen channel 12 is 0.5MPa;Gas circuit change-over switch 10 is adjusted, helium is passed through the first temperature control chamber 1;Set the heating schedule and of the first temperature control chamber 1 The temperature of two temperature control chamber 3;The source rock sample powder below the mesh of 100~120mg granularities 200 is weighed, is placed in pyrolysis oven 2;50 DEG C in 800 DEG C of temperature ranges, the temperature of pyrolysis oven 2 is controlled with staged temperature-programmed mode, is made organic in source rock sample Volatilization, evaporation and thermal cracking occur successively under helium stream for matter, and after the completion of thermal cracking, regulation gas circuit change-over switch 10, make Oxygen is passed through the first temperature control chamber 1, and remnant organic matter is flowed down into complete oxidation in air (or oxygen);
(2) thermal decomposition product aoxidizes
Oxidation tube 4 is heated to 600 DEG C to 800 DEG C by the second temperature control chamber 3, opens the air circuit breaker of oxygen manifold 14 13, make all to be oxidized to CO in the case where there is oxygen stream from the thermal decomposition product that pyrolysis oven 2 flows out2
(3) oxidation product detects
The gas obtained in step (2) is passed through clean unit, after removing moisture and solid particle, is sent into detection unit, profit CO with infrared detector 9 to output2Carry out on-line checking;
(4) test data is handled
1. by 50 DEG C~90 DEG C, 90 DEG C~300 DEG C, 300 DEG C~800 DEG C of thermal decomposition product is in turn divided into gaseous hydrocarbon, trip From hydrocarbon, cracked hydrocarbon;Oxidable organic matter after the completion of thermal cracking is divided into remnant organic matter;
2. by implementing standard substance test, gaseous hydrocarbon, free hydrocarbon, cracked hydrocarbon and remnant organic matter test data are distinguished It is associated with S0, S1, S2, S4 parameter value of conventional rock pyrologger, obtain consistent with conventional rock pyrologger Hydrocarbon source rock rock pyrolysis analysis supplemental characteristic;
3. on the basis of being calibrated with standard substance to test data, by gaseous hydrocarbon in source rock sample, free hydrocarbon, The organic carbon content of cracked hydrocarbon and the test data of remnant organic matter content sum up, and obtain and use carbon sulphur instrument traditional test knot The consistent hydrocarbon source rock total content of organic carbon data (TOC) of fruit.
Above-mentioned steps (1), (2), (3), (4) are carried out by control process unit 15, such as computer.
Some embodiments are exemplified below, the utility model is further illustrated.
Embodiment 1
Sample description:Niutitang group mud shale.
Test condition:The heating schedule of first temperature control chamber 1:50 DEG C of initial temperature, constant temperature is after 1 minute with 20 DEG C/min of speed 90 DEG C are warming up to, constant temperature 1 minute;300 DEG C are warming up to 50 DEG C/min of speed, constant temperature 5 minutes;Heated up with 50 DEG C/min of speed To 800 DEG C, constant temperature 1 minute.650 DEG C of second temperature control chamber, 3 temperature.100 DEG C of 5 temperature < of gas cooling chamber.Helium flow velocity 18mL/ Min, air velocity 20mL/min.4.26 microns of 9 wavelength of infrared detector.
Test result:S0:0.00mg/g;S1:0.08mg/g;S2:0.61mg/g;S4:25.04mg/g;TOC:2.57%.
Embodiment 2
Sample description:Heshan group carbonaceous mud shale.
Test condition:The heating schedule of first temperature control chamber 1:50 DEG C of initial temperature, constant temperature is after 1 minute with 20 DEG C/min of speed 90 DEG C are warming up to, constant temperature 1 minute;300 DEG C are warming up to 50 DEG C/min of speed, constant temperature 5 minutes;Heated up with 50 DEG C/min of speed To 800 DEG C, constant temperature 1 minute.650 DEG C of second temperature control chamber, 3 temperature.100 DEG C of 5 temperature < of gas cooling chamber.Helium flow velocity 18mL/ Min, air velocity 20mL/min.4.26 microns of 9 wavelength of infrared detector.
Test result:S0:0.03mg/g;S1:0.16mg/g;S2:2.55mg/g;S4:38.21mg/g;TOC:4.09%.
Embodiment 3
Sample description:Coal of Longtan Coal Series In The Middle.
Test condition:The heating schedule of first temperature control chamber 1:50 DEG C of initial temperature, constant temperature is after 1 minute with 20 DEG C/min of speed 90 DEG C are warming up to, constant temperature 1 minute;300 DEG C are warming up to 50 DEG C/min of speed, constant temperature 5 minutes;Heated up with 50 DEG C/min of speed To 800 DEG C, constant temperature 1 minute.650 DEG C of second temperature control chamber, 3 temperature.100 DEG C of 5 temperature < of gas cooling chamber.Helium flow velocity 18mL/ Min, air velocity 20mL/min.4.26 microns of 9 wavelength of infrared detector.
Test result:0.05mg/g;S1:0.13mg/g;S2:9.05mg/g;S4:590.67mg/g;TOC:59.99%.
Embodiment 4
Sample description:Jurassic system carbonaceous mudstone.
Test condition:The heating schedule of first temperature control chamber 1:50 DEG C of initial temperature, constant temperature is after 1 minute with 20 DEG C/min of speed 90 DEG C are warming up to, constant temperature 1 minute;300 DEG C are warming up to 50 DEG C/min of speed, constant temperature 5 minutes;Heated up with 50 DEG C/min of speed To 600 DEG C, constant temperature 1 minute.650 DEG C of second temperature control chamber, 3 temperature.100 DEG C of 5 temperature < of gas cooling chamber.Helium flow velocity 18mL/ Min, air velocity 20mL/min.4.26 microns of 9 wavelength of infrared detector.
Test result:0.08mg/g;S1:0.89mg/g;S2:9.48mg/g;S4:26.40mg/g;TOC:3.68%.
Embodiment 5
Sample description:Fly celestial pass group marl.
Test condition:The heating schedule of first temperature control chamber 1:50 DEG C of initial temperature, constant temperature is after 1 minute with 20 DEG C/min of speed 90 DEG C are warming up to, constant temperature 1 minute;300 DEG C are warming up to 50 DEG C/min of speed, constant temperature 5 minutes;Heated up with 50 DEG C/min of speed To 600 DEG C, constant temperature 1 minute.650 DEG C of second temperature control chamber, 3 temperature.100 DEG C of 5 temperature < of gas cooling chamber.Helium flow velocity 18mL/ Min, air velocity 20mL/min.4.26 microns of 9 wavelength of infrared detector.
Test result:S0:0.04mg/g;S1:0.21mg/g;S2:7.79mg/g;S4:9.76mg/g;TOC:1.78%.
In summary, the utility model hydrocarbon source rock organic carbon pyrolysis analysis device, it has following advantages:
(1) highest pyrolysis temperature can reach 850 DEG C, suitable for general evolution level to high evolution level mud shale Organic carbon analysis;
(2) by the way that hydrogen flame ion signal of the conventional rock pyrolysis instrument for each pyrolysis temperature stage thermal cracking products is examined Survey (FID) is changed into the detection for its carbon signal so that test data directly embodies the organic carbon content of hydrocarbon source rock, without logical Cross empirical equation to be calculated, avoid because the content of organic carbon of hydrocarbon source rock data error that properties of samples difference is brought;
(3) the philosophy and technique method based on hydrocarbon source rock rock pyrolysis analysis, the rock pyrolysis ginseng of the utility model device Number can correspond with the rock pyrolysis parameter of conventional rock pyrolysis instrument, possess the analysis test work(of conventional rock pyrolysis instrument Can, thus hydrocarbon primary rock producing hydrocarbon potentiality parameter can be obtained;
(4) S0, S1, S2, S4 pyrolysis parameters of rock and TOC indexs with regard to hydrocarbon source rock can be obtained, simple operation, test are once tested Efficiency high.
The merely exemplary explanation of above-described embodiment principle of the present utility model and its effect are new not for this practicality is limited Type.The utility model also has many aspects to be improved on the premise of without prejudice to overall thought, any to be familiar with this technology Personage all modifications and changes can be carried out to above-described embodiment without prejudice under spirit and scope of the present utility model.Therefore, lift All those of ordinary skill in the art are complete without departing from the spirit disclosed in the utility model and institute under technological thought Into all equivalent modifications or change, should be covered by claim of the present utility model.

Claims (5)

1. a kind of hydrocarbon source rock organic carbon pyrolysis analysis device, it is characterised in that it includes pyrolysis unit, the oxidation list being sequentially connected Member, clean unit, detection unit, and the operation for device and control, the control process unit of data acquisition and procession;
The pyrolysis unit includes the first temperature control chamber and internal pyrolysis oven, and the armouring that the pyrolysis oven includes 1000 DEG C of heatproof heats Silk;The oxidation unit includes the second temperature control chamber and internal oxidation tube, and the armouring that the second temperature control chamber includes 1000 DEG C of heatproof adds Heated filament;The clean unit includes gas cooling chamber and internal moisture dispels component and solid particle dispels component, and the moisture is dispelled Component series connection, which is dispelled, except component and solid particle is placed in gas cooling intracavitary;The detection unit includes detector and is resident chamber and interior The infrared detector in portion;
The first temperature control chamber one end is connected by gas pipeline with gas circuit change-over switch, and the other end passes through gas path pipe and the oxidation The inlet end connection of pipe;The gas circuit change-over switch connects helium pipeline and oxygen channel respectively;The oxygen channel is additionally provided with band gas The oxygen manifold of way switch, the oxygen manifold are also connected to the inlet end of the oxidation tube;The outlet side of the oxidation tube passes through gas The inlet end that pipeline dispels component with the moisture is connected;The solid particle dispels the outlet side of component and entering for the infrared detector Gas end connects, the outlet side of the infrared detector and atmosphere.
2. hydrocarbon source rock organic carbon pyrolysis analysis device according to claim 1, it is characterised in that:The control process unit It is connected by sensor and digital communications ports with the pyrolysis unit, oxidation unit, clean unit, detection unit.
3. hydrocarbon source rock organic carbon pyrolysis analysis device according to claim 1 or 2, it is characterised in that:The oxygen channel Flow stabilizing valve is equipped with helium pipeline.
4. hydrocarbon source rock organic carbon pyrolysis analysis device according to claim 1, it is characterised in that:The oxygen channel connects oxygen Source of the gas or air-source, the helium pipeline connect helium gas source.
5. hydrocarbon source rock organic carbon pyrolysis analysis device according to claim 1, it is characterised in that:The control process unit For computer.
CN201720603290.8U 2017-05-26 2017-05-26 A kind of hydrocarbon source rock organic carbon pyrolysis analysis device Active CN206832715U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107219245A (en) * 2017-05-26 2017-09-29 国家地质实验测试中心 A kind of hydrocarbon source rock organic carbon pyrolysis analysis apparatus and method
WO2022187600A1 (en) * 2021-03-04 2022-09-09 Saudi Arabian Oil Company Accelerated programmed source rock pyrolysis

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107219245A (en) * 2017-05-26 2017-09-29 国家地质实验测试中心 A kind of hydrocarbon source rock organic carbon pyrolysis analysis apparatus and method
CN107219245B (en) * 2017-05-26 2023-11-24 国家地质实验测试中心 Organic carbon pyrolysis analysis device for hydrocarbon source rock
WO2022187600A1 (en) * 2021-03-04 2022-09-09 Saudi Arabian Oil Company Accelerated programmed source rock pyrolysis

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