CN101333446A - Device for pyrolyzing kerogen in stages for hydrocarbon-generating dynamics research - Google Patents
Device for pyrolyzing kerogen in stages for hydrocarbon-generating dynamics research Download PDFInfo
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- CN101333446A CN101333446A CNA2008100298458A CN200810029845A CN101333446A CN 101333446 A CN101333446 A CN 101333446A CN A2008100298458 A CNA2008100298458 A CN A2008100298458A CN 200810029845 A CN200810029845 A CN 200810029845A CN 101333446 A CN101333446 A CN 101333446A
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Abstract
The invention discloses a step-by-step kerogen pyrolysis device used for hydrocarbon generation kinetics study. The step-by-step kerogen pyrolysis device comprises a heating tube(1) and an overturn mechanism which is capable of vertically turning the heating tube for 180 degrees. Both ends of the heating tube are provided with sealing covers. A sample tube(2)which can axially slide is arranged in the heating tube, and a first heating device(3), a first thermocouple(4), a carrier gas inlet and a carrier gas outlet are arranged on the upper half segment of the heating tube. The carrier gas inlet and the carrier gas outlet are respectively connected with a carrier gas inlet pipe and a carrier gas outlet pipe(8). A second heating device(9), a second thermocouple(10), a cooling gas inlet(11) and a cooling gas outlet(12)are arranged on the lower half segment of the heating tube; the cooling gas inlet(11) and the cooling gas outlet(12) are respectively connected with a cooling gas inlet pipe(13)and a cooling gas outlet pipe(14). The pyrolysis device can pyrolyze kerogen step by step and has the advantages of high experimental precision, small liquid nitrogen consumption amount, simple structure and low cost.
Description
Technical field
The present invention relates to a kind of pyrolysis installation, specifically be meant and a kind of kerogen in the rock carried out the pyrolyzing kerogen in stages device that pyrolytic stage by stage is used for hydrocarbon-generating dynamics research.
Background technology
In hydrocarbon-generating dynamics research research, need oil generation productive rate and the composition of research kerogen in the differing temps section.According to chemical kinetics formula (Arrhenius formula), the oil generation productive rate is subjected to the acting in conjunction of temperature and time, and for improving analysis precision, just accurately the control sample makes temperature deviation less than 1 ℃ at the heating temperature of each temperature section as far as possible.At present, carry out the continuous of sample both at home and abroad or be interrupted type of heating mainly containing following 3 kinds, its relative merits are as follows:
1, continuous heating-type: promptly sample in well heater from low temperature, persistently overheating with certain temperature rise rate, (generally being to be elevated to 600 ℃) from 300 ℃, conversion by valve, the hydrocarbon product of differing temps section is collected in a series of cold-trap, after thermal analogy finishes, analyze quantity, the composition of hydrocarbon product in each cold-trap more one by one.In this type of heating, because sample is to be subjected to continuous, stable heating, not having the interruption of temperature, so there is not temperature deviation basically, is the ideal type of heating.But this type of heating, also bring very big defective for whole analytical system: (1) is because heating is a successive, so the product of differing temps section must be delivered to earlier in the cold-trap and preserve, after thermal analogy finishes, analyze quantity, the composition of hydrocarbon product in each cold-trap more one by one.Cold-trap is generally 10, and the thermal analogy time (the longest is 10 hours) adds that 10 product analysis (gas chromatographic analysis) times in the cold-trap reach 25 hours, to keep in long-time the low-temperature condition of cold-trap, needs a large amount of liquid nitrogen, has increased job costs; (2) from the pyrolysis chamber when different cold-traps are carried pyrolysis product, need with 22 logical high temperature shift valves, the accessory of this import is worth 600 dollars, and rotor material wherein is very soft, because carrier gas is by sample the time, mineral grain fine in the sample can be blown off enters carrier gas, and under the wearing and tearing of entrained fine mineral, rotor is quick-wearing very in carrier gas, cause carrier gas to be revealed, thereby influence experiment accuracy, appliance requires often safeguard, more exchanging rotor.(3) in the whole work period, any one step goes wrong, and experiment is scrapped.(4) the pyrolysis product difference of different cold-traps acceptance because the smeary deposition can make the adsorptive power of cold-trap produce difference, influences the credibility of experimental result after the long term operation.
2, interrupted heating-type: sample is placed in the heating tube, with the usual manner heating, arrive the temperature of setting after, stop heating, allow heating tube and sample naturally cooling or feed nitrogen and cool off.The characteristics of this method are simple and reliable, but because heating tube and sample have the same thermal process that is subjected to, and heating tube has bigger thermal capacity and thermal inertia, very difficult realization heats up fast and accurately, lowers the temperature, for example, when needs were heated to 520 ℃ to sample from 500 ℃ in 2 minutes, must experience from the warm of room temperature to 500 ℃, this process may need 10 minutes, because a lot of as the too fast temperature overshot that will make of heating.Arrive 520 ℃ in temperature, also can not make heating tube and sample wherein be reduced to room temperature in moment.This type of heating does not reach the requirement of hydrocarbon-generating dynamics.
3, platinum filament heating method: the method that external CDS company adopts.Twine the platinum filament of energising in the silica tube outside that sample is housed, platinum filament is as heating member, again as temperature element.It is very accurate that this type of heating, the temperature of platinum filament itself can be controlled, but the sample in the silica tube is bad because of the thermal conductivity of silica tube, and the influence of the carrier gas that temperature is lower in the pyrolysis chamber, makes the temperature of sample will be lower than the platinum filament temperature; Simultaneously, because each when placing the quartz specimen pipe, the relative position of sample hose and platinum filament can not repeat fully, so the repeatability of each experiment also is difficult to assurance.For above-mentioned reasons, this method can not satisfy the precision of hydrocarbon-generating dynamics research to temperature survey, control.
Summary of the invention
The object of the present invention is to provide a kind of experimental precision height, the liquid nitrogen consumption is few, simple in structure, cost the is low pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research, comprise heating tube and can be with the vertical switching mechanism of degree of upset of heating tube, the two ends of described heating tube are provided with sealing cover, be provided with sample hose in axial sliding in the heating tube, the upper semisection of described heating tube is provided with primary heater, first thermopair, carrier gas inlet mouth and carrier gas venting port, carrier gas inlet mouth and carrier gas venting port are connected to carrier gas intake ducting and carrier gas gas exhaust duct respectively, the lower semisection of described heating tube is provided with the secondary heater and second thermopair, cold gas inlet mouth and cold gas venting port, cold gas inlet mouth and cold gas venting port are connected to cold gas intake ducting and cold gas gas exhaust duct respectively.
Owing to adopted above-mentioned structure, the present invention has following beneficial effect:
1, can realize reaching fast to the heating of sample and set Heating temperature, be reduced to the requirement of stopped reaction temperature fast; Analytical data reaches the accuracy requirement of hydrocarbon-generating dynamics research fully.
2, only need 1 cold-trap, and just just need cooling, thereby the liquid nitrogen consumption reduces greatly in the product collection stage.
3, cancelled cost an arm and a leg, failure rate is high 22 logical valves, reduced equipment cost, improved the equipment reliability.Device structure is simple, need not safeguard substantially.
4, all working step can adopt time variable control to carry out high efficiency automatically.
Description of drawings
Fig. 1 is the structural representation that is used for the pyrolyzing kerogen in stages device of hydrocarbon-generating dynamics research;
Fig. 2 is the time variable control block diagram that is used for the pyrolyzing kerogen in stages device of hydrocarbon-generating dynamics research.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail, but does not constitute any limitation of the invention.
As shown in Figure 1, the pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research of the present invention comprises heating tube 1 and heating tube 1 vertically can be turned over the switching mechanism of turnback, and described heating tube 1 is made by stainless material.The two ends of heating tube 1 are provided with sealing cover 17, are provided with carbon seal ring 18 between the pipe end face of heating tube 1 and the sealing cover 17.Be provided with sample hose 2 in the described heating tube 1, sample hose 2 is made by the porous Stainless Steel Cloth, and its external diameter is slightly less than the internal diameter of heating tube 1, and when switching mechanism vertically overturn heating tube 1, sample hose 2 just can axially slide in heating tube 1.Can place powdered sample in the middle of the sample hose 2, the two ends of sample hose 2 are stopped up with silica wool and are prevented that sample scatters and disappears, and sample hose 2 and quartzy Cottonopolis have excellent air permeability.The upper semisection of described heating tube 1 is provided with primary heater 3, first thermopair 4, carrier gas inlet mouth 5 and carrier gas venting port 6, and carrier gas inlet mouth 5 and carrier gas venting port 6 are connected to carrier gas intake ducting 7 and carrier gas gas exhaust duct 8 respectively.The upper semisection of described heating tube 1 is as the programmed heating district, the upper semisection of 3 pairs of heating tubes 1 of primary heater heats, first thermopair 4 can be measured the temperature of the upper semisection of heating tube 1 in real time, makes things convenient for the programmed heating of primary heater 3, and carrier gas can be taken sample pyrolytic oil gas product out of collection.The lower semisection of heating tube 1 is as samples pre-heated and cooling zone, the lower semisection of heating tube 1 is provided with secondary heater 9 and second thermopair 10, cold gas inlet mouth 11 and cold gas venting port 12, and cold gas inlet mouth 11 and cold gas venting port 12 are connected to cold gas intake ducting 13 and cold gas gas exhaust duct 14 respectively.The lower semisection of 9 pairs of heating tubes 1 of secondary heater heats, and second thermopair 10 can be measured the temperature of the lower semisection of heating tube 1 in real time, the heating of convenient control primary heater 3.Cooling gas enters into heating tube 1 from cold gas inlet mouth 11, cold gas intake ducting 13 sample is cooled off, and discharges from cold gas venting port 12, cold gas gas exhaust duct 14 again.
Described switching mechanism comprises support 15 and the reducing motor 16 that is fixed on the support 15, and the motor shaft of described reducing motor 16 is connected with heating tube 1.The middle part union lever of described heating tube 1 is connected with motor shaft, and heating tube is in vertical state all the time.When the motor shaft of reducing motor 16 rotates, heating tube 1 is vertically overturn, the angle of the motor shaft rotation of control reducing motor 16 can realize easily that heating tube 1 vertically turns over turnback, and sample hose 2 just can be made evolution between programmed heating district, samples pre-heated and cooling zone like this.Heating tube 1 is connected with sequence controller by the softish electric wire, and heating tube 1 is same by soft, resilient pipeline introducing carrier gas and heat outputting analog product (oil gas).Circuit and gas circuit adopt soft the connection, when heating tube 1 is shifted one's position, do not produce stiff resistance.
Described primary heater 3 is enclosed within outside the heating tube 1, and primary heater 3 can be electric heating device.Described carrier gas intake ducting 7 around cloth between primary heater 3 and heating tube 1,3 pairs of carrier gas intake ductings of described first heating unit 7 carry out preheating, carrier gas enters the heating tube 1 and can the sample in the sample hose 2 be heated from carrier gas intake ducting 7, and sample just can be heated equably.
Described carrier gas inlet mouth 5 is located at the bottom of heating tube 1 upper semisection, and described carrier gas venting port 6 is located at the top of heating tube 1 upper semisection, can reduce the lower semisection that carrier gas enters into heating tube 1 so as far as possible, can not increase the temperature of the lower semisection of heating tube 1.
Described cold gas inlet mouth 11 is located at the bottom of heating tube 1 lower semisection, and described cold gas venting port 12 is located at the top of heating tube 1 lower semisection, and cold gas is flowed to temperature end from low-temperature end, increases refrigerative efficient.
Described first thermopair 4 is plugged on the sealing cover 17, and first thermopair 4 can weld together to guarantee sealing with sealing cover 17.The inner of first thermopair 4 is located on the axial line of heating tube 1, and when movable, the inner of first thermopair 4 can be inserted in the sample hose 2 sample hose 2, directly touches sample, to realize exact temperature measurement in heating tube 1.
Described second thermopair 10 is plugged on the sealing cover 17, and the 2nd thermopair 10 can weld together to guarantee sealing with sealing cover 17. and the inner of second thermopair 10 is located on the axial line of heating tube 1.When movable, the inner of second thermopair 10 can be inserted in the sample hose 2 sample hose 2, directly touches sample, to realize exact temperature measurement in heating tube 1.
Be respectively equipped with carrier gas intake valve 19, carrier gas vent valve 20, cold gas intake valve 21, cold gas vent valve 22 on described carrier gas intake ducting 7, carrier gas gas exhaust duct 8, cold gas intake ducting 13, the cold gas gas exhaust duct 14.The break-make of control carrier gas intake valve 19, carrier gas vent valve 20, cold gas intake valve 21, cold gas vent valve 22 is the circulation of may command carrier gas and cold gas, to realize time variable control easily.Wherein carrier gas gas exhaust duct 7 and carrier gas vent valve 20 need be heated to 300 ℃ oily noncondensing with what guarantee that pyrolysis produces in the carrier gas, carrier gas vent valve 20 can guarantee 300 ℃ of works better through particular design.
As shown in Figure 2, the present invention also includes sequence controller 23, and described sequence controller 23 connects primary heater 3, first thermopair 4, secondary heater 9, second thermopair 10, reducing motor 16, carrier gas intake valve 19, carrier gas vent valve 20, cold gas intake valve 21, cold gas vent valve 22.The temperature signal of first thermopair 4 and second thermopair 10 inputs to sequence controller 23; Sequence controller 23 is given primary heater 3 and secondary heater 9 control heat-processedes according to program setting output control signal; Sequence controller 23 output control signals are given carrier gas intake valve 19, carrier gas vent valve 20, cold gas intake valve 21, cold gas vent valve 22, with entering of control carrier gas and cold gas; The work of sequence controller 23 output control signal control reducing motors 16 is to realize the vertical 180 degree upsets of heating tube 1.All working step of the present invention can adopt time variable control to carry out high efficiency automatically.
Being heated to 600 ℃ flow process with one from 300 ℃ of temperature rise rates with 10 ℃/h below is example, and principle of work of the present invention and experiment flow are described:
(1) sample hose 2 that sample is housed is placed in the heating tube 1, the two end cap top cover labyrinth 17 of heating tube 1 is closed cold gas intake valve 21 and cold gas vent valve 22, and heating tube is in vertical position, be in the below as the lower semisection of preheating zone, be in the top as the upper semisection in programmed heating district.
(2) open carrier gas intake valve 19, carrier gas vent valve 20, carrier gas enters the heating tube 1 from carrier gas intake ducting 7, carrier gas inlet mouth 5, discharges from carrier gas venting port 6, carrier gas gas exhaust duct 8 again.
(3) primary heater 3 and secondary heater 9 heat simultaneously, and wherein secondary heater 9 constant temperature are at 300 ℃, and sample hose 2 is positioned at 300 ℃ preheating zone because of action of gravity.
(4) (temperature is lower than 300 ℃ to primary heater 3 when room temperature is heated to 300 ℃ with the temperature rise rate of 10 ℃/h, it is extremely slow to give birth to hydrocarbon reaction, can ignore), 180 ° of reducing motor 16 forward twirl in the switching mechanism, it is downward that heating tube 1 position becomes upper semisection, and sample hose 2 falls downwards because of action of gravity, is positioned at the programmed heating district of the upper semisection of heating tube 1, first thermopair 4 is near the sample in the sample hose 2, for the sample heating provides temperature control accurately.Secondary heater 9 stops heating; The beginning naturally cooling.Primary heater 3 follow procedures continue heating.Because the porousness of sample hose 2, the carrier gas of process preheating enters between the particle of sample immediately, and sample is heated.Because only 100 milligrams of the gross weights of sample and sample hose 2, quality only is 1/2000 of heating tube 1 and primary heater 3 quality summations, and sample has carried out preheating in the preheating zone, so to enter the temperature fluctuation that the programmed heating district causes suddenly very little because of sample hose 2, according to surveying and determination, actual temperature fluctuates less than 1 ℃, the fluctuation time was less than 2 seconds, that is to say that sample begins to carry out normal pyrolytic process by temperature program(me) in the instantaneous temperature that promptly reaches setting.Pyrolytic oil gas product enters cold-trap and collects.
(5) when the temperature of first thermopair 4 arrives 320 ℃, primary heater 3 stops heating, 180 ° of reducing motor 16 reverse twirl in the switching mechanism, it is downward that the heating tube position becomes the preheating zone, sample hose 2 falls downwards into the preheating zone because of action of gravity, (because that preheating zone and programmed heating district are separated by is far away, during the heating of programmed heating district, the temperature of preheating zone is not higher than 300 ℃ all the time.) cold gas intake valve 21 and cold gas vent valve 22, the nitrogen of importing the room temperature of 500ml/min from cold gas intake ducting 13 cools off sample, and sample hose 2 and sample wherein can be cooled to below 300 ℃ in less than 2 seconds time, and reaction stops.Cold gas intake valve 21 and cold gas vent valve 22 are opened after 10 seconds and are closed, and close carrier gas intake valve 19, carrier gas vent valve 20 then.
(6) pyrolysis product is delivered to gas chromatograph analysis, about 1.5 hours of analytic process.Preceding half period of section at this moment, all circuit of heating tube, gas circuit are closed, and are ready.
(7) time second half section of analyzing of gas chromatograph, 320 ℃-340 ℃ pyrolysis and product analysis carried out in beginning repeated execution of steps (2)-(6).
(8) repeating step (2)-(6) repeatedly reach 600 ℃ until temperature, and experiment is finished.
Claims (9)
1. pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research, it is characterized in that: comprise heating tube (1) and heating tube (1) vertically can be turned over the switching mechanism of turnback, the two ends of described heating tube (1) are provided with sealing cover (17), be provided with sample hose (2) in axial sliding in the heating tube (1), the upper semisection of described heating tube (1) is provided with primary heater (3), first thermopair (4), carrier gas inlet mouth (5) and carrier gas venting port (6), carrier gas inlet mouth (5) and carrier gas venting port (6) are connected to carrier gas intake ducting (7) and carrier gas gas exhaust duct (8) respectively, the lower semisection of described heating tube (1) is provided with secondary heater (9) and second thermopair (10), cold gas inlet mouth (11) and cold gas venting port (12), cold gas inlet mouth (11) and cold gas venting port (12) are connected to cold gas intake ducting (13) and cold gas gas exhaust duct (14) respectively.
2. according to the described pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research of claim 1, it is characterized in that: described switching mechanism comprises support (15) and is fixed on reducing motor (16) on the support (15) that the motor shaft of described reducing motor (16) is connected with heating tube (1).
3. according to the described pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research of claim 1, it is characterized in that: described primary heater (3) is enclosed within outside the heating tube (1), between primary heater (3) and heating tube (1), described first heating unit (3) carries out preheating to carrier gas intake ducting (7) to described carrier gas intake ducting (7) around cloth.
4. according to the described pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research of claim 1, it is characterized in that: described carrier gas inlet mouth (5) is located at the bottom of heating tube (1) upper semisection, and described carrier gas venting port (6) is located at the top of heating tube (1) upper semisection.
5. according to the described pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research of claim 1, it is characterized in that: described cold gas inlet mouth (11) is located at the bottom of heating tube (1) lower semisection, and described cold gas venting port (12) is located at the top of heating tube (1) lower semisection.
6. according to the described pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research of claim 1, it is characterized in that: described first thermopair (4) is plugged on the sealing cover (17), and the inner of first thermopair (4) is located on the axial line of heating tube (1).
7. according to the described pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research of claim 6, it is characterized in that: described second thermopair (10) is plugged on the sealing cover (17), and the inner of second thermopair (10) is located on the axial line of heating tube (1).
8. according to the described pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research of claim 1, it is characterized in that: be respectively equipped with carrier gas intake valve (19), carrier gas vent valve (20), cold gas intake valve (21), cold gas vent valve (22) on carrier gas intake ducting (7), carrier gas gas exhaust duct (8), cold gas intake ducting (13), the cold gas gas exhaust duct (14).
9. according to the described pyrolyzing kerogen in stages device that is used for hydrocarbon-generating dynamics research of claim 8, it is characterized in that: also include sequence controller (23), described sequence controller (23) connects primary heater (3), first thermopair (4), secondary heater (9), second thermopair (10), reducing motor (16), carrier gas intake valve (19), carrier gas vent valve (20), cold gas intake valve (21), cold gas vent valve (22).
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| CN2008100298458A CN101333446B (en) | 2008-07-30 | 2008-07-30 | Device for pyrolyzing kerogen in stages for hydrocarbon-generating dynamics research |
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| CN2008100298458A CN101333446B (en) | 2008-07-30 | 2008-07-30 | Device for pyrolyzing kerogen in stages for hydrocarbon-generating dynamics research |
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| CN101333446B CN101333446B (en) | 2012-05-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102269745A (en) * | 2010-06-04 | 2011-12-07 | 北京市产品质量监督检验所 | Thermal desorption sampling device |
| CN103279146A (en) * | 2013-05-31 | 2013-09-04 | 上海天美科学仪器有限公司 | Method and system for temperature rise based on PID control |
| CN108896592A (en) * | 2018-08-27 | 2018-11-27 | 中国石油天然气股份有限公司 | Shale oil ground in-situ heats kerogenic test method and device in upgrading processes |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100457855C (en) * | 2007-02-28 | 2009-02-04 | 中国科学院广州地球化学研究所 | Pressing open type cracking hydrocarbon simulating device |
-
2008
- 2008-07-30 CN CN2008100298458A patent/CN101333446B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102269745A (en) * | 2010-06-04 | 2011-12-07 | 北京市产品质量监督检验所 | Thermal desorption sampling device |
| CN103279146A (en) * | 2013-05-31 | 2013-09-04 | 上海天美科学仪器有限公司 | Method and system for temperature rise based on PID control |
| CN103279146B (en) * | 2013-05-31 | 2015-02-04 | 上海天美科学仪器有限公司 | Method and system for temperature rise based on PID control |
| CN108896592A (en) * | 2018-08-27 | 2018-11-27 | 中国石油天然气股份有限公司 | Shale oil ground in-situ heats kerogenic test method and device in upgrading processes |
| CN108896592B (en) * | 2018-08-27 | 2021-01-01 | 中国石油天然气股份有限公司 | Method and device for testing kerogen in shale oil underground in-situ heating modification process |
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