CN104849172A - Oil shale oil content test experiment apparatus and test method thereof - Google Patents

Oil shale oil content test experiment apparatus and test method thereof Download PDF

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Publication number
CN104849172A
CN104849172A CN201410054940.9A CN201410054940A CN104849172A CN 104849172 A CN104849172 A CN 104849172A CN 201410054940 A CN201410054940 A CN 201410054940A CN 104849172 A CN104849172 A CN 104849172A
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oil
resinous shale
sealing press
heated sealing
gas collection
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CN201410054940.9A
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Chinese (zh)
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CN104849172B (en
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马中良
郑伦举
徐旭辉
余晓露
李志明
王强
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中国石油化工股份有限公司
中国石油化工股份有限公司石油勘探开发研究院
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Abstract

The invention discloses an oil shale oil content test experiment apparatus and a test method thereof. The apparatus comprises: a heating sealing pressure mechanism used for applying a stratum pressure to an oil shale sample and heating the oil shale sample to generate oil and gas; an oil and gas extraction mechanism connected with the inlet of the heating sealing pressure mechanism and used for extracting oil and gas from the oil shale sample; and an oil and gas collecting mechanism connected with the outlet of the heating sealing pressure mechanism and used for collecting the oil and the gas discharged from the heating sealing pressure mechanism. The apparatus can be used to determine the content of the oil shale in an underground in situ state in order to facilitate exploration of the oil shale.

Description

Oil content of oil shale experimental apparatus for testing and method of testing thereof
Technical field
The present invention relates to resinous shale exploration and development technical field, be specifically related to a kind of oil content of oil shale experimental apparatus for testing and method of testing thereof.
Background technology
The oil content of resinous shale is the most important index that resinous shale develops.The oil content of current resinous shale measures conventional rice steamer aluminium cracking process and extraction technics.Cracking process is that resinous shale sample comminution is loaded destructive distillation pipe to a certain size, 520 DEG C are heated to certain programming rate under isolated air conditions, and keep the regular hour, measure the yield of gained oil, water, semicoke and destructive distillation product after destructive distillation, its oil content drawn is the important parameter whether evaluation regional resinous shale has ground destructive distillation value.
Usually, the oil shale resources that buried depth is less than 300m can pass through strip mining transformation, are transported to destructive distillation factory and extract oil shale fuel.The resinous shale that buried depth is greater than 300m only has by oil shale layer heating (be greater than the direct cost of winning of 300m oil shale reserves too high, cost-effective exploitation is by directly heating oil shale layer, and converted in-situ olefiant gas is exploited), is converted into oil shale fuel.Traditional ground distillation process technology refine from resinous shale oil shale fuel costly, seriously polluted, the oil produced containing polar compound up to 40% ~ 60%, nitrogenate is more than 1%.First hydrotreating polar compound must be removed, then conventional method refining could be used.For mid-deep strata oil shale recovery, because cost of winning is too high and cause economic benefit lower, thus from 20 century 70s, many internationally recognizable energy companies start the research being devoted to oil shale in-situ production technique, the environmental pollution that the waste water that this technology generates during hot-working after can avoiding oil shale recovery in destructive distillation device, waste gas and waste residue cause, realizes the maximum using of resource.But the oil shale in-situ mining resources quantifier elimination apparatus and method at present almost not to a certain area before formal exploitation, thus the oil content of resinous shale cannot be judged more exactly.If judge that the inaccurate oil mass causing exploiting out is very few because of oil content or cause the interruption of recovery process, the significant wastage of human and material resources and financial resources will be caused.
Summary of the invention
A technical matters to be solved by this invention provides a kind of oil content of oil shale experimental apparatus for testing, and it can be used for judging oil content of oil shale under home state thus more be conducive to the exploration and development of resinous shale.
For this technical matters, technical solution of the present invention is, provides a kind of oil content of oil shale experimental apparatus for testing with following structure, comprising:
Heated sealing press structure, its for reservoir pressure is applied to resinous shale sample and resinous shale sample is carried out heating generate oily gentle;
Oil gas extraction mechanism, it is connected with the import of heated sealing press structure, gentle for the oil in extraction oil shale sample; With
Oil gas collection mechanism, is connected with the outlet of heated sealing press structure, gentle for collecting from heated sealing press structure oil out.
Compared with prior art, oil content of oil shale experimental apparatus for testing of the present invention has the following advantages.The environment under reservoir pressure simulated oil shale in-situ state can be applied due to the heated sealing press structure in the present invention to the resinous shale sample put into wherein, and obtained the oil gas of resinous shale by heating and oil gas extraction.The oil generated by oil gas collection collect resinous shale is gentle, by calculating the hydrocarbon content that can obtain resinous shale.Because the hydrocarbon content of resinous shale can provide most important foundation for oil shale in-situ mining resources amount, be conducive to resinous shale exploration and development, save human and material resources and financial resources.
In one embodiment, heated sealing press structure comprises:
High-temperature high-pressure reaction kettle, for holding resinous shale sample;
Primary heater, for heating high-temperature high-pressure reaction kettle; With
To exert pressure assembly, act on resinous shale sample with the reservoir pressure that sample during alternative home state is subject to.The formation function power that when carrying out pressure-loaded to simulate state in position by assembly of exerting pressure to resinous shale sample, resinous shale is subject to.Therefore, the experimental situation of heated sealing press structure structure is closer to the environment under resinous shale in position state.
In a preferred embodiment, assembly of exerting pressure comprises:
Upper load cylinder, acts on the upper surface of resinous shale sample to substitute the reservoir pressure be subject at the upper surface of ground in-situ state resinous shale; With
Lower load cylinder, acts on the lower surface of resinous shale sample to substitute the reservoir pressure be subject at the lower surface of ground in-situ state resinous shale.The approximate substitution resinous shale formation function power that is subject to of state is in position carried out by the acting force of upper and lower load cylinder to resinous shale sample.Thus the oil content that test experiments can be made to obtain is closer to oil content when exploiting under resinous shale in position state.
In one embodiment, supercritical carbon dioxide oil gas extraction mechanism comprises:
Supercritical carbon dioxide storage tank;
Secondary heater, secondary heater is connected with supercritical carbon dioxide storage tank, for heating supercritical carbon dioxide storage tank;
Pressurizer, its import is connected with supercritical carbon dioxide storage tank, and its outlet is connected with the import of heated sealing press structure.
Type of heating generate and collect the part oil obtained in resinous shale gentle after, remain in resinous shale by supercritical carbon dioxide extracting and oil in high-temperature high-pressure reaction kettle gentle, make oil content test result closer to the exploitation result under home state.
In a preferred embodiment, described pressurizer comprises:
Pressurized container, its epicoele is connected with supercritical carbon dioxide storage tank by pipeline; With
Electrodynamic pump, is connected with the cavity of resorption of pressurized container, and to the carbon dioxide compression supercharging in pressurized container, the carbon dioxide after supercharging is connected with the import of heated sealing press structure by the road by the outlet of pressurized container.Being pressurized to the carbon dioxide in pressurized container by electrodynamic pump makes carbon dioxide reach supercriticality, then electrodynamic pump remain in resinous shale after supercritical carbon dioxide being pumped in high-temperature high-pressure reaction kettle extraction heating and oil in high-temperature high-pressure reaction kettle gentle, when the oil collecting resinous shale is gentle, pressure reduces, supercritical carbon dioxide becomes gas again, pollution-free, and test experiments result is not affected.
In a preferred embodiment, the pipeline between described supercritical carbon dioxide storage tank and pressurized container is provided with the first valve, and the pipeline between the import of described pressurized container and heated sealing press structure is provided with the second valve.First open the first valve, carbon dioxide enters pressurized container.Then, when the first valve and the second valve are all closed, pressurization is carried out to the carbon dioxide in pressurized container and forms supercritical carbon dioxide.Open the second valve again, make supercritical carbon dioxide enter extraction oil in high-temperature high-pressure reaction kettle gentle.
In one embodiment, oil gas collection mechanism comprises: oil header, is connected with the outlet of heated sealing press structure; 3rd well heater, for keeping the temperature of oil header; Water aspirator, is connected with the outlet of oil header; Gas collector, is connected with the outlet of water aspirator; With vacuumize assembly, be connected with the outlet of water aspirator.Vacuumize assembly before the reaction, pipeline and the in-house gas of oil gas collection to be extracted, make test result more accurate.And extracting vacuum constructs environment under low pressure before oil gas collection, the oil be more conducive in high-temperature high-pressure reaction kettle is gentle to the direction flowing of oil gas collection mechanism.
In a preferred embodiment, vacuum device comprises vacuum pump, and the outlet of water aspirator is connected with gas collector through the first arm, and the first arm is provided with valve; The outlet of described water aspirator connects vacuum pump through the second arm, and the second arm is provided with valve.Realize realizing gas collection and vacuum respectively in different situations by two arms and two valves.
Another technical matters to be solved by this invention is, provide a kind of can more exactly test oil shale ground in-situ state oil content thus for judging that oil shale in-situ resource can the amount of adopting stock number provide the oil content of oil shale method of testing of foundation.
For this technical matters, the technical solution provided is, provide a kind of oil content of oil shale method of testing its adopt oil content of oil shale proving installation described in above-mentioned any one, and to comprise the following steps:
1) choose column resinous shale sample, at ambient temperature after dry a period of time, weigh and be designated as M 0; The oil header weight of oil gas collection mechanism of weighing counts M 1;
2) column resinous shale sample is loaded heated sealing press structure, and carry out pressure-loaded and sealing;
3) start vacuum device, heated sealing press structure, oil gas collection mechanism and connecting line vacuumized and carries out air-leakage test, reaching after requirement until vacuum tightness and close vacuum device;
4) connecting line between heated sealing press structure with oil gas collection mechanism is connected with the intermediate receptacle storing local water and the electrodynamic pump be connected with intermediate receptacle by arm, start electrodynamic pump the local water in this intermediate receptacle is injected in the high-temperature high-pressure reaction kettle in heated sealing press structure, the hydrostatic pressing force value of corresponding depth segment when the hydrodynamic pressure that resinous shale sample is subject to reaches ground in-situ state;
5) start heated sealing press structure heat resinous shale sample and keep constant temperature; It is gentle that constant temperature terminates rear unlatching oil gas collection collect oil;
6) extract by oil gas extraction mechanism the oil remained in resinous shale sample gentle, and gentle by oil gas collection collect oil;
7) unload the oil header of oil gas collection mechanism, weigh and be designated as M 2, then the oil offtake of resinous shale sample is M 2-M 1, the oil content of this resinous shale is (M 2-M 1)/M 0.
Preferably, in step 3), first vacuumize, then by be filled with high pressure nitrogen detect heated sealing press structure, oil gas collection mechanism and between the impermeability of connecting line; When impermeability is good, then carry out the vacuum tightness being evacuated down to needs.Ensure the reliability of test result.
In step 5), after constant temperature terminates, first the connecting line between sealing load mechanism and oil gas collection mechanism and oil gas collection mechanism are evacuated down to the vacuum tightness of needs, then the oil flowed out from sealing load mechanism by oil gas collection collect is gentle.The oil being conducive to extracting is gentle to the flowing of oil gas collection mechanism, ensures the reliability of test result.
Accompanying drawing explanation
It is a kind of specific embodiment of oil content of oil shale experimental apparatus for testing of the present invention shown in Fig. 1.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Be illustrated in figure 1 a kind of specific embodiment of oil content of oil shale experimental apparatus for testing of the present invention.In this embodiment, this oil content of oil shale experimental apparatus for testing comprises heated sealing press structure, the oil gas extraction mechanism be connected by pipeline with heated sealing press structure and the oil gas collection mechanism be connected with the outlet of heated sealing press structure.Wherein, heated sealing press structure is for holding resinous shale sample and the reservoir pressure that resinous shale is subject under simulating state in position and to make resinous shale sample generate oil by heated sealed gentle.In addition, oil gas extraction mechanism is as gentle in 360 ° of oil that can not be expelled in oil gas collection mechanism for being heated to experimental temperature in extraction oil shale sample.Therefore, in the present embodiment, the oil that heating process generation is not only collected by oil gas collection mechanism is gentle, and it is gentle also to collect by the oil of supercritical carbon dioxide extracting.
In the present embodiment, heated sealing press structure comprises:
High-temperature high-pressure reaction kettle 110, for holding resinous shale sample 111;
Primary heater 109, this primary heater 109 generally adopts sealed-box type electric furnace, and it holds high-temperature high-pressure reaction kettle 110 and for carrying out heated sealed to high-temperature high-pressure reaction kettle 110;
Upper pressure exerting arrangement, the upper surface acting on high-temperature high-pressure reaction kettle 110 is with the upper surface of alternative resinous shale sample 111 reservoir pressure that is subject to of state in position; With
Lower pressure exerting arrangement, the lower surface being supported on high-temperature high-pressure reaction kettle 110 is with the lower surface of the alternative resinous shale sample 111 formation function power that is subject to of state in position.
In a preferred embodiment, upper pressure exerting arrangement and lower pressure exerting arrangement include: load cylinder 107,113, and bar 108,112 of exerting pressure.As shown in Figure 1, upper load cylinder 107 acts on the upper surface of resinous shale sample 111 by bar 108 of above exerting pressure; Bar 112 of exerting pressure under lower load cylinder 113 passes through acts on the lower surface of resinous shale sample 111.
In the present embodiment, oil gas extraction mechanism comprises supercritical carbon dioxide storage tank 101, secondary heater 102 and pressurizer.Wherein, secondary heater 102 is connected with supercritical carbon dioxide storage tank 101, for heating supercritical carbon dioxide storage tank 101.This pressurizer comprises pressurized container 104 and electrodynamic pump 105.The epicoele of pressurized container 104 is connected with supercritical carbon dioxide storage tank 101 with the first valve 103 by pipeline; The cavity of resorption of pressurized container 104 is connected with electrodynamic pump 105.By the carbon dioxide compression supercharging of electrodynamic pump 105 pairs of pressurized containers 104, the carbon dioxide after supercharging is connected with the import of the second valve 106 with the high-temperature high-pressure reaction kettle 110 in heated sealing press structure by pipeline through the outlet of pressurized container 104.In the present embodiment, below the import of high-temperature high-pressure reaction kettle 110 is located at, and its outlet is located in the above.
In the present embodiment, this oil gas collection mechanism comprises:
Oil header 124, is connected with the outlet of heated sealing press structure;
3rd well heater 123, heats to keep the temperature of oil header 124 at about 80 DEG C to oil header 124;
Water aspirator 125, is connected with the outlet of oil header 124, for collecting moisture;
Cold-trap 126, is located at outside water aspirator 125, for making the water vapor rapid condensation in water aspirator 125;
Gas collector 129, is connected with the outlet of valve 131 with water aspirator 125 by the first arm 121; With
Vacuum pump 127, is connected with the outlet of valve 128 with water aspirator 125 by the second arm 132, and vacuum pump 127 vacuumizes heated sealing press structure, oil gas collection mechanism and the pipeline for connecting before heating.First arm 121 and the second arm 132 are set up in parallel.
In FIG, the main line between high-temperature high-pressure reaction kettle 110 and oil header 124 is provided with successively valve 117, valve 118 and valve 122, valve 118 is multiport valve.Wherein, an interface of valve 118 is connected high-pressure nitrogen bottle 120 by bye-pass with valve 119, and an interface is connected with outlet branch road and air release 130, also has an interface to be connected high pressure pump assembly 114 and 115 by bye-pass with valve 116.High pressure pump assembly 114 and 115 is for regulating the pressure of main line.
The invention still further relates to a kind of oil content of oil shale method of testing, it adopts above-mentioned oil content of oil shale proving installation, and comprises the following steps:
1) choose the column resinous shale sample 111 that diameter is 30 ~ 50mm, high 50 ~ 100mm, at ambient temperature after dry a period of time, weigh and be designated as M 0; The weight of oil header 124 of oil gas collection mechanism of weighing counts M 1;
2) column resinous shale sample 111 is loaded heated sealing press structure, by exerting pressure, assembly carries out pressure-loaded to resinous shale sample 111, is sealed resinous shale sample 111 by high-temperature high-pressure reaction kettle and sealed-box type electric furnace;
3) open other valve of valve 117,122 and 128 and be now in closed condition; Open vacuum pump 127, heated sealing press structure, oil gas collection mechanism and connecting line are vacuumized, when vacuum tightness arrival-1KPa, valve-off 128, open high-pressure nitrogen bottle 120 pairs of heated sealing press structures, oil gas collection mechanism and connecting line inflated with nitrogen, and carry out air-leakage test; Observe at least 15 minutes, if pressure has decline, impermeability does not reach requirement, then overhaul; If pressure is without decline, then impermeability is good, opens vent valve 130 and discharges nitrogen; Then valve-off 130 and 119, Open valve 128, vacuumizes system, and vacuum repeats 3 ~ 5 times, vacuumizes valve-off 122 and 128 after terminating; Open valve 116 and 117, starting high pressure pump assembly 114 and 115 is driven in high-temperature high-pressure reaction kettle 110 by the local water in local water container 115 epicoele, and make the hydrodynamic pressure of resinous shale sample 111 reach the hydrostatic pressing force value of the degree of depth residing for research purpose layer resinous shale, valve-off 117 and 116;
4) start box electric furnace 109 pairs of resinous shale samples 111 and be heated to 360 DEG C with 1 DEG C/min, and keep constant temperature 24 hours, open simultaneously the 3rd well heater 123 pairs of oil headers 124 heat and the temperature controlling oil header 124 at about 80 DEG C;
5), after thermostatic process terminates, Open valve 122,128 and 131, opens vacuum pump 127 pairs of oil gas collection mechanisms and vacuumizes, when vacuum tightness reaches-1KPa, and valve-off 128,131 and 122; Open valve 117,122 and 131, the fluid in high-temperature high-pressure reaction kettle 110 is successively by oil header 124 and water aspirator 125 and gas collector 129; And the gas that gas collector 129 is collected in this step can be used for doing component analysis;
Valve-off 117, preheats 60 DEG C by the carbon dioxide in secondary heater 102 pairs of supercritical carbon dioxide storage tanks 101; Open valve 103 makes carbon dioxide enter pressurized container 104; Valve-off 103 also starts electrodynamic pump 105 pairs of carbon dioxides and carries out compression and be pressurized to 10MPa; Open valve 106, starts electrodynamic pump 105 by carbon dioxide flooding to high-temperature high-pressure reaction kettle 110, and keeps 2h; Then Open valve 117 and 122, the fluid in high-temperature high-pressure reaction kettle 110 by oil header 124 and water aspirator 125 and gas collector 129, completes a supercritical carbon dioxide extracting process successively;
Repeat supercritical carbon dioxide extracting process 3 ~ 5 times;
6) close all valves, unload oil header 124, weigh and be designated as M 2; Oil offtake then based on the resinous shale of oil shale in-situ production of resources amount evaluation is M 2-M 1, the oil content of this resinous shale is (M 2-M 1)/M 0.
Although invention has been described in conjunction with specific embodiments, but be appreciated that without departing from the scope of the invention, various improvement or replacement can be carried out to it.Especially, only otherwise there is structural conflict, the feature in each embodiment all can be combined with each other, and the combined type feature formed still is within the scope of the present invention.The present invention is not limited to specific embodiment disclosed in literary composition, but comprises all technical schemes fallen in the scope of claim.

Claims (11)

1. an oil content of oil shale experimental apparatus for testing, comprising:
Heated sealing press structure, its for reservoir pressure is applied to resinous shale sample and resinous shale sample is carried out heating generate oily gentle;
Oil gas extraction mechanism, it is connected with the import of heated sealing press structure, gentle for the oil in extraction oil shale sample; With
Oil gas collection mechanism, is connected with the outlet of heated sealing press structure, gentle for collecting from heated sealing press structure oil out.
2. device according to claim 1, is characterized in that, heated sealing press structure comprises:
High-temperature high-pressure reaction kettle, for holding resinous shale sample;
Primary heater, for heating high-temperature high-pressure reaction kettle; With
To exert pressure assembly, act on resinous shale sample with the reservoir pressure that sample during alternative home state is subject to.
3. device according to claim 2, is characterized in that, assembly of exerting pressure comprises:
Upper load cylinder, acts on the upper surface of resinous shale sample to substitute the reservoir pressure be subject at the upper surface of ground in-situ state resinous shale; With
Lower load cylinder, acts on the lower surface of resinous shale sample to substitute the reservoir pressure be subject at the lower surface of ground in-situ state resinous shale.
4. the device according to any one of claims 1 to 3, is characterized in that, supercritical carbon dioxide oil gas extraction mechanism comprises:
Supercritical carbon dioxide storage tank;
Secondary heater, secondary heater is connected with supercritical carbon dioxide storage tank, for heating supercritical carbon dioxide storage tank;
Pressurizer, its import is connected with supercritical carbon dioxide storage tank, and its outlet is connected with the import of heated sealing press structure.
5. device according to claim 4, is characterized in that, described pressurizer comprises:
Pressurized container, its epicoele is connected with supercritical carbon dioxide storage tank by pipeline; With
Electrodynamic pump, is connected with the cavity of resorption of pressurized container, and to the carbon dioxide compression supercharging in pressurized container, the carbon dioxide after supercharging is connected with the import of heated sealing press structure by the road by the outlet of pressurized container.
6. device according to claim 5, is characterized in that, the pipeline between described supercritical carbon dioxide storage tank and pressurized container is provided with the first valve, and the pipeline between the import of described pressurized container and heated sealing press structure is provided with the second valve.
7. the device according to any one of claim 1 ~ 6, is characterized in that, oil gas collection mechanism comprises:
Oil header, is connected with the outlet of heated sealing press structure;
3rd well heater, for keeping the temperature of oil header;
Water aspirator, is connected with the outlet of oil header;
Cold-trap, condenses for making the water vapor in water aspirator;
Gas collector, is connected with the outlet of water aspirator; With
Vacuumize assembly, be connected with the outlet of water aspirator.
8. device according to claim 7, is characterized in that, vacuum device comprises vacuum pump, and the outlet of water aspirator is connected with gas collector through the first arm, and the first arm is provided with valve; The outlet of described water aspirator connects vacuum pump through the second arm, and the second arm is provided with valve.
9. an oil content of oil shale method of testing, adopts the oil content of oil shale proving installation according to any one of claim 1 ~ 8, and comprises the following steps:
1) choose column resinous shale sample, at ambient temperature after dry a period of time, weigh and be designated as M 0; The oil header weight of oil gas collection mechanism of weighing counts M 1;
2) column resinous shale sample is loaded heated sealing press structure, and carry out pressure-loaded and sealing;
3) start vacuum device, heated sealing press structure, oil gas collection mechanism and connecting line vacuumized and carries out air-leakage test, reaching after requirement until vacuum tightness and close vacuum device;
4) connecting line between heated sealing press structure with oil gas collection mechanism is connected with the intermediate receptacle storing local water and the electrodynamic pump be connected with intermediate receptacle by arm, start electrodynamic pump the local water in this intermediate receptacle is injected in the high-temperature high-pressure reaction kettle in heated sealing press structure, the hydrostatic pressing force value of corresponding depth segment when the hydrodynamic pressure that resinous shale sample is subject to reaches ground in-situ state;
5) start heated sealing press structure heat resinous shale sample and keep constant temperature; It is gentle that constant temperature terminates rear unlatching oil gas collection collect oil;
6) extract by oil gas extraction mechanism the oil remained in resinous shale sample gentle, and gentle by oil gas collection collect oil;
7) unload the oil header of oil gas collection mechanism, weigh and be designated as M 2, then the oil offtake of resinous shale sample is M 2-M 1, the oil content of this resinous shale is (M 2-M 1)/M 0.
10. method according to claim 9, is characterized in that, in step 3), first vacuumizes, then by be filled with high pressure nitrogen detect heated sealing press structure, oil gas collection mechanism and between the impermeability of connecting line; When impermeability is good, then carry out the vacuum tightness being evacuated down to needs.
11. methods according to claim 9, it is characterized in that, in step 5), after constant temperature terminates, first the connecting line between sealing load mechanism and oil gas collection mechanism and oil gas collection mechanism are evacuated down to the vacuum tightness of needs, then the oil flowed out from sealing load mechanism by oil gas collection collect is gentle.
CN201410054940.9A 2014-02-18 2014-02-18 Oil content of oil shale experimental apparatus for testing and its method of testing CN104849172B (en)

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