CN103575834B - Enrichment device and enrichment method for light hydrocarbon in dry gas - Google Patents
Enrichment device and enrichment method for light hydrocarbon in dry gas Download PDFInfo
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- CN103575834B CN103575834B CN201210271615.9A CN201210271615A CN103575834B CN 103575834 B CN103575834 B CN 103575834B CN 201210271615 A CN201210271615 A CN 201210271615A CN 103575834 B CN103575834 B CN 103575834B
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Abstract
The invention discloses an enrichment device and an enrichment method for a light hydrocarbon in dry gas. The device comprises a dry gas storage pot, a six-way valve, an enrichment pipe, a purifier and two heating hearths, wherein the dry gas storage pot is arranged in one heating hearth; the purifier and the six-way valve are arranged in the other heating hearth; the enrichment pipe is arranged in a cold trap; the cold trap is arranged outside the heating hearths; the enrichment pipe is connected with the six-way valve; the dry gas storage pot is connected with the purifier and then is connected with the six-way valve; a carrier gas introduction pipeline and a back-blowing gas introduction pipeline are arranged outside the heating hearths; the carrier gas introduction pipeline enters the heating hearth to be connected with a flowing valve; the back-blowing gas introduction pipeline enters the heating hearth to be communicated with a pipeline between the purifier and the six-way valve; the six-way valve is connected with a chromatographic instrument and a ventilation cabinet respectively. The method comprises the following step that dry gas is enriched and then enters the chromatographic instrument to be subjected to light hydrocarbon analysis. According to the enrichment device and the enrichment method for the light hydrocarbon in the dry gas, fingerprint information of the light hydrocarbon lower than a detection limit in a conventional chromatographic analysis can be obtained and real and complete data information is obtained.
Description
Technical field
The present invention relates to petroleum exploration domain, say further, relate to enriching apparatus and the enrichment method of lighter hydrocarbons in a kind of dry gas.
Background technology
The associated natural gas in oil field, through dehydration, purification and process for recovering light hydrocarbon, after extracting liquefied gas and lightweight oil, principal ingredient is that the process rock gas of methane is dry gas.In general, in rock gas, methane content is dry gas more than 90%.
At present, the analysis of rock gas, is all generally gather gas sample at normal temperature and pressure drainage or small steel cylinder method, directly carries out gas chromatographic analysis with syringe sampling.Such conventional method, concerning general moisture, along with the raising of chromatogram sensitivity, likely analyzes more light hydrocarbon component, is applied to geologic interpretation.But for dry gas, its lighter hydrocarbons composition is based on the minority such as methane, ethane component, part dry gas methane content is other hydrocarbon gas content very micro-(can be little of the ppt order of magnitude) up to more than 95%, and gas chromatogram often only shows a few component such as methane, ethane.The information provided due to stratographic analysis is few, and can not obtain the fingerprint characteristic and the parameter that reflect lighter hydrocarbons character, the geochemical comparison that carry out rock gas just also exists very large difficulty, and GEOLOGICAL APPLICATION is very limited.
Summary of the invention
For solving problems of the prior art, the invention provides enriching apparatus and the enrichment method of lighter hydrocarbons in a kind of dry gas.Enrichment can be carried out to lighter hydrocarbons in dry gas, the finger print information lower than the lighter hydrocarbons part of detectability in conventional chromatography evaluation can be obtained, by blowback, the solvent effect of methane can be removed, propane and peak afterwards are effectively separated, obtain more truly perfect data information.
An object of the present invention is to provide the enriching apparatus of lighter hydrocarbons in a kind of dry gas.
Described device comprises: dry gas hold-up vessel, six-way valve, enrichment pipe, clarifier and heating furnace, and heating furnace is two, and dry gas hold-up vessel is arranged in a heating furnace, clarifier and six-way valve are arranged in another heating furnace,
Described enrichment pipe is arranged in cold-trap, and cold-trap is arranged on outside heating furnace, and enrichment pipe is connected with six-way valve;
Dry gas hold-up vessel is connected with six-way valve after connecting clarifier;
Heating furnace is outside equipped with carrier gas and passes into pipeline and blowback air passes into pipeline, and carrier gas passes into pipeline and enters in heating furnace and be connected with flowing valve, and blowback air passes into pipeline and enters that heating furnace is interior to be communicated with the pipeline between clarifier and six-way valve;
Six-way valve connects chromatograph and vent cabinet respectively;
The connection status of six-way valve:
During enrichment blowback, dry gas passes into and is communicated with enrichment pipe, and the enrichment pipe other end is communicated with vent cabinet, and carrier gas passes into and is communicated with chromatograph;
When sample introduction is analyzed, carrier gas passes into and is communicated with enrichment pipe, and the enrichment pipe other end connects chromatograph.
Pipeline between described dry gas hold-up vessel and clarifier is provided with reduction valve A and flowrate control valve A;
Described blowback air passes on pipeline and is provided with reduction valve B and flowrate control valve B.
Wherein, described dry gas hold-up vessel is the instrument of common storage dry gas in prior art, as small steel cylinder etc.The in-built water absorbing agent of described clarifier is the moisture in order to adsorb in dry gas.Pipeline in device is sealing pipeline, can adopt all applicable materials in prior art, can preferred stainless-steel tube, the preferred stainless-steel tube of enrichment pipe.
Two of object of the present invention is to provide the enrichment method of lighter hydrocarbons in a kind of dry gas.
Comprise:
(1) dry gas is after heating, removing moisture, enters enrichment pipe enrichment by six-way valve;
(2) pass into blowback air and purge the gas do not liquefied;
(3) heat cold-trap, brought into chromatograph by the dry gas of enrichment by carrier gas and detect.
In step (1), dry gas is heated to 60 DEG C ~ 100 DEG C by heating furnace, and the flow that dry gas enters enrichment pipe is 4.0 ~ 5.0ml/min, and condenser temperature is-70 DEG C ~-90 DEG C, and enrichment time is 25min ~ 35min;
In step (2), blowback air purge time is 4.5min ~ 5.5min, and blowback air flow is 3.0 ~ 3.5ml/min;
In step (3), cold-trap is heated to 150 ~ 200 DEG C, keeps 9.5min ~ 10.5min.
The heating-up temperature of two heating furnaces is 60 DEG C ~ 100 DEG C.
Method mainly comprises two processes, enrichment blowback process and sample introduction analytic process,
Enrichment blowback process: small steel cylinder (in-built dry gas) is placed in preheating in heating furnace, reduction valve A and flowrate control valve A is regulated to make gas flow reach stationary value, dry gas is removed moisture through clarifier and is then entered six-way valve and enrichment pipe, set the chilling temperature of cold-trap, make dry gas in enrichment pipe, carry out lighter hydrocarbons liquefaction enrichment, at the rear 5min of enrichment state, reduction valve B and flowrate control valve B is regulated to make blowback air flow reach stationary value, gas (the mainly methane utilizing blowback air to purge not liquefy, ethane), the dry gas be not liquefied and blowback air absorb through alkali lye bottle and wherein enter vent cabinet emptying after acidic components.
Sample introduction analytic process: enrichment blowback process terminates rear rapid switching six-way valve, utilizes the heating function of cold-trap to improve rapidly enrichment pipe temperature, makes the lighter hydrocarbons Quick-gasifying of liquefaction, and enter chromatograph with carrier gas and carry out light hydrocarbon analysis.
Small steel cylinder heating furnace preheat temperature in above-mentioned enrichment blowback process is 60 DEG C ~ 100 DEG C, pipeline heating furnace temperature is 60 DEG C ~ 100 DEG C, the flow that dry gas enters enrichment pipe is 4.0 ~ 5.0ml/min, condenser temperature is-80 DEG C, enrichment time is 30min, blowback air purge time is 5min, and blowback air flow is 3.0 ~ 3.5ml/min.In above-mentioned sample introduction analytic process, condenser temperature is 150 ~ 200 DEG C, keeps 10min.
Always whole process carrier gas passes into, and after just six-way valve switches, institute changes through passage; Time sample introduction is analyzed, pass into blowback air.
Adopt apparatus of the present invention and method can carry out enrichment to lighter hydrocarbons in dry gas, the finger print information lower than the lighter hydrocarbons part of detectability in conventional chromatography evaluation can be obtained, pass through blowback, the solvent effect of methane can be removed, propane and peak afterwards are effectively separated, obtain more truly perfect data information.By these data, obtain the fingerprint characteristic and the parameter that reflect lighter hydrocarbons character, the genetic type of rock gas, evolution grade can be reflected, for gas/gas, gas/source contrast, in the multiple GEOLOGICAL APPLICATION such as the preservation condition of reflection oil gas, expand the research range to rock gas, enrich geologic information.
Accompanying drawing explanation
Fig. 1 enriching apparatus structural representation
Fig. 2-1 enrichment blowback process six-way valve connection diagram
Fig. 2-2 sample introduction analytic process six-way valve connection diagram
The lighter hydrocarbons chromatogram of Fig. 3-1 comparative example
The lighter hydrocarbons chromatogram of Fig. 3-2 embodiment
Description of reference numerals:
101 dry gas hold-up vessels, 102 reduction valve A, 103 small steel cylinder heating furnaces, 104 flowrate control valve A, 105 pipeline heating furnaces, 106 clarifiers (in-built water absorbing agent), 107 six-way valves, 108 enrichment pipes, 109 cold-traps (band heating), 110 alkali lye bottles, 111 reduction valve B, 112 flowrate control valve B, 113 vent cabinets, 114 chromatographs
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment:
As shown in Figure 1, the enriching apparatus of lighter hydrocarbons in a kind of dry gas, comprise: dry gas hold-up vessel 101, six-way valve 107, enrichment pipe 108, clarifier 106 and heating furnace, heating furnace is two, dry gas hold-up vessel 101 is arranged in a heating furnace, clarifier 106 and six-way valve 107 are arranged in another heating furnace
Described enrichment pipe 108 is arranged in cold-trap 109, and cold-trap 109 is arranged on outside heating furnace, and enrichment pipe 108 is connected with six-way valve 107;
Dry gas hold-up vessel 101 is connected with six-way valve 107 after connecting clarifier 106;
Heating furnace is outside equipped with carrier gas and passes into pipeline a and blowback air passes into line b, and carrier gas passes into pipeline a and enters in heating furnace and be connected with flowing valve 107, and blowback air passes into line b and enters that heating furnace is interior to be communicated with the pipeline between clarifier 106 and six-way valve 107;
Six-way valve 107 connects chromatograph 114 and vent cabinet 113 respectively;
The connection status of six-way valve 107:
During enrichment blowback, dry gas passes into and is communicated with enrichment pipe 108, and enrichment pipe 108 other end is communicated with vent cabinet 113, and carrier gas passes into and is communicated with chromatograph 114;
When sample introduction is analyzed, carrier gas passes into and is communicated with enrichment pipe 108, and enrichment pipe 108 other end connects chromatograph.
Pipeline between described dry gas hold-up vessel 101 and clarifier 106 is provided with reduction valve A102 and flowrate control valve A104;
Described blowback air passes on pipeline and is provided with reduction valve B111 and flowrate control valve B112.
Wherein dry gas hold-up vessel is small steel cylinder, and clarifier is the glass tube that inside is provided with water absorbing agent.
All pipelines are 1/16 inch of stainless-steel tube; 108 enrichment pipe materials are 1/16 inch of stainless-steel tubes, and stretching length is 15cm;
Enriching step is as follows:
First we have chosen an aridity coefficient and reach the dry gas of 99.7% as laboratory sample gas A,
Regulating enriching apparatus makes it enter duty, and setting two heating furnace preheat temperatures is 100 DEG C, and condenser temperature is-80 DEG C, and reduction valve A, flowrate control valve A, reduction valve B and flowrate control valve B are in closed condition, and six-way valve is in enrichment blowback state.
Enrichment blowback process: the dry gas hold-up vessel that sample gas A is housed to be placed in heating furnace first preheating 30min at 100 DEG C of temperature, then open and regulate reduction valve A and flowrate control valve A until 107 six-way valve No. 4 positions, the flow of sample gas A is 4.5ml/min, sample gas A removes moisture through clarifier and then enters six-way valve and enrichment pipe, because enrichment pipe is arranged in cold-trap, so dry gas carries out lighter hydrocarbons liquefaction enrichment in low temperature enrichment pipe, enrichment time is 30min
At the last 5min of enrichment; Close reduction valve A and flowrate control valve A, open and regulate reduction valve B and flowrate control valve B until the flow of six-way valve No. 4 position blowback airs is 3.5ml/min, the gas (mainly methane, ethane) utilizing blowback air to purge not liquefy, blowback time 5min.The sample gas A be not liquefied in said process and blowback air enter vent cabinet emptying after alkali lye bottle.Alkali lye bottle act as and absorbs acidic components in sample gas A.
Sample introduction analytic process: enrichment blowback process terminates rear rapid switching six-way valve, now reduction valve B and flowrate control valve B remains stationary, heating cold-trap improves rapidly enrichment pipe temperature to 200 DEG C, maximum temperature keeps 10min, make the lighter hydrocarbons Quick-gasifying of liquefaction, and enter chromatograph with carrier gas and carry out light hydrocarbon analysis.
Comparative example:
Test specimen gas A directly sends into chromatograph without enrichment and carries out light hydrocarbon analysis.
Fig. 3-1 and Fig. 3-2 is sample gas A two kinds different input mode 10 ~ 62min lighter hydrocarbons chromatograms.
Can find out from the contrast of Fig. 3-1 and Fig. 3-2: direct injected cannot catch the information of light hydrocarbon in natural gas part; And owing to carrying out enrichment to sample, C
3the response of rear compound obviously strengthens, C
10peak still can clearly be identified, owing to having carried out blowback, methane, ethane all can be blown off major part, and the chromatogram making propane later is effectively separated, and the information of the spectrogram therefore obtained is more clear, obtains more truly perfect data information.By these data, obtain the fingerprint characteristic and the parameter that reflect lighter hydrocarbons character, enrich geologic information.
Claims (7)
1. the enriching apparatus of lighter hydrocarbons in dry gas, described device comprises: dry gas hold-up vessel, six-way valve, enrichment pipe, clarifier and heating furnace, and enrichment pipe is connected with six-way valve, and dry gas hold-up vessel is connected with six-way valve after connecting clarifier, it is characterized in that:
Heating furnace is two, and dry gas hold-up vessel is arranged in a heating furnace, clarifier and six-way valve are arranged in another heating furnace;
Described enrichment pipe is arranged in cold-trap, and cold-trap is arranged on outside heating furnace;
Heating furnace is outside equipped with carrier gas and passes into pipeline and blowback air passes into pipeline, and carrier gas passes into pipeline and enters in heating furnace and be connected with six-way valve, and blowback air passes into pipeline and enters that heating furnace is interior to be communicated with the pipeline between clarifier and six-way valve;
Six-way valve connects chromatograph and vent cabinet respectively;
The connection status of six-way valve:
During enrichment blowback, dry gas passes into and is communicated with enrichment pipe, and the enrichment pipe other end is communicated with vent cabinet, and carrier gas passes into and is communicated with chromatograph;
When sample introduction is analyzed, carrier gas passes into and is communicated with enrichment pipe, and the enrichment pipe other end connects chromatograph.
2. the enriching apparatus of lighter hydrocarbons in dry gas as claimed in claim 1, is characterized in that:
Pipeline between described dry gas hold-up vessel and clarifier is provided with reduction valve A and flowrate control valve A;
Described blowback air passes on pipeline and is provided with reduction valve B and flowrate control valve B.
3. adopt an enrichment method for the enriching apparatus of lighter hydrocarbons in dry gas as claimed in claim 1 or 2, it is characterized in that described method comprises:
(1) open reduction valve A and flowrate control valve A, dry gas, after heating, removing moisture, enters enrichment pipe enrichment by six-way valve;
(2) close reduction valve A and flowrate control valve A, open reduction valve B and flowrate control valve B, pass into blowback air and purge the gas do not liquefied;
(3) heat cold-trap, brought into chromatograph by the dry gas of enrichment by carrier gas and detect.
4. enrichment method as claimed in claim 3, is characterized in that:
In step (1), dry gas is heated to 60 DEG C ~ 100 DEG C by heating furnace, and the flow that dry gas enters enrichment pipe is 4.0 ~ 5.0ml/min, and condenser temperature is-70 DEG C ~-90 DEG C, and enrichment time is 25min ~ 35min.
5. enrichment method as claimed in claim 4, is characterized in that:
In step (2), blowback air purge time is 4.5min ~ 5.5min, and blowback air flow is 3.0 ~ 3.5ml/min.
6. enrichment method as claimed in claim 5, is characterized in that:
In step (3), cold-trap is heated to 150 ~ 200 DEG C, keeps 9.5min ~ 10.5min.
7. enrichment method as claimed in claim 3, is characterized in that:
The flow that dry gas enters enrichment pipe is controlled by reduction valve A and flowrate control valve A;
Blowback air flow is controlled by reduction valve B and flowrate control valve B.
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| CN201210271615.9A CN103575834B (en) | 2012-08-01 | 2012-08-01 | Enrichment device and enrichment method for light hydrocarbon in dry gas |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105784889B (en) * | 2014-12-25 | 2018-11-30 | 中国科学院广州能源研究所 | The quick analysis system and method for thick gas tar oil content |
| CN105548416B (en) * | 2015-12-21 | 2018-03-13 | 中国石油天然气股份有限公司 | Method for analyzing hydrogen isotopes of light hydrocarbon monomer hydrocarbon in natural gas and light hydrocarbon enrichment device |
| CN110470527B (en) * | 2018-05-11 | 2022-07-15 | 中国石油化工股份有限公司 | Dry gas quantitative enrichment system and method |
| CN110095545B (en) * | 2019-05-25 | 2021-11-23 | 东北石油大学 | Millimeter-level sample oil source direct analysis and comparison system for tight reservoir |
| CN112816272B (en) * | 2020-12-30 | 2024-08-27 | 杭州谱育科技发展有限公司 | Gas enrichment method and device |
| CN115108879A (en) * | 2021-03-23 | 2022-09-27 | 中国石油化工股份有限公司 | Light hydrocarbon component separation, collection and online quantification device and method |
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