CN202735187U - Instrument for rapidly detecting residual gas quantity by using high temperature method - Google Patents

Instrument for rapidly detecting residual gas quantity by using high temperature method Download PDF

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CN202735187U
CN202735187U CN 201220359546 CN201220359546U CN202735187U CN 202735187 U CN202735187 U CN 202735187U CN 201220359546 CN201220359546 CN 201220359546 CN 201220359546 U CN201220359546 U CN 201220359546U CN 202735187 U CN202735187 U CN 202735187U
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measuring cylinder
instrument
high temperature
gas collection
sample
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张金川
朱亮亮
林腊梅
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Abstract

The utility model provides an instrument for rapidly detecting residual gas quantity by using a high temperature method; the instrument comprises a sample heating tank, a collected gas measuring cylinder, a microwave heating device and a bracket, wherein the sample heating tank and the collected gas measuring cylinder are connected with each other in a sealed way by corresponding a male buckle and a female buckle; the bracket is mounted between the collected gas measuring cylinder and the sample heating tank to support the collected gas measuring cylinder; and the sample heating tank is placed in the microwave heating device. The instrument for rapidly detecting the residual gas quantity by using the high temperature method, provided by the utility model, is greatly improved on aspects of testing success rate, operational feasibility, measuring value reliability, result accuracy and the like; a procedure of crushing and grinding a sample is omitted; contact with air is avoided; moreover, residual or remaining gas in shales or rocks can be rapidly and efficiently released; and the instrument is convenient to move and carry.

Description

Utilize the instrument of high temperature method Fast Measurement residual volume
Technical field
The utility model relates to experimental apparatus and the experimental technique thereof that a kind of gas content is measured, and particularly relates to a kind of instrument that utilizes high temperature method Fast Measurement residual volume.
Background technology
In the present rock gas especially exploratory development as the coal-seam gas in the non-conventional gas field of energy focus and shale gas, air content is a very important parameter, and it is the important evidence of non-conventional reservoir gas fundamental research, resource evaluation analysis and exploratory development strategic plan.Analyze from experimental viewpoint, air content mainly is made of loss gas, resolution gas and residual gas three parts.Wherein, loss gas refers to meet the rock gas that the target core loses to the process that core is placed airtight parsing tank from boring, and usually reaches near core surface sorption gas as main take free gas; After resolution gas referred to that core is got the earth's surface, under the formation temperature conditions of normal pressure and simulation, with the gas summation that analyzing device parsed within certain parsing time, main body was reflected as the adsorbed gas quantity in the core; Residual gas refer to still remain in after normally parsing work stops in the core rock gas or through obtainable rock gas just of longer time, generally, when naturally resolving, it is difficult to parse from sample, even perhaps by some means, may not resolve yet and thoroughly cause still having the part residual gas to residue in the sample.
It is reported that the Coalbed Methane In China residual volume accounts for 10-40% in total gas content, and in the shale of low porosity and low permeability, the resolution speed of gas is relatively slow, the high energy of proportion that residual gas accounts for total air content surpasses 50%, and particularly when core diameter was larger, the parsing time of gas was longer, therefore, no matter be coal petrography or shale etc., the research of residual gas all should be paid attention to, and accurately measures efficiently residual gas and also seems particularly important.Want accurately to record residual gas and the gas sample is carried out various analyses, must at first try every means, as much as possible residual gas is parsed from sample, and measure with rational method.
Now, existing more researcher is studied the measuring method of loss gas and resolution gas content, and solution and evaluation method have been proposed, and a little less than the research relative thin aspect the residual gas, also lack effective method and carry out science, rationally, residual volume is measured accurately.
2008, by State Administration for Quality Supervision and Inspection and Quarantine and the issuing and implementation of national standardization management committee, be numbered the GB (the coal bed gas content Testing Guideline of this criterion referenced United States Bureau of Mines (USBM) direct method (USBM) and U.S. rock gas research institute is revised) of GB/T19559-2008, residual gas content assay method in coal-seam gas has been done some elaborations, now briefly is described below:
A, the assay method of residual volume when resolving at a slow speed:
Naturally after resolving end, smash sample to pieces to 2cm-3cm size, get 300-500g, the ball grinder of packing into sealing is carried out residual volume and is measured.To be fixed on bowl mill for the ball grinder that residual gas is measured, broken 2-4h puts into thermostat, and observed reading and record related data after recovering reservoir temperature afterwards, is resolved mensuration by every 24h interval.Parsing lasts till that continuous 7 days average parsing every day amounts are not more than 10cm 3, residual volume is measured and is stopped.After residual gas was measured and finished, can opening was used the 0.2464mm(60 order) standard sieve screening sample, the quality of the lower coal sample of weighing sieve is carried out residual volume and is calculated.
The mensuration of residual volume when B, quick air assay:
After fast resolving finishes, the broken 60min of coal sample ball mill crushing 15-30min(ash content is higher or high coal rank), put into thermostat and naturally resolve; Repeat later on fragmentation, parsing.Until the tolerance of double fragmentation, parsing is all less than 10cm 3The time, residual volume is measured and is finished.
2009, State Administration for Quality Supervision and Inspection and Quarantine and national standardization management committee issued again the GB that is numbered GB/T 23249-2009 on this basis, i.e. " survey coal seam gas-bearing capacity assay method in period ".The method has been utilized vacuum degasser and ball grinder device, and it is front degassed rear degassed with pulverizing that coal sample has been carried out pulverizing, and finally the two converts to add up and obtains residual volume.
More than be the standard of colliery industry, at present gradually with the field of its application to the measurement of the other types rock gases such as shale gas.In other words, the measurement of residual gas mainly is to use above method to measure at present.
The Estimation and Measurement method of existing residual gas mainly contains 4 kinds, i.e. crush method, graphic interpretation, ball-milling method and curve fitting method.This several method all exists certain theoretical defects and weak point in a way:
1, GB/T 19559-2008 and GB/T 23249-2009, the common ground of these two standards on the residual volume measuring method is all the sample of having resolved will to be taken out from vapor tight tank, continues to resolve after then with bowl mill sample being ground; Difference is that the latter has increased the degassed link of vacuum high-temperature (95 ℃-100 ℃), yet unconventional gas is composed and deposited main body is nanoscale-micron-sized, even crushing is ground, its grade generally also can only reach 60 orders (0.2464mm), and residual gas is resolved smoothly;
2, on the heating mode to sample, the transmission of traditional heating mode heat is inhomogeneous, not thorough, speed is slow, causes sample interior and surface temperature difference large, particularly when core diameter is larger, show particularly evidently, be unfavorable for that residual gas resolves, directly affect measurement result;
If 3 with sample fragmentation or ball milling (also claiming dry grinding), can cause the part residual gas to scatter and disappear in the operating process, and in the operating process, the impact that very difficult deaeration is sneaked into; In addition, even vacuumize, also can not reach completely vacuum state; If when grinding, adopt water mill (also claiming wet-milling), can cause lapping liquid to become muddy, viscosity is large, is unfavorable for equally the parsing of residual gas;
4, grind the heavinesses such as muller of using, carry operation inconvenience, experimental period is relatively long simultaneously, inefficiency;
5, there are a lot of valves, switch, conduit etc. in the experimental provision system, and is extremely numerous and jumbled, so that experimental implementation is very complicated, difficulty is large;
6, other residual volume estimation algorithm, method is based on the crush method expansion as shown, so its degree of reliability is lower; And curve fitting method is a kind of method of carrying out theoretical prediction from the angle of numerical value, and its value reliability seriously is subject to the factor affecting such as length of parsing time, causes having a certain distance between result and the actual value.
In a word, because in the heating process, be heated inhomogeneous, the thermal efficiency is low, in the restriction and process of lapping of heating-up temperature, grinding grade size is got and is changed air that sample pot, the degree of vacuumizing may cause is sneaked into all can affect residual gas measurement result and residual volume with scattering and disappearing of gas etc. gas composition analysis; In addition, in the forecasting process, the imperfection of theoretical calculation model etc. also may cause theory and systematic error, thereby cause residual volume estimation result inaccurate.
This shows that measure pointedly in the situation of residual gas lacking special experimental apparatus and experimental technique, the correlation technique of applying mechanically the coal-seam gas research field remains in problems.And as the air content important component part, experimental apparatus and Research on experimental methods that residual gas is measured are very necessary, it is one of important step of obtaining the air content parameter, research and develop the situation that seriously lags behind the exploratory development production practices with directly changing present pertinent instruments equipment, to the important meaning of exploratory development generation of the especially unconventional reservoir natural gas source of natural gas source.In addition, also can be extended application in metal mine exploitation and methane explosion prevention, petrological study, pedology research, oceanographic research, environmental protection and the fields such as detection, chemical-biological.
The utility model content
The technical problems to be solved in the utility model provides a kind of instrument that utilizes high temperature method Fast Measurement residual volume, make its compact conformation, volume is little, impermeability good, heat temperature raising is rapid, easy and simple to handle, measure accurately, be convenient to move and carry, not only be fit to open-air that also be fit to indoor use and can be specifically designed in the samples such as shale, coal petrography various residual gas and especially measure the collection of weak breath body and accurately measure.
For solving the problems of the technologies described above, a kind of instrument that utilizes high temperature method Fast Measurement residual volume of the utility model, comprise sample heating tank, gas collection measuring cylinder, microwave heating equipment and carriage, wherein: sample heating tank and gas collection measuring cylinder are tightly connected by the box and pin of correspondence; Carriage is installed between gas collection measuring cylinder and the sample heating tank, supports gas collection measuring cylinder; The sample heating tank is positioned in the microwave heating equipment.
As a kind of improvement of the present utility model, described sample heating tank is made of tank body, base and top cover, and at top cover valve port is set; Described gas collection measuring cylinder is made of cylindrical shell and the sealing with scale, offers osculum and air hole in the sealing; Air hole is corresponding with the valve port of sample heating tank, and is provided with switch valve.
Also by adjusting bolt throttle disk and control hand wheel are installed in the sealing of described gas collection measuring cylinder, are equipped with the hole corresponding with the osculum position on throttle disk and the control hand wheel.
Be provided with correspondingly with the osculum position of gas collection measuring cylinder in the described carriage, be used for the tank of the saturated aqueous common salt that the splendid attire gas collection measuring cylinder discharges.
Described gas collection measuring cylinder is coniform.
Described gas collection measuring cylinder inwall cone vertex (vertices) is sharp, and the outer wall cone end is round and smooth.
Described sample heating tank adopts PFA or devitrified glass material.
Described microwave heating equipment comprises casing, top cover, plug and is installed in microwave source in the casing, and is provided with control panel at casing, is provided with transparent window and sample pot leans out the hole at top cover.
After adopting such design, the utility model has the following advantages at least:
1, can realize the continuity that resolution gas and residual gas are measured, saved the broken sample operating process in the normal experiment, thereby avoided the sneaking into of process Air of broken sample, realized not can opening, be not subjected to air impact to obtain residual gas, improved greatly experimental precision;
2, introduce microwave as type of heating, change traditional heat conducting mode of dependence medium, belong to dielectric heating, do not need heat transfer medium, by radiation, can be deep into the inside of material, cause the effects such as electromagnetic oscillation of molecule, increase the motion of molecule, cause the generation of heat, has instantaneous heating, the selectivity heating, thermal inertia is little, penetration power is strong, homogeneous heating, the thermal efficiency is high, do not rely on the heat conduction, process is easy to control, the advantages such as equipment is simple have shortened experimental period greatly, improve conventional efficient, really realized the measurement of the quick residual gas of high temperature;
3, microwave top cover, taper gas collection measuring cylinder and sample heating tank all are that transparent nonmetallic materials (such as PFA, devitrified glass) are made, friction factor little, high temperature resistant (at least 250 ℃), corrosion-resistant, radiation hardness, dielectricity are good, and experiment omnidistance " visual ", directly perceived and be easy to control;
4, adopt intelligent infrared temperature-measuring, accurately sensitive, can regulate as required temperature (0-200 ℃), thereby really realize increasing temperature quick acquisition residual gas (in the conventionally test method, heating-up temperature is general≤100 ℃);
5, energy-conserving and environment-protective than the about 30%-60% of general conventional heating power saving, do not produce waste heat and dust pollution;
6, device structure simple, be convenient to move and carry, operate simple and easy, experimentation is easy to control, be conducive to robotization.
As mentioned above, the utility model is compared with method with existing instrument, test success ratio, operation possibility, measured value reliability and as a result the aspect such as accuracy have and significantly improve, not only economized the crushing grinding sample link, avoided the contact of air, and can extremely quickly and efficiently remaining in shale, the coal petrography or residual gas be parsed, convenient mobile the carrying of instrument, the indoor and outdoor is all easy to use.
Description of drawings
Above-mentioned only is the general introduction of technical solutions of the utility model, and for can clearer understanding technological means of the present utility model, the utility model is described in further detail below in conjunction with accompanying drawing and embodiment.
Fig. 1 is the apparatus structure synoptic diagram that the utility model utilizes high temperature method Fast Measurement residual volume.
Embodiment
See also shown in Figure 1ly, a kind of instrument that utilizes high temperature method Fast Measurement residual volume of the utility model comprises sample heating tank 1, gas collection measuring cylinder 2, microwave heating equipment 3 and carriage 4.Wherein, sample heating tank 1 and gas collection measuring cylinder 2 can adopt structure and the connected mode of patent ZL201010137275.1, box and pin by correspondence is tightly connected, carriage 4 is installed between gas collection measuring cylinder 2 and the sample heating tank 1, support gas collection measuring cylinder 2, sample heating tank 1 is positioned in the microwave heating equipment 3.
Specifically, sample heating tank 1 is by tank body 12, consist of with the top cover 13 that is connected with the tank body top cover with base 11 that tank body one end is fixedly connected with, and at top cover 13 valve port 14 is set.This sample heating tank 1 can be translucent by PFA, devitrified glass etc.-and transparent, friction factor is little, high temperature resistant (250 ℃), corrosion-resistant, radiation hardness, dielectricity nonmetallic materials good, excellent performance are made.
Gas collection measuring cylinder 2 is by sealing and indicate the cylindrical shell 26 of scale mark and be provided with osculum and the sealing of air hole 22 consists of.Air hole is corresponding with the valve port 14 of sample heating tank 1, and is provided with switch valve 25 at the air hole place.Gas collection measuring cylinder 2 is preferably coniform that inwall cone vertex (vertices) is sharp, the outer wall cone end is round and smooth, measures, and prevent more accurately the exterior tip position when convenient amount when gas is few and collide with.In addition, also can in the sealing 22 of gas collection measuring cylinder 2 throttle disk 23 and control hand wheel 21 be installed by adjusting bolt 24, be equipped with the hole corresponding with the osculum position on throttle disk 23 and the control hand wheel 21.
Microwave heating equipment 3 can be comprised of casing 33, top cover 34, attaching plug 31 and the microwave source that is installed in the casing, and at casing 33 control panel 32 is set, and at top cover 34 sample pot is set and leans out the hole.Wherein, microwave source is take magnetron as core, and experiment is observed and controlled to the microwave leakage preventing technology that casing 33 and top cover 34 adopt take choking structure as core, and adopt the Intelligent infrared temperature control, and the visual window that transparent material is made is set at this top cover 34 conveniently at any time.
Can be provided with the tank corresponding with the osculum position of gas collection measuring cylinder 2 in the carriage 4, support on the one hand and stable taper gas collection measuring cylinder 2, can be used on the other hand the saturated aqueous common salt of discharging in the splendid attire gas collection measuring cylinder 2.
The method of utilizing high temperature method Fast Measurement residual volume that the utility model utilizes above-mentioned instrument to carry out may further comprise the steps:
(1) utilize the sample heating tank to resolve experiment, better, before resolving the experiment beginning, can in the sample sealable tank, fill saturated aqueous common salt and an amount of stirrer;
(2) open the top cover of microwave heating equipment, under the condition of not opening the sample heating tank, the sample heating tank that has just carried out the parsing experiment is put into microwave heating equipment together with sample, build the top cover with the transparent visual window;
(3) will fill saturated aqueous common salt in the gas collection measuring cylinder, and open and regulate the osculum of gas collection measuring cylinder according to the scheme of patent ZL201010137275.1 record, by box and pin gas collection measuring cylinder and sample heating tank are tightly connected again;
(4) power supply of connection microwave heating equipment is set heating-up temperature and heat time heating time, begins the sample in the sample heating tank is carried out high-temperature heating;
(5) gas volume and other related experiment data in observation and the record gas collection measuring cylinder realize the efficient of the sample residual gass such as shale, coal petrography accurately measured.
Treating that gas volume is advanced the speed (approaches zero) less than to a certain degree the time, outage, and close osculum and gas collection measuring cylinder and the tank connected valve port of sample of gas collection measuring cylinder.
The above; it only is preferred embodiment of the present utility model; be not that the utility model is done any pro forma restriction, those skilled in the art utilize the technology contents of above-mentioned announcement to make a little simple modification, equivalent variations or modification, all drop in the protection domain of the present utility model.

Claims (8)

1. an instrument that utilizes high temperature method Fast Measurement residual volume is characterized in that comprising sample heating tank, gas collection measuring cylinder, microwave heating equipment and carriage, wherein:
Sample heating tank and gas collection measuring cylinder are tightly connected by the box and pin of correspondence;
Carriage is installed between gas collection measuring cylinder and the sample heating tank, supports gas collection measuring cylinder;
The sample heating tank is positioned in the microwave heating equipment.
2. the instrument that utilizes high temperature method Fast Measurement residual volume according to claim 1 is characterized in that:
Described sample heating tank is made of tank body, base and top cover, and at top cover valve port is set;
Described gas collection measuring cylinder is made of cylindrical shell and the sealing with scale, offers osculum and air hole in the sealing;
Air hole is corresponding with the valve port of sample heating tank, and is provided with switch valve.
3. the instrument that utilizes high temperature method Fast Measurement residual volume according to claim 2, it is characterized in that also by adjusting bolt throttle disk and control hand wheel being installed in the sealing of described gas collection measuring cylinder, be equipped with the hole corresponding with the osculum position on throttle disk and the control hand wheel.
4. the instrument that utilizes high temperature method Fast Measurement residual volume according to claim 2 is characterized in that the osculum position that is provided with in the described carriage with gas collection measuring cylinder is corresponding, is used for the tank of the saturated aqueous common salt that the splendid attire gas collection measuring cylinder discharges.
5. the instrument that utilizes high temperature method Fast Measurement residual volume according to claim 1 is characterized in that described gas collection measuring cylinder is coniform.
6. the instrument that utilizes high temperature method Fast Measurement residual volume according to claim 5 is characterized in that described gas collection measuring cylinder inwall cone vertex (vertices) is sharp, and the outer wall cone end is round and smooth.
7. the instrument that utilizes high temperature method Fast Measurement residual volume according to claim 1 is characterized in that described sample heating tank adopts PFA or devitrified glass material.
8. the instrument that utilizes high temperature method Fast Measurement residual volume according to claim 1, it is characterized in that described microwave heating equipment comprises casing, top cover, plug and is installed in the interior microwave source of casing, and be provided with control panel at casing, be provided with transparent window and sample pot leans out the hole at top cover.
CN 201220359546 2012-07-23 2012-07-23 Instrument for rapidly detecting residual gas quantity by using high temperature method Expired - Lifetime CN202735187U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102768165A (en) * 2012-07-23 2012-11-07 张金川 Instrument and method for quickly detecting residual gas volume by high temperature method
CN104914030A (en) * 2015-07-06 2015-09-16 中国地质大学(北京) Whole-journey gas-proof gas content measuring instrument and method for using the same to measure residual gas of rock sample
CN104977224A (en) * 2015-07-06 2015-10-14 中国地质大学(北京) High-temperature phase-control desorption instrument

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102768165A (en) * 2012-07-23 2012-11-07 张金川 Instrument and method for quickly detecting residual gas volume by high temperature method
CN104914030A (en) * 2015-07-06 2015-09-16 中国地质大学(北京) Whole-journey gas-proof gas content measuring instrument and method for using the same to measure residual gas of rock sample
CN104977224A (en) * 2015-07-06 2015-10-14 中国地质大学(北京) High-temperature phase-control desorption instrument
CN104977224B (en) * 2015-07-06 2017-12-26 中国地质大学(北京) A kind of phased desorption instrument of high temperature

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Granted publication date: 20130213