CN103245540A - Hydrate reaction kettle suitable for direct measurement in terahertz spectrum - Google Patents
Hydrate reaction kettle suitable for direct measurement in terahertz spectrum Download PDFInfo
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- CN103245540A CN103245540A CN2013101639484A CN201310163948A CN103245540A CN 103245540 A CN103245540 A CN 103245540A CN 2013101639484 A CN2013101639484 A CN 2013101639484A CN 201310163948 A CN201310163948 A CN 201310163948A CN 103245540 A CN103245540 A CN 103245540A
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Abstract
The invention relates to a hydrate reaction kettle suitable for direct measurement in a terahertz spectrum. The reaction kettle comprises a cooling housing which consists of a shell and a through type pipeline transversely arranged in the shell. A seal chamber for accommodating a cooling medium is formed between the outer wall of the pipeline and the shell. A first quartz window and a second quartz window are axially and fixedly arranged in the pipeline at an interval, and the quartz windows are hermetically and fixedly connected with the inner wall of the pipeline. A hydrate generation space is formed between the first and second quartz windows and is hermetically communicated with a gas supply tube and a water supply tube. The reaction kettle further comprises a pressure sensing element and a temperature sensing element for monitoring the pressure and temperature in the hydrate generation space. The reaction kettle integrates production and measurement of hydrate, and the hydrate generated in the reaction kettle is directly measured in a terahertz light path, so that the steps of taking out and tabletting in a low temperature room are canceled, the time and cost are saved, and the probability that a hydrate sample is interfered is avoided.
Description
Technical field
The invention relates to a kind of hydrate reaction still, relate in particular to a kind of hydrate reaction still that is applicable to that tera-hertz spectra is directly measured.
Background technology
Gas hydrate (being commonly called as combustible ice) are a kind of natural ice shape solids that is present in a large number, inflammable gass such as a large amount of methane, ethane are rich in inside, estimate that carbon content is 2 times that the carbon reserves are verified in the present whole world in the global gas hydrate, be called as " future source of energy ".Combustible ice has different extraction values according to the difference of constituent and the difference of alkane content, therefore, is necessary before exploitation combustible ice to be carried out component and the content analysis of alkane.Utilizing Terahertz (Tera hz) technology that gas hydrate are characterized is present emerging characterizing method.As be published in the document " terahertz time-domain spectroscopy be used for structure I I type gas hydrate " (Treahertz Time Domain Spectroscopy for Structure-II Gas Hydrates) of Appl Phys Express 2 (2009) 122303, document author is: Kei Takeya, Caihong Zhang, Lwao Kawayama, Hironaru Murakami, Peter Uhd Jepsen, Jian Chen, Peiheng Wu, Kazunari Ohgaki, and Masayoshi Tonouchi etc.
But doing experiment up to now all is to generate combustible ice in advance in reactor, takes out combustible ice then from reactor, and compressing tablet in low temperature chamber is put into the surveying instrument of low temperature chamber and measured; Because combustible ice takes out and measuring process from reactor, need carry out in the low temperature chamber of a low temperature or high pressure, building and moving of described low temperature chamber all needs very high expense, and measuring process is also inconvenient, therefore, the experiment to terahertz light spectrometry hydrate causes puzzlement.
Thus, the inventor relies on experience and the practice of being engaged in relevant industries for many years, proposes a kind of hydrate reaction still that is applicable to that tera-hertz spectra is directly measured, to overcome the defective of prior art.
Summary of the invention
The object of the present invention is to provide a kind of hydrate reaction still that is applicable to that tera-hertz spectra is directly measured, the catchment compound production and measuring in one of this reactor, hydrate is directly measured in the Terahertz light path after generating in reactor, saved the step of taking-up, compressing tablet in low temperature chamber, save time and cost, and avoided the disturbed possibility of hydrate sample.
Another object of the present invention is to provide a kind of hydrate reaction still that is applicable to that tera-hertz spectra is directly measured, the foundation of having omitted low temperature chamber has reduced experimental cost.
The object of the present invention is achieved like this, and a kind of hydrate reaction still that is applicable to that tera-hertz spectra is directly measured, described reactor comprise a cooling housing, and described cooling housing is made of the pipeline of shell and a perforation of horizontally set in this shell; Form the seal chamber that holds heat eliminating medium between the outer wall of described pipeline and the described shell; In described pipeline, axially be fixed with first quartz window and second quartz window that arrange at interval, the shape of cross section of the shape of cross section of described two quartz windows and size and described pipeline and measure-alike, and quartz window and inner-walls of duct are sealedly and fixedly connected; Form the hydrate span between described first quartz window and second quartz window; Described hydrate span sealing is communicated in air supply pipe and feed pipe; Described reactor also includes pressure responsive element and the temperature sensitive member of monitoring hydrate span internal pressure and temperature.
In a preferred embodiments of the present invention, fix sheathed certain position spacer ring in the inner-walls of duct between described first quartz window and second quartz window; The inner face that described first quartz window is relative with second quartz window is resisted against the both sides of location spacer ring respectively; The thickness of described location spacer ring is 0.2～5mm.
In a preferred embodiments of the present invention, the outer face of described first quartz window and second quartz window is respectively by first fixed part and second fixed part location and fixing that are connected on the inner-walls of duct.
In a preferred embodiments of the present invention, the axially interior outer face of described first quartz window and second quartz window is parallel mutually.
In a preferred embodiments of the present invention, described first fixed part and second fixed part are loop configuration.
In a preferred embodiments of the present invention, the xsect of described pipeline is circle, rectangle or polygon.
In a preferred embodiments of the present invention, described cooling housing is made by stainless steel material.
In a preferred embodiments of the present invention, described heat eliminating medium is circulating coolant, and described seal chamber top is provided with the circulating coolant inlet, and described seal chamber bottom is provided with the circulating coolant flow export.
In a preferred embodiments of the present invention, described air supply pipe is connected with air-supplying valve, tensimeter, reduction valve, flowmeter and gas cylinder; Described feed pipe is connected with water supply valve; Described pressure responsive element and temperature sensitive member are connected with control and display device.
In a preferred embodiments of the present invention, be positioned at and be respectively equipped with an insulation thin slice on the cooling housing sidewall of pipe ends; Described insulation thin slice is made by tygon or quartz material; Described insulation thin slice both sides smooth smooth and with the cooling housing sidewall closely contact; Form an airtight incubation cavity respectively in the pipeline of each insulation thin slice inboard, be filled with nitrogen or inert gas in the described airtight incubation cavity.
From the above mentioned, the present invention is applicable to the hydrate reaction still that tera-hertz spectra is directly measured, its compound production and measuring in one of catchmenting, after generating in reactor, can directly in the Terahertz light path, measure in hydrate, saved the step of taking-up, compressing tablet in low temperature chamber, save time and cost, and avoided the disturbed possibility of hydrate sample.The hydrate sample that generates in reactor is the smooth parallel laminar solid in two sides, is fit to utilize the Terahertz instrument to measure.The quartz window of both sides absorbs tera-hertz spectra is low, can directly measure in the Terahertz light path.
Description of drawings
The following drawings only is intended to the present invention done and schematically illustrates and explain, not delimit the scope of the invention.Wherein:
Fig. 1: the structural representation that is applicable to the hydrate reaction still that tera-hertz spectra is directly measured for the present invention.
Fig. 2: be the side-looking structural representation of Fig. 1.
Fig. 3: be the structural representation of a kind of fixed form of quartz window among the present invention.
Fig. 4: be the structural representation of the another kind of fixed form of quartz window among the present invention.
Embodiment
Understand for technical characterictic of the present invention, purpose and effect being had more clearly, now contrast description of drawings the specific embodiment of the present invention.
As shown in Figure 1 and Figure 2, the present invention proposes a kind of hydrate reaction still 100 that is applicable to that tera-hertz spectra is directly measured, described reactor 100 comprises a cooling housing 1, and described cooling housing 1 is made of the pipeline 12 of shell 11 and a perforation of horizontally set in this shell 11; Form the seal chamber 8 that holds heat eliminating medium between the outer wall of described pipeline 12 and the described shell 11; In the present embodiment, described heat eliminating medium is circulating coolant, and described seal chamber 8 tops are provided with circulating coolant inlet 81, and described seal chamber 8 bottoms are provided with circulating coolant flow export 82; In described pipeline 12, axially be fixed with first quartz window 21 and second quartz window 22 that arrange at interval, the shape of cross section of described two quartz windows 21,22 shape of cross section and size and described pipeline 12 and measure-alike, and quartz window and inner-walls of duct are sealedly and fixedly connected, in order to improve sealing effectiveness, between described quartz window sidewall and pipeline 12 inwalls O-ring seal (not shown) can be set; Form the hydrate span 3 between described first quartz window 21 and second quartz window 22; In the present embodiment, the hydrate span 3 pressure that can bear is not less than 5MPa; In order to improve its bearing resistance, described first quartz window 21 and second quartz window 22 should be made thicklyer, and the wall thickness of described pipeline 12 also should be enough thick; The described hydrate span 3 sealings are communicated in air supply pipe 4 and feed pipe 5, and described air supply pipe 4 is connected with air-supplying valve, tensimeter, reduction valve, flowmeter and gas cylinder (being existing structure, not shown); Described feed pipe 5 is connected with the water supply valve (not shown); Described reactor 100 also includes pressure responsive element and the temperature sensitive member of monitoring hydrate span internal pressure and temperature; Described cooling housing 1 bottom is provided with support 9.
The above-mentioned hydrate reaction still 100 that is applicable to that tera-hertz spectra is directly measured has multiple using method in use, now describes its use with a kind of method wherein.
During on-test, by the hydrate span inner feeding water of feed pipe 5 to reactor 100, add water and should not fill up whole hydrate reaction space earlier, but should not be very little, amount of water should be greater than 3/4 of hydrate reaction space; After water flowing finishes, close the water supply valve of feed pipe 5; 3 feed and to desire to produce the hydrate desired gas (for example: methane gas), in order to keep the constant voltage of 3MPa, venting process is not interrupted before reaction finishes to the hydrate reaction space with pressure 3MPa by air supply pipe 4; In the present embodiment, described pressure responsive element and temperature sensitive member are connected with control and display device; Observe force value by the display device that pressure responsive element connects, after pressure stability, circulating coolant begins circulation and is the reaction compartment refrigeration; The a little higher than zero degrees celsius of circulating coolant temperature, but the highlyest be no more than 2 degrees centigrade above freezing; Along with circulating coolant is lowered the temperature to the hydrate reaction space, hydrate begins to generate; Be separated by the set time by suprasil window observation hydrate generation situation; Observe the internal-response thing and no longer change when seeing through quartz window, and air supply pipe 4 flowmeter that connects is when also no longer changing, can think that hydrate generates to finish.Close the air-supplying valve of air supply pipe 4 this moment, and disconnect air supply pipe 4 and the feed pipe 5 that reactor connects, cut-out is connected with circulating coolant pipeline, pressure responsive element and temperature sensitive member, place refrigerator to preserve (also can not put in the present embodiment, the refrigerator preservation and directly measure) reactor 100.
During measurement, from refrigerator, take out reactor 100, connect pressure responsive element, temperature sensitive member and circulating coolant pipeline, after circulating coolant is started working, reactor 100 is put into the Terahertz light path, thz beam needs axially to pass through suprasil window (that is: thz beam is axially by a side quartz window, the hydrate sample of generation, opposite side quartz window), arrives detector at last.Whole process need be observed temperature and pressure, and temperature must not be higher than 2 degrees centigrade, and pressure must not be higher than reactor design pressure.
From the above mentioned, the present invention is applicable to the hydrate reaction still that tera-hertz spectra is directly measured, its compound production and measuring in one of catchmenting, after generating in reactor, can directly in the Terahertz light path, measure in hydrate, saved the step of taking-up, compressing tablet in low temperature chamber, save time and cost, and avoided the disturbed possibility of hydrate sample.The hydrate sample that generates in reactor is the smooth parallel laminar solid in two sides, is fit to utilize the Terahertz instrument to measure.The quartz window of both sides absorbs tera-hertz spectra is low, can directly measure in the Terahertz light path.
Further, in the present embodiment, described cooling housing 1 is made by stainless steel material; The axially interior outer face of described first quartz window 21 and second quartz window 22 is parallel mutually; Fix sheathed certain position spacer ring 31 in the inner-walls of duct between described first quartz window and second quartz window, this location spacer ring 31 can adopt prior art such as screw to be fixed on the inwall of pipeline 12; Described first quartz window 21 is resisted against the both sides of locating spacer ring 31 respectively with second quartz window, 22 relative inner faces; The thickness of described location spacer ring 31 is 0.2～5mm; The outer face of described first quartz window 21 and second quartz window 22 is respectively by first fixed part 71 and second fixed part, 72 location and fixing that are connected on the inner-walls of duct.
As Fig. 1, shown in Figure 3, in the present embodiment, described first fixed part 71 and second fixed part 72 are loop configuration, are fixed on pipeline 12 inwalls by screw respectively.Can certainly adopt other existing fixed form that two fixed parts are fixed on the pipeline.
As shown in Figure 4, in the present embodiment, inwall that can also pipeline 12 is set to step structure; The inwall of described location spacer ring and pipeline 12 is structure as a whole, internal diameter is set greater than the end difference 121 of location spacer ring internal diameter on the spacer ring pipelines on two sides inwall of described location, described two quartz windows 21,22 are fixedlyed connected with end difference 121 inner wall sealings, and two relative inner faces of quartz window are resisted against the both sides of location spacer ring respectively; Described two fixed parts 71,72 are fixedly connected on respectively on end difference 121 outer faces, and with two quartz window location and fixing.
Further, in the present embodiment, the xsect of described pipeline 12 can be circle, also can be rectangle or polygon.
In the present embodiment, as Fig. 1, Fig. 3, shown in Figure 4, be positioned at and be respectively equipped with an insulation thin slice 131,132 on the cooling housing sidewall of pipe ends; Described insulation thin slice is made by tygon or quartz material; Described insulation thin slice both sides smooth smooth and with the cooling housing sidewall closely contact; Form an airtight incubation cavity 141,142 respectively in the pipeline of each insulation thin slice inboard, be filled with nitrogen or inert gas in the described airtight incubation cavity.
In the present embodiment, described pressure responsive element is pressure transducer, and described temperature sensitive member is temperature sensor; As shown in Figure 1 and Figure 2, described temperature sensor is connected in control and the display device (not shown) of cooling off outside the housing 1 by a lead 61; Described pressure transducer is connected in control and the display device (not shown) of cooling off outside the housing 1 by a pressure monitoring pipe 62.
The present invention is applicable to the catchment compound production and measuring in one of hydrate reaction still that tera-hertz spectra is directly measured, and reaction compartment is designed to the thin rounded flakes shape, makes the hydrate form of generation be particularly suitable for the detection of Terahertz system; Reactor provides firm transparent quartz window, and the convenient hydrate that detects generates state, also is fit to thz beam and passes through; This reactor can the conserve water compound detection time, omit the foundation of large-scale low-temperature chamber, save the scientific research fund; This reactor reduces the temperature in hydrate reaction space by circulating coolant, helps to reduce the pressure conditions that hydrate generates, and has reduced the reactor cost of manufacture; This reactor overall volume is little, is easy to carry and shifts, and also can put into refrigerator easily and preserve.
The above only is the schematic embodiment of the present invention, is not in order to limit scope of the present invention.Any those skilled in the art, the equivalent variations of having done under the prerequisite that does not break away from design of the present invention and principle and modification all should belong to the scope of protection of the invention.
Claims (10)
1. one kind is applicable to the directly hydrate reaction still of measurement of tera-hertz spectra, it is characterized in that: described reactor comprises a cooling housing, and described cooling housing is made of the pipeline of shell and a perforation of horizontally set in this shell; Form the seal chamber that holds heat eliminating medium between the outer wall of described pipeline and the described shell; In described pipeline, axially be fixed with first quartz window and second quartz window that arrange at interval, the shape of cross section of the shape of cross section of described two quartz windows and size and described pipeline and measure-alike, and quartz window and inner-walls of duct are sealedly and fixedly connected; Form the hydrate span between described first quartz window and second quartz window; Described hydrate span sealing is communicated in air supply pipe and feed pipe; Described reactor also includes pressure responsive element and the temperature sensitive member of monitoring hydrate span internal pressure and temperature.
2. the hydrate reaction still that is applicable to that tera-hertz spectra is directly measured as claimed in claim 1 is characterized in that: fix sheathed certain position spacer ring in the inner-walls of duct between described first quartz window and second quartz window; The inner face that described first quartz window is relative with second quartz window is resisted against the both sides of location spacer ring respectively; The thickness of described location spacer ring is 0.2～5mm.
3. the hydrate reaction still that is applicable to that tera-hertz spectra is directly measured as claimed in claim 2, it is characterized in that: the outer face of described first quartz window and second quartz window is respectively by first fixed part and second fixed part location and fixing that are connected on the inner-walls of duct.
4. the hydrate reaction still that is applicable to that tera-hertz spectra is directly measured as claimed in claim 3 is characterized in that: described first quartz window and second quartz window axially in the outer face parallel mutually.
5. the hydrate reaction still that is applicable to that tera-hertz spectra is directly measured as claimed in claim 3, it is characterized in that: described first fixed part and second fixed part are loop configuration.
6. the hydrate reaction still that is applicable to that tera-hertz spectra is directly measured as claimed in claim 1 is characterized in that: the xsect of described pipeline is circular, rectangle or polygon.
7. the hydrate reaction still that is applicable to that tera-hertz spectra is directly measured as claimed in claim 1, it is characterized in that: described cooling housing is made by stainless steel material.
8. the hydrate reaction still that is applicable to that tera-hertz spectra is directly measured as claimed in claim 1, it is characterized in that: described heat eliminating medium is circulating coolant, described seal chamber top is provided with the circulating coolant inlet, and described seal chamber bottom is provided with the circulating coolant flow export.
9. the hydrate reaction still that is applicable to that tera-hertz spectra is directly measured as claimed in claim 1, it is characterized in that: described air supply pipe is connected with air-supplying valve, tensimeter, reduction valve, flowmeter and gas cylinder; Described feed pipe is connected with water supply valve; Described pressure responsive element and temperature sensitive member are connected with control and display device.
10. the hydrate reaction still that is applicable to that tera-hertz spectra is directly measured as claimed in claim 1 is characterized in that: be positioned on the cooling housing sidewall of pipe ends and be respectively equipped with an insulation thin slice; Described insulation thin slice is made by tygon or quartz material; Described insulation thin slice both sides smooth smooth and with the cooling housing sidewall closely contact; Form an airtight incubation cavity respectively in the pipeline of each insulation thin slice inboard, be filled with nitrogen or inert gas in the described airtight incubation cavity.
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| CN201310163948.4A CN103245540B (en) | 2013-05-07 | 2013-05-07 | Hydrate reaction kettle suitable for direct measurement in terahertz spectrum |
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| CN201310163948.4A CN103245540B (en) | 2013-05-07 | 2013-05-07 | Hydrate reaction kettle suitable for direct measurement in terahertz spectrum |
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| CN103245540B CN103245540B (en) | 2015-05-20 |
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Citations (7)
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| US20050056785A1 (en) * | 2003-09-16 | 2005-03-17 | Northrop Grumman Corporation | Detection and analysis of chemical and biological materials by passive emission of terahertz wave against a cold background target |
| US20070267575A1 (en) * | 2006-05-17 | 2007-11-22 | Sandor Holly | Cryogenic terahertz spectroscopy |
| US20090194744A1 (en) * | 2007-08-14 | 2009-08-06 | Adebimpe David O B A | Methods for making scent simulants of chemical explosives, and compositions thereof |
| CN102706831A (en) * | 2012-05-30 | 2012-10-03 | 中国矿业大学 | Frequency-domain Tera Hertz device and method for monitoring CO concentration in coal spontaneous combustion gas |
| CN202794013U (en) * | 2012-05-23 | 2013-03-13 | 中国科学院上海应用物理研究所 | Liquid sample pool |
| CN202794017U (en) * | 2012-08-21 | 2013-03-13 | 中国科学院上海应用物理研究所 | Liquid sample cell |
| CN203244962U (en) * | 2013-05-07 | 2013-10-23 | 中国石油大学(北京) | Hydrate reactor suitable for direct measurement of terahertz spectrum |
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2013
- 2013-05-07 CN CN201310163948.4A patent/CN103245540B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050056785A1 (en) * | 2003-09-16 | 2005-03-17 | Northrop Grumman Corporation | Detection and analysis of chemical and biological materials by passive emission of terahertz wave against a cold background target |
| US20070267575A1 (en) * | 2006-05-17 | 2007-11-22 | Sandor Holly | Cryogenic terahertz spectroscopy |
| US20090194744A1 (en) * | 2007-08-14 | 2009-08-06 | Adebimpe David O B A | Methods for making scent simulants of chemical explosives, and compositions thereof |
| CN202794013U (en) * | 2012-05-23 | 2013-03-13 | 中国科学院上海应用物理研究所 | Liquid sample pool |
| CN102706831A (en) * | 2012-05-30 | 2012-10-03 | 中国矿业大学 | Frequency-domain Tera Hertz device and method for monitoring CO concentration in coal spontaneous combustion gas |
| CN202794017U (en) * | 2012-08-21 | 2013-03-13 | 中国科学院上海应用物理研究所 | Liquid sample cell |
| CN203244962U (en) * | 2013-05-07 | 2013-10-23 | 中国石油大学(北京) | Hydrate reactor suitable for direct measurement of terahertz spectrum |
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