CN203929646U - For the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring - Google Patents
For the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring Download PDFInfo
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- CN203929646U CN203929646U CN201420287933.9U CN201420287933U CN203929646U CN 203929646 U CN203929646 U CN 203929646U CN 201420287933 U CN201420287933 U CN 201420287933U CN 203929646 U CN203929646 U CN 203929646U
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- quartz capillary
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- hydrate
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Abstract
High-pressure mini reaction unit for the monitoring of gas hydrate situ Raman Spectroscopy comprises hydrate reaction container, gas cylinder, temperature control modules, vacuumize module, syringe and pressure control module, hydrate reaction container is quartz capillary, temperature control modules comprises cold and hot and cold and hot controller, quartz capillary is fixed on cold and hot inside, cold and hot is provided with the window that is suitable for micro-Raman camera lens monitoring quartz capillary, vacuumize module and comprise vacuum pump and vacuum meter, vacuum pump, gas cylinder is all connected with quartz capillary, vacuum meter is communicated with on the pipeline of vacuum pump and quartz capillary, syringe is communicated with quartz capillary, pressure control module comprises forcing pump and pressure transducer, the two is communicated with on the pipeline between gas cylinder and quartz capillary.The utility model temperature controlling range is-198 DEG C～500 DEG C, and top pressure can reach 40MPa, can stablize and control temperature, pressure, detects in real time the each component in gas hydrate generative process.
Description
Technical field
The utility model relates to a kind of high-pressure mini reaction unit for the monitoring of gas hydrate situ Raman Spectroscopy.
Background technology
Gas hydrate is the cage compound being generated under cryogenic high pressure by gas molecule and hydrone, and its thermodynamics and kinetics research is two important aspects of hydrate research field.Although the research of the thermodynamics and kinetics of gas-water-hydrate three-phase system is quite deep, the achievement in research of three-phase system has also solved problem relevant to hydrate zone in a lot of geology, but people are still not fully aware of to some micromechanisms of sea bottom hydrate formation of ore deposits and extinction.Current most scholar thinks by dissolved methane in original place or migrates to changes the most general mechanism that hydrate is ocean water compound formation of ore deposits in stable region, therefore, people are expecting the transformation microprocess of dissolved methane and hydrate in direct observation water-hydrate two-phase system always, carry out very important of direct experimental observation therefore hydrate in two-phase system is generated-dissolve this reversible dynamic process.
In laboratory, utilize the generative process of hydrate in advanced experimental provision simulating ocean environment, carry out the real-time detection of fluid intermediate ion parameter and hydrate growth-dispersion process, disclose the important parameters such as crystal structure, hole occupation rate, hydration index in multicomponent gas hydrate to understand in depth hydrate in actual natural surroundings formation, developing has great importance.
At present, while adopting laser Raman spectroscopy mensurated gas composition hydrate both at home and abroad, cold and hot is the most frequently used accessory, and temperature range is-196 DEG C～400 DEG C, and temperature-controlled precision is very high, and gas hydrate sample can be measured at low temperatures.But, due to it can not controlled pressure (only under normal pressure), therefore can only measure a kind of state of hydrate, can not carry out the in-situ monitoring of hydrate generation, decomposable process.
Publication number is the Chinese patent micro Raman spectra high-pressure temperature control experiment device of CN201749085, a kind of experimental provision that comprises air supply system, pressure transducer, temperature sensor, reactor, data acquisition unit, control module is disclosed, but this experimental provision temperature-controlling system adopts semiconductor refrigerating, temperature range-10 DEG C～30 DEG C, pressure is up to 10MPa, is difficult to the pressure condition of simulated sea bottom hydrate stable existence.
Utility model content
The technical problems to be solved in the utility model is to provide a kind of high-pressure mini reaction unit for the monitoring of gas hydrate situ Raman Spectroscopy, its temperature controlling range is-198 DEG C～500 DEG C, top pressure can reach 40MPa, can stablize and control temperature, pressure, detect in real time the each component in gas hydrate generative process.
The utility model is for the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring, comprise hydrate reaction container, gas cylinder, temperature control modules, vacuumize module, also comprise syringe and pressure control module, described hydrate reaction container is quartz capillary, described temperature control modules comprises cold and hot and cold and hot controller, described quartz capillary is fixed on cold and hot inside, cold and hot offers the window that is suitable for micro-Raman camera lens monitoring quartz capillary, the described module that vacuumizes comprises vacuum pump and vacuum meter, described vacuum pump, gas cylinder is all connected with quartz capillary, described vacuum meter is communicated with on the pipeline of vacuum pump and quartz capillary, described syringe is communicated with quartz capillary, described pressure control module comprises forcing pump and pressure transducer, described forcing pump and pressure transducer are communicated with on the pipeline between gas cylinder and quartz capillary.
The utility model is that for the high-pressure mini reaction unit difference from prior art of gas hydrate situ Raman Spectroscopy monitoring it is device supercharging that the utility model is set up pressure control module for the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring, cold and hot is carried out high precision to hydrate reaction container, temperature control on a large scale, ensure experimental temperature, stablizing of pressure, hydrate reaction container adopts quartz capillary, can bear high pressure, transparent quartz capillary is directly welded on stainless steel pipeline, due to the whole clearing of quartz capillary, Raman spectrum can detect the each component in gas hydrate generative process in real time, can mensurated gas composition at the rate of propagation of solution and the formation speed of hydrate.
Further, for ensureing the effectively succinct of line system, the utility model arranges described vacuum pump for the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring, gas cylinder is connected with quartz capillary through the first Triple Valve with High Pressure, described vacuum meter is communicated with on the pipeline between vacuum pump and the first Triple Valve with High Pressure by the first high pressure four-way valve, described syringe is communicated with on the pipeline between the first Triple Valve with High Pressure and the first high pressure four-way valve by the second Triple Valve with High Pressure, described forcing pump and pressure transducer are communicated with on the pipeline between gas cylinder and the first Triple Valve with High Pressure by the second high pressure four-way valve.
Further, the utility model, for the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring, also comprises computer acquisition system.
Connect micro-Raman camera lens by computer acquisition system, not only can carry out Real-Time Monitoring to the sample in quartz capillary, can also sample variation in quartz capillary be taken pictures, be recorded a video.
Further, enter cold and hot and fixing in cold and hot for convenience of quartz capillary, the utility model is provided with and is suitable for the port that quartz capillary passes for cold and hot of the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring, cold and hot inside is provided with fixing quartzy metal platform capillaceous, and described metal platform is provided with and is suitable for the groove that quartz capillary holds.
Further, the utility model, for the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring, also comprises three-dimensional fine-tuning frame, and described three-dimensional fine-tuning frame is suitable for placing quartz capillary.
Quartz capillary when inserting in cold and hot, is first placed on three-dimensional fine-tuning frame, regulates three-dimensional fine-tuning frame, until the quartz capillary on it aligns mutually with cold and hot you mouth, quartz capillary can accurately be inserted in cold and hot smoothly.
Below in conjunction with accompanying drawing, the high-pressure mini reaction unit for the monitoring of gas hydrate situ Raman Spectroscopy of the present utility model is described further.
Brief description of the drawings
Fig. 1 is the ingredient schematic diagram of the utility model for the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring.
Embodiment
As shown in Figure 1, the utility model comprises hydrate reaction container 1, gas cylinder 2, temperature control modules, vacuumizes module, syringe 3 and pressure control module for the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring.
Hydrate reaction container 1 is quartz capillary, temperature control modules comprises cold and hot 4 and cold and hot controller 5, be provided with for cold and hot 4 and be suitable for the port that quartz capillary passes, cold and hot 4 inside are provided with fixing quartzy metal platform capillaceous, metal platform is provided with and is suitable for the groove that quartz capillary holds, and cold and hot 4 also offers the window that is suitable for micro-Raman camera lens monitoring quartz capillary.
Vacuumize module and comprise vacuum pump 6 and vacuum meter 7, vacuum pump 6, gas cylinder 2 are connected with quartz capillary through the first Triple Valve with High Pressure 8, vacuum meter 7 is communicated with on the pipeline between vacuum pump 6 and the first Triple Valve with High Pressure 8 by the first high pressure four-way valve 9, and syringe 3 is communicated with on the pipeline between the first Triple Valve with High Pressure 8 and the first high pressure four-way valve 9 by the second Triple Valve with High Pressure 10.
Pressure control module comprises forcing pump 11 and pressure transducer 12, and forcing pump 11 and pressure transducer 12 are communicated with on the pipeline between gas cylinder 2 and the first Triple Valve with High Pressure 8 by the second high pressure four-way valve 13.
The utility model, for the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring, also comprises computer acquisition system 14, for connecting sample variation in micro-Raman camera lens monitoring record quartz capillary.
In use, concrete operation step is as follows for the high-pressure mini reaction unit that the utility model is monitored for gas hydrate situ Raman Spectroscopy:
1, prepare quartz capillary
Burn the diaphragm of quartz capillary outside with spirit lamp; by quartz capillary one end oxyhydrogen flame sealing; the other end of quartz capillary is clung with the stainless steel pipeline that is communicated with the first Triple Valve with High Pressure 8 with epoxy resin; place after 36h; be placed on three-dimensional fine-tuning frame 15, regulated three-dimensional fine-tuning frame, until the quartz capillary on it aligns mutually with the port of cold and hot 4; quartz capillary is inserted to cold and hot inside through port, be placed in metal platform groove fixing.
2, vacuumize
Referring to Fig. 1, close the V5 switch of the first Triple Valve with High Pressure 8, make quartz capillary and gas cylinder 2, the connection of forcing pump 11 disconnects, close the V2 switch of the second Triple Valve with High Pressure 10, make the disconnection that is communicated with of syringe and quartz capillary, close the V1 switch of the first high pressure four-way valve 9, make itself and the disconnection that is communicated with of extraneous air, open the V3 of the second Triple Valve with High Pressure 10 and the V4 switch of the first Triple Valve with High Pressure 8, make vacuum pump 6, vacuum meter 7, pipeline between quartz capillary keeps connected state, opening vacuum pump 6 vacuumizes, until vacuum meter 7 shows vacuum state.
3, filling liquid
Close the V3 switch of the second Triple Valve with High Pressure 10, the pipeline that makes the second Triple Valve with High Pressure 10 be communicated with vacuum pump 6 directions is closed, and opens the V2 switch of the second Triple Valve with High Pressure 10, starts syringe 3, to filling liquid in quartz capillary.
4, injecting gas
Close the V2 switch of the second Triple Valve with High Pressure 10, disconnect being communicated with of syringe 3 and quartz capillary, the V5 switch of unlatching the first Triple Valve with High Pressure 8, makes the unlatching that is communicated with of quartz capillary and gas cylinder 2, forcing pump 11, open the V6 switch of gas cylinder 2, to injecting gas in quartz capillary.
5, pressurization
Opening pressure pump 11, the utility model adopts Manual pressurization pump, to gas boosting in pipeline between gas cylinder 2 and quartz capillary and in quartz capillary, shows the required force value of experiment until be raised to pressure transducer 12.
6, temperature control
Open cold and hot controller 5, the quartz capillary in cold and hot 4 is carried out to temperature control, until test temperature required.
7, test
Adopt laser Raman spectrometry to carry out spectral detection to sample in quartz capillary, and by computer system record, obtain Raman spectrum behavioral characteristics in different gas sample hydrate growth-dissolution mechanism.
8, after experiment finishes, gas in the whole device of emptying, makes whole device pressure return to normal pressure, according to the data of obtaining, analyzes the Changing Pattern of the key indexs such as hole occupation rate, hydration index, each concentration of component in hydrate growth course.
Above-described embodiment is described preferred implementation of the present utility model; not scope of the present utility model is limited; do not departing under the prerequisite of the utility model design spirit; various distortion and improvement that those of ordinary skill in the art make the technical solution of the utility model, all should fall in the definite protection domain of the utility model claims.
Claims (5)
1. the high-pressure mini reaction unit for the monitoring of gas hydrate situ Raman Spectroscopy, comprise hydrate reaction container (1), gas cylinder (2), temperature control modules, vacuumize module, it is characterized in that: also comprise syringe (3) and pressure control module, described hydrate reaction container (1) is quartz capillary, described temperature control modules comprises cold and hot (4) and cold and hot controller (5), described quartz capillary is fixed on cold and hot (4) inside, cold and hot (4) offer the window that is suitable for micro-Raman camera lens monitoring quartz capillary, the described module that vacuumizes comprises vacuum pump (6) and vacuum meter (7), described vacuum pump (6), gas cylinder (2) is all connected with quartz capillary, described vacuum meter (7) is communicated with on the pipeline of vacuum pump (6) and quartz capillary, described syringe (3) is communicated with quartz capillary, described pressure control module comprises forcing pump (11) and pressure transducer (12), described forcing pump (11) and pressure transducer (12) are communicated with on the pipeline between gas cylinder (2) and quartz capillary.
2. the high-pressure mini reaction unit for the monitoring of gas hydrate situ Raman Spectroscopy according to claim 1, it is characterized in that: described vacuum pump (6), gas cylinder (2) is connected with quartz capillary through the first Triple Valve with High Pressure (8), described vacuum meter (7) is communicated with on the pipeline between vacuum pump (6) and the first Triple Valve with High Pressure (8) by the first high pressure four-way valve (9), described syringe (3) is communicated with on the pipeline between the first Triple Valve with High Pressure (8) and the first high pressure four-way valve (9) by the second Triple Valve with High Pressure (10), described forcing pump (11) and pressure transducer (12) are communicated with on the pipeline between gas cylinder (2) and the first Triple Valve with High Pressure (8) by the second high pressure four-way valve (13).
3. the high-pressure mini reaction unit for the monitoring of gas hydrate situ Raman Spectroscopy according to claim 1 and 2, it is characterized in that: also comprise computer acquisition system (14), for connecting sample variation in micro-Raman camera lens monitoring record quartz capillary.
4. the high-pressure mini reaction unit for the monitoring of gas hydrate situ Raman Spectroscopy according to claim 3, it is characterized in that: described cold and hot (4) are provided with and are suitable for the port that quartz capillary passes, cold and hot (4) inside is provided with fixing quartzy metal platform capillaceous, and described metal platform is provided with and is suitable for the groove that quartz capillary holds.
5. the high-pressure mini reaction unit for the monitoring of gas hydrate situ Raman Spectroscopy according to claim 4, is characterized in that: also comprise three-dimensional fine-tuning frame (15), described three-dimensional fine-tuning frame (15) is suitable for placing quartz capillary.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420287933.9U CN203929646U (en) | 2014-05-30 | 2014-05-30 | For the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring |
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| CN201420287933.9U CN203929646U (en) | 2014-05-30 | 2014-05-30 | For the high-pressure mini reaction unit of gas hydrate situ Raman Spectroscopy monitoring |
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| CN105466907A (en) * | 2015-12-30 | 2016-04-06 | 浙江工业大学 | Method and special device for in-situ online determination of expansion coefficient of CO2-alkane system |
| CN105548137A (en) * | 2015-12-25 | 2016-05-04 | 中国科学院广州能源研究所 | High-pressure cooling-heating table device for in-situ observation of aquo-complex microscopic reaction kinetics process and application method |
| CN107290328A (en) * | 2016-04-13 | 2017-10-24 | 吉林化工学院 | Raman vibrational spectrum temperature control sample testing stand |
| CN107290327A (en) * | 2016-04-13 | 2017-10-24 | 吉林化工学院 | Raman vibrational spectrum low-temperature sample detection frame |
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| CN110441286A (en) * | 2019-08-31 | 2019-11-12 | 大连理工大学 | Gas hydrate pressure maintaining displacement apparatus and method for in-situ Raman analysis |
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| CN105548137A (en) * | 2015-12-25 | 2016-05-04 | 中国科学院广州能源研究所 | High-pressure cooling-heating table device for in-situ observation of aquo-complex microscopic reaction kinetics process and application method |
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| CN107290327A (en) * | 2016-04-13 | 2017-10-24 | 吉林化工学院 | Raman vibrational spectrum low-temperature sample detection frame |
| CN108267401A (en) * | 2017-12-29 | 2018-07-10 | 中国石油天然气股份有限公司 | Capillary fluid observation system |
| CN108267401B (en) * | 2017-12-29 | 2020-12-01 | 中国石油天然气股份有限公司 | Capillary fluid observation system |
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| CN109470684A (en) * | 2018-11-30 | 2019-03-15 | 江苏大学 | A kind of device and method of quartz ampoule combination Raman spectrometer monitoring hydrothermal liquefaction process |
| CN110487771A (en) * | 2019-08-31 | 2019-11-22 | 大连理工大学 | Gas hydrate generation/decomposing system and method for in-situ Raman analysis |
| CN110530844A (en) * | 2019-08-31 | 2019-12-03 | 大连理工大学 | The quantitative gas-liquid multiphase hydrate generation/decomposer of in-situ Raman and method |
| CN110530844B (en) * | 2019-08-31 | 2020-10-20 | 大连理工大学 | In-situ Raman quantitative gas-liquid multiphase hydrate generation/decomposition device and method |
| CN110441286B (en) * | 2019-08-31 | 2020-10-20 | 大连理工大学 | Gas hydrate pressure maintaining and replacing device and method for in-situ Raman analysis |
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Granted publication date: 20141105 Termination date: 20150530 |
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