CN102156009B - Device for measuring thermal power - Google Patents
Device for measuring thermal power Download PDFInfo
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- CN102156009B CN102156009B CN2011100800732A CN201110080073A CN102156009B CN 102156009 B CN102156009 B CN 102156009B CN 2011100800732 A CN2011100800732 A CN 2011100800732A CN 201110080073 A CN201110080073 A CN 201110080073A CN 102156009 B CN102156009 B CN 102156009B
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Abstract
The invention provides a device for measuring thermal power. The device comprises a thermostat, a thermal measuring device, a thermal calibration device and a data acquisition and control device, wherein the thermostat comprises a temperature controller and a thermostat furnace body connected with the temperature controller; a thermal metering cylinder is arranged in the thermostat furnace body and comprises a reaction tank cavity body and a constant-temperature screen which is sleeved outside the reaction tank cavity body, and an annular cavity is arranged between the reaction tank cavity body and the constant-temperature screen; two end parts of the annular cavity are respectively provided with a soaking block; each soaking block is internally provided with a groove; the thermal measuring device comprises a temperature measuring electric bridge, the temperature measuring electric bridge comprises two temperature measuring resistance wires wound on the reaction tank cavity body corresponding to the annular cavity, two temperature measuring resistance wires wound on the inner walls of the grooves, a bridge current regulation resistor and a direct current signal source; the thermal calibration device comprises a calibration resistance wire which is wound on the reaction tank cavity corresponding to the annular cavity and a direct current power supply which is connected with the calibration resistance wire; the temperature controller is connected with the data acquisition and control device; and the temperature measuring electric bridge and the direct current power supply are both connected with the control device.
Description
Technical field
The present invention relates to a kind of thermal power measurement device, be applicable to that the thermal power in the physical and chemical process is measured.
Background technology
Existing business-like isothermal (or the accurate isothermal) thermal power measurement device that is used for physical chemical process heat release (or thermal absorption) can't directly be applied to the high temperature and high pressure condition simultaneously under room temperature or the atmospheric pressure.Maximum operating temperature like the Alexsys-1000 type isothermal calorimeter of Sai Talamu (SETARAM) company is 1000 ℃, and the thermal power that realize high-pressure process is measured and also needed special high pressure resistant reaction tank.Can be applied to isothermal or half isothermal thermal power measurement device under the high temperature and high pressure condition and be mainly used in the reaction heat measured between two kinds of fluids (like X.Chen et al, Thermochim.Acta, 1996; That designs in 285,11 literary compositions can be applicable to 450 ℃, the flow-type calorimeter under the 5MPa condition) or be used to measure heat of evaporation (the Parisod et al of single component; Rev.Sci.Instrum., 1982,53; That designs in 54 literary compositions can be applicable to 500 ℃, the calorimeter under the 83MPa condition).Mostly other high temperature and or condition of high voltage the thermal measurement device of work down are that adiabatic or near heat-insulating is (as quickening calorimeter; Ginseng www.thermalhazardtechnology.com), the constant temperature jacket-type is (like E.Djamali et al; Rev.Sci.Instrum.2010; And non-isothermal or accurate isothermal thermal power measurement device the calorimeter that designs in 81,075105 literary compositions).
In addition, for the solid-solid/liquid/gas reactions process under the high-temperature and high-pressure conditions, existing thermal measurement means can provide some thermodynamics informations, but for kinetic parameters such as the order of reaction, reaction rate constant, energy of activation, need isothermal or quasi isothermal thermal power measurement device.
Summary of the invention
The purpose of this invention is to provide a kind of quasi isothermal, high-temperature and high-pressure conditions heat release or endothermic process thermal power measurement device in solid-solid/liquid/gas reactions down.
Thermal power measurement device provided by the invention comprises thermostat, thermal measurement device, hot caliberating device and data acquisition and control device; Said thermostat comprises temperature controller and the thermostat body of heater that is attached thereto; Be provided with the calorimetric tube in the said thermostat body of heater; Said calorimetric tube comprises the constant temperature screen that the reaction tank cavity is outer with being set in said reaction tank cavity, is provided with ring cavity between said reaction tank cavity and the said constant temperature screen; Two ends of said ring cavity are respectively equipped with the soaking piece; Be equipped with groove in each said soaking piece; Said thermal measurement device comprises bridge for measuring temperature, and said bridge for measuring temperature comprises that two temperature detecting resistance silks on the said reaction tank cavity that is wrapped in said ring cavity counterpart, two temperature detecting resistance silks, the bridge that is wrapped on the said groove inwall flow adjusting resistance and dc signal source; Said hot caliberating device comprises that on the said reaction tank cavity that is wrapped in said ring cavity counterpart demarcates resistance wire and the direct supply that is attached thereto; Said temperature controller links to each other with control device with said data acquisition; Said bridge for measuring temperature links to each other with control device with said data acquisition; Said direct supply links to each other with control device with said data acquisition.
In the above-mentioned measurement mechanism, said thermostat can be the tubular type thermostat, and said tubular type thermostat provides the constant high temperature environment that needs.
In the above-mentioned measurement mechanism, the outer wall of the said reaction tank cavity of said ring cavity counterpart is provided with insulation course; The inwall of said groove is provided with insulation course.
In the above-mentioned measurement mechanism, said temperature detecting resistance silk and said demarcation resistance wire all can be resistive platinum wire; Produce (or absorption) hot-fluid in the said reaction tank cavity and cause that the temperature of said reaction tank cavity raises (or reduction), and and then make around the resistance value of thermometric resistive platinum wire increase (or reduction), cause said bridge for measuring temperature out of trim output electric signal.
In the above-mentioned measurement mechanism, said direct supply can be programme-controlled dc power, and the permanent power electric current that provides through said programme-controlled dc power makes said resistive platinum wire generation Joule heat come thermal power measurement device provided by the present invention is demarcated.
In the above-mentioned measurement mechanism, said temperature detecting resistance silk uniform winding is on said reaction tank cavity and said groove inwall, thereby the thermal power of accurately measuring in the said reaction tank cavity changes; Said demarcation resistance wire uniform winding is demarcated thereby said measurement mechanism is carried out thermal power on said reaction tank cavity.
In the above-mentioned measurement mechanism, said data acquisition and control device comprise data collecting card and computing machine that is attached thereto and corresponding software; Said temperature controller links to each other with said computing machine; Said bridge for measuring temperature links to each other with said data collecting card; Said direct supply links to each other with said computing machine; The temperature and the demarcation thermal power of demarcating thermal resistance of said thermostat measured and controlled to said data acquisition and control device, measures the output signal of said bridge for measuring temperature, and record and the processing data of surveying.
In the above-mentioned measurement mechanism, the material of the material of said reaction tank cavity and said soaking piece all can be high temperature high voltage resistant, corrosion resistant metal or alloy, like stainless steel, Hastelloy or titanium alloy etc.; But loading solid reactant in the said reaction tank cavity, the both ends open of said reaction tank cavity can be reacting fluid inlet and fluid product outlet respectively.
In the above-mentioned measurement mechanism, can be provided with pressure transducer and/or flowmeter on the said reaction tank cavity, can measure pressure in the physical and chemical process and/physical quantitys such as flow; Said reaction tank cavity can link to each other with chromatograph, mass spectrometer or spectrometer, thereby can be used for the research of reaction mechanism.
The present invention has the following advantages owing to take above technical scheme: 1, in the measurement mechanism provided by the invention the reaction tank cavity can under high-temperature and high-pressure conditions, work, can be used for the monitoring and the mechanism research of physical and chemical process under the high-temperature and high-pressure conditions; 2, the reaction tank cavity in the measurement mechanism provided by the invention is reserved with stream socket, can be used for flow-type (also can be used for enclosure-type certainly) solid-fluid reaction; 3, the present invention adopts the temperature variant characteristic of resistive platinum wire to measure in thermal power, and four incorporating resistors of said bridge for measuring temperature are in hot environment, and the thermal perturbation of the environment of having cancelled out each other is to the interference of output signal; 4, the resistive platinum wire of thermometric described in the present invention guarantees hot-fluid as much as possible is converted into electric signal around being uniformly distributed in said reaction tank cavity; This design is equal on the thermal diffusion equipotential surface carries out the area branch to hot-fluid, has reduced the dependence of thermal power signal to reaction zone position in the reaction tank cavity; 5, the built-in demarcation thermal resistance of thermal power measurement device of the present invention and realize the power supply of permanent power through programme-controlled dc power has improved the degree of accuracy of hot demarcation, has simplified hot calibration process.The present invention can be used for measuring solid-fluid reaction under high temperature, the condition of high voltage; Like the thermokinetics research of physical and chemical processes such as combustion (of oil) in site, synthetic fatty acid chemical industry, high-temperature oxydation or catalytic reaction in the oil exploitation, combining to be further used for study on mechanism with composition detection means (like chromatogram, mass spectrum, spectrum etc.).
Description of drawings
Fig. 1 is the structural representation of the thermal power measurement device of the embodiment of the invention 1.
Fig. 2 is the cross-sectional schematic of the calorimetric tube in the thermal power measurement device of the embodiment of the invention 1.
Fig. 3 is the thermal power calibration result under the different temperatures in the embodiment of the invention 2.
Fig. 4 be in the embodiment of the invention 2 under the different temperatures thermal power of dotriacontane oxidizing process measure and fitting result.
Each mark is following among the figure: 1 temperature controller, 2 tubular type thermostat bodies of heater, 3 calorimetric tubes, 4 reaction tank cavitys, 5 constant temperature screen, 6 ring cavities, 7 soaking pieces, 8 grooves, 9 insulation courses, 10 bridge for measuring temperature, 11; 13 resistive platinum wire, 12,15 resistance leads, 14 programme-controlled dc powers, 16 data collecting cards, 17 computing machines.
Embodiment
Below in conjunction with accompanying drawing the present invention is explained further details, but the present invention is not limited to following examples.
Embodiment 1, thermal power measurement device
Thermal power measurement device provided by the invention comprises tubular type thermostat, thermal measurement device, hot caliberating device and data acquisition and control device; The tubular type thermostat comprises temperature controller 1 and the tubular type thermostat body of heater 2 that links to each other with this temperature controller 1; Be provided with calorimetric tube 3 in the tubular type thermostat body of heater 2, its material is a stainless steel; Calorimetric tube 3 comprises stainless reaction tank cavity 4 and the stainless steel constant temperature screen 5 that is set in outside this reaction tank cavity 4, is provided with ring cavity 6 between reaction tank cavity 4 and the constant temperature screen 5; Be equipped with stainless steel soaking piece 7 on two ends of ring cavity 6, constant temperature screen 5 is reaction tank cavity 4 with soaking piece 7 provides the even temperature environment; The reaction tank cavity 4 of ring cavity 6 counterparts can be high temperature reaction zone; Be equipped with groove 8 in each soaking piece 7; All scribble insulation course 9 on the reaction tank cavity 4 of ring cavity 6 counterparts (being the part of the high temperature reaction zone) outer wall and on the inwall of groove 8; The thermal measurement device comprises bridge for measuring temperature 10; Bridge for measuring temperature 10 comprises that resistive platinum wire 11, two piece uniform winding (through inorganic high-temp structure glue adhere to) resistive platinum wire 11, the bridge stream on the inwall of groove 8 of two uniform winding (adhering to through the inorganic high-temp structure glue) on the reaction tank cavity 4 of ring cavity 6 counterparts regulates resistance (not shown) and dc signal source (not shown); Four resistive platinum wire 11 are all drawn as lead-in wire through resistance lead 12 (for the Ni-Cr silk), are connected for spot welding between resistance lead 12 and the resistive platinum wire 11; Hot caliberating device comprises the resistive platinum wire 13 of a uniform winding (adhering to through the inorganic high-temp structure glue) on the reaction tank cavity 4 of ring cavity 6 counterparts and the programme-controlled dc power 14 that is attached thereto; Resistive platinum wire 13 and programme-controlled dc power 14 are connected through resistance lead 15 (for the Ni-Cr silk), are connected for spot welding between resistance lead 15 and the resistive platinum wire 13; Data acquisition and control device comprise data collecting card 16 and the computing machine 17 that is attached thereto; Computing machine 17 links to each other with temperature controller 1, and the temperature of tubular type thermostat body of heater 2 is measured and controlled; Bridge for measuring temperature 10 links to each other with data collecting card 16, exports electric signal to data collecting card 16 through signal wire; Programme-controlled dc power 14 links to each other with computing machine 17, realizes the conversion between electric signal and the thermal power; The fluid intake end of reaction tank cavity 4 is connected with pressure transducer (not shown) and flowmeter (not shown), can detect pressure in the course of reaction and flow; The fluid outlet of reaction tank cavity 4 is connected with the gas chromatograph (not shown); These instruments all link to each other with control device with data acquisition, but reach with the variation of (pressure, time) of each controlled variable through computing machine 17 on-line measurement product time of occurrences and content.
The reaction tank cavity 4 of above-mentioned thermal power measurement device can be more than the withstand voltage 8MPa in the time of 600 ℃, and reaction tank cavity 4 adopts metal card shell type joint to be connected with gas circuit.780 ℃ of insulation course 9 ability heatproofs.The long-term service condition of this thermal power measurement device is: room temperature to 600 ℃, normal pressure are to 6MPa; The short-term serviceability temperature can reach 700 ℃, pressure and reach 8MPa.The LDL of this thermal power measurement device reaches 1mW.
In the above-mentioned thermal power measurement device, the material of calorimetric tube 3 and soaking piece 7 can be other high temperature high voltage resistant, corrosion resistant metal or alloy, like Hastelloy or titanium alloy etc.; The size of reaction tank cavity 4 can be regulated as required; Thermostat also can be other configuration beyond the tubular type, as box, vertical etc.
The application of the thermal power measurement device of embodiment 2, embodiment 1
Be measured as the use of example explanation thermal power measurement device provided by the invention below with the thermal power of dotriacontane oxidizing process:
Through different thermal powers test bridge for measuring temperature 10 output voltages of demarcating of input under different temperatures, set up the funtcional relationship between output voltage and thermal power, thus the thermal power numerical value in the corresponding reaction tank cavity 4 when obtaining different output electric signal under the different temperatures.
Fig. 3 is the calibration result under room temperature to 315 ℃ condition, and wherein horizontal ordinate is a temperature, and ordinate is the ratio of calorimetric constant-be output power and bridge for measuring temperature output signal (voltage), and this ratio increases and dull increasing with temperature.
Fig. 4 is for measuring the oxidation kinetics result of dotriacontane silica sand under four temperature who contains 7.6wt%, and discrete point is a measurement data, and solid line is based on the matched curve of reaction mechanism.Can obtain thermodynamics and thermokinetic parameters such as this organic reaction heat, the order of reaction (one-level), energy of activation and rate constant according to these results.This experiment can be used for the chemical simulation of combustion (of oil) in site in the tertiary oil recovery.
Claims (9)
1. thermal power measurement device, it is characterized in that: said device comprises thermostat, thermal measurement device, hot caliberating device and data acquisition and control device; Said thermostat comprises temperature controller and the thermostat body of heater that is attached thereto; Be provided with the calorimetric tube in the said thermostat body of heater; Said calorimetric tube comprises the constant temperature screen that the reaction tank cavity is outer with being set in said reaction tank cavity, is provided with ring cavity between said reaction tank cavity and the said constant temperature screen; Two ends of said ring cavity are respectively equipped with the soaking piece; Be equipped with groove in each said soaking piece; Said thermal measurement device comprises bridge for measuring temperature, and said bridge for measuring temperature comprises that two temperature detecting resistance silks on the said reaction tank cavity that is wrapped in said ring cavity counterpart, two temperature detecting resistance silks, the bridge that is wrapped on the said groove inwall flow adjusting resistance and dc signal source; Said hot caliberating device comprises that on the said reaction tank cavity that is wrapped in said ring cavity counterpart demarcates resistance wire and the direct supply that is attached thereto; Said temperature controller links to each other with control device with said data acquisition; Said bridge for measuring temperature links to each other with control device with said data acquisition.
2. measurement mechanism according to claim 1 is characterized in that: the outer wall of the said reaction tank cavity of said ring cavity counterpart is provided with insulation course.
3. measurement mechanism according to claim 1 and 2 is characterized in that: the inwall of said groove is provided with insulation course.
4. measurement mechanism according to claim 1 is characterized in that: said temperature detecting resistance silk and said demarcation resistance wire are resistive platinum wire.
5. measurement mechanism according to claim 1 is characterized in that: said direct supply is a programme-controlled dc power.
6. measurement mechanism according to claim 1 is characterized in that: said temperature detecting resistance silk uniform winding is on the said reaction tank cavity and on the inwall of said groove; Said demarcation resistance wire uniform winding is on said reaction tank cavity.
7. measurement mechanism according to claim 1 is characterized in that: said data acquisition and control device comprise data collecting card and the computing machine that is attached thereto; Said bridge for measuring temperature links to each other with said data collecting card; Said direct supply links to each other with said computing machine.
8. measurement mechanism according to claim 1 is characterized in that: said reaction tank cavity is provided with pressure transducer and/or flowmeter.
9. measurement mechanism according to claim 1 is characterized in that: said reaction tank cavity links to each other with chromatograph, mass spectrometer or spectrometer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100800732A CN102156009B (en) | 2011-03-31 | 2011-03-31 | Device for measuring thermal power |
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| CN2011100800732A CN102156009B (en) | 2011-03-31 | 2011-03-31 | Device for measuring thermal power |
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| CN102156009B true CN102156009B (en) | 2012-08-08 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102435352B (en) * | 2011-09-13 | 2013-05-29 | 中国航天科工集团第二研究院二〇三所 | Control and acquisition device of microwave power calorimeter |
| CN103712716B (en) * | 2014-01-06 | 2016-03-23 | 中国科学院化学研究所 | A kind of thermal power measurement device |
| CN104199492A (en) * | 2014-08-15 | 2014-12-10 | 北京无线电计量测试研究所 | Temperature regulating device for measuring radio frequency/microwave power |
| CN106950250B (en) * | 2017-05-05 | 2019-09-27 | 中国科学院化学研究所 | Thermal power measurement device with Visible imaging simulation measurement function |
| CN107976467B (en) * | 2017-12-04 | 2019-12-10 | 中国科学院化学研究所 | Thermal power measuring device with Raman spectrum measuring function |
| CN108318156B (en) * | 2018-03-08 | 2019-05-14 | 中国科学院化学研究所 | A kind of thermal power measurement device and measurement method |
| CN113418623A (en) * | 2021-05-17 | 2021-09-21 | 天津钢铁集团有限公司 | Non-contact type temperature measuring device for slag line part of lower nozzle and slag line adjusting method |
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| CN101470088A (en) * | 2007-12-28 | 2009-07-01 | 中国航天科技集团公司第五研究院第五一〇研究所 | Test method for low-temperature thermal conductivity of fluid |
| CN101576520A (en) * | 2009-06-03 | 2009-11-11 | 中国科学院化学研究所 | Thermal power measurement device |
| CN101842679A (en) * | 2007-10-25 | 2010-09-22 | 梅特勒-托利多公开股份有限公司 | Thermostat |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101842679A (en) * | 2007-10-25 | 2010-09-22 | 梅特勒-托利多公开股份有限公司 | Thermostat |
| CN101470088A (en) * | 2007-12-28 | 2009-07-01 | 中国航天科技集团公司第五研究院第五一〇研究所 | Test method for low-temperature thermal conductivity of fluid |
| CN101576520A (en) * | 2009-06-03 | 2009-11-11 | 中国科学院化学研究所 | Thermal power measurement device |
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