CN103196784B - Device and method for measuring gas-liquid chemical reaction rate based on volumetric method - Google Patents
Device and method for measuring gas-liquid chemical reaction rate based on volumetric method Download PDFInfo
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- CN103196784B CN103196784B CN201310120133.8A CN201310120133A CN103196784B CN 103196784 B CN103196784 B CN 103196784B CN 201310120133 A CN201310120133 A CN 201310120133A CN 103196784 B CN103196784 B CN 103196784B
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Abstract
The invention discloses a device and a method for measuring the gas-liquid chemical reaction rate based on a volumetric method, and belongs to the field of chemical reaction engineering. The device consists of a gas source system, a vacuum system, a gas metering system, a gas-liquid reaction system, a heating system, a stirring system, a cooling system and a data acquisition system, wherein a solution and a magnetic stirrer are arranged in a gas-liquid reaction cavity through a liquid inlet; the vacuum pump is used for vacuumizing a metering cavity and the gas-liquid reaction cavity; residual gas is eliminated; a vacuum electromagnetic valve is closed; gas with appointed pressure is fed into the metering cavity; the mole number of the gas is calculated; a gas source electromagnetic valve is closed; then the solution is subjected to temperature control and stirring; when a reaction condition is achieved, a pressure equivalence electromagnetic valve is opened; reaction gas is injected into the gas-liquid reaction cavity; when the pressure is balanced, the pressure equivalence electromagnetic valve is closed; and the chemical reaction rate is obtained by monitoring the change of the gas along with the time in the gas-liquid reaction cavity. According to the device, a test process is automatic, and the temperature control precision and the temperature measurement precision are high; and the device is convenient to operate.
Description
Technical field
The invention belongs to Chemical Reaction Engineering field, relate to a kind of device based on volumetric determination gas-liquid chemical reaction rate and assay method, be suitable for rate constant when mensurated gas composition and liquid generation chemical reaction, and obtain corresponding rate equation.
Background technology
Gas liquid reaction is typical process control link in Chemical Reaction Engineering, plays an important role in fields such as industry, medical treatment, teaching, scientific researches.As, adopt wet method to remove SO in generating plant or kiln tail gas
2, absorb in CO, industrial methane with copper ammon solution in ammonia synthesizing industry and adopt alkaline solution absorption CO
2, adopt CO more than NaOH solution absorption of residual in copper gas washing
2, adopt in chemical analysis copper ammon solution to demarcate in oxygen concentration, medical oxygen to adopt silver ammino solution to detect trace amounts of CO etc.The speed of reaction rate determines the input ability of raw material, the fan-out capability of product and the size of reaction vessel, directly affect one-time investment and the operation expense of enterprise, efficient reaction conditions for reduction energy consumption, raise the efficiency and increase profit and have great importance, therefore, the speed and the acquisition respective rate equation that measure chemical reaction are the keys solved the problem.
Usually, in gas liquid reaction, the concentration of liquid adopts titrimetry, chromatography or pH value method etc. to carry out labor measurement, and data acquisition is delayed, cannot obtain the instantaneous value of chemical reaction rate, have impact on the measurement precision of data; And gas is a kind of compressible medium, no matter as reactant or product, all can there is transient change with the carrying out of reaction in its volume or pressure, carry out tight tracking, reflected the real time status of chemical reaction to chemical reaction process.In addition, for high-temperature high-voltage reaction condition, get liquid analytic process more difficult, measure concrete condition when liquid property cannot reflect high-temperature high-pressure state at normal temperatures and pressures, and the now change of gas property is sensitiveer, the physical parameter of measurement gas expands the measurement range of chemical reaction rate.
At present, the report measuring chemical reaction rate is more common in education experiment, as, " improvement of a measurement zinc and sulfuric acid reaction rate experiments device " literary composition (experimental teaching and instrument, 2010, (9): 30) adopt the volume of syringe meter gaseous " ' different catalysts is on the impact of hydrogen peroxide dissociation reaction speed ' experimental provision designs and a probes into " literary composition (Cangzhou teacher training school journal, 2008,24(3): 42) adopt soap bubble flowmeter to measure the volume producing gas; " hydrochloric acid and acetic acid reaction RATES and dissociation equilibrium move experimental provision " literary composition (instruments used for education and experiment, 2004, (4): 31-32) adopts graduated cylinder to measure the volume producing gas.These methods belong to constant-voltage method, and by measurement gas volume change chemistry reaction rate, its weak point is comparatively obvious.First, syringe, soap bubble flowmeter or graduated cylinder etc. cannot realize the automatic measurement to volume, and necessary manual operation and reading registration, add the error of indication and subjectivity; Secondly, in gasmetry process, because the error caused that vanishes of residual gas, frictional resistance or soap bubble in container is difficult to eliminate; Again, this kind of experiment all adopts glass container, cannot be applicable to high pressure or pyroreaction condition; Finally, for complex conditions reaction rate measuring process, due to cannot robotization be realized, add labour cost, be difficult to raise the efficiency.
Summary of the invention
The object of the invention is to develop a kind of device based on volumetric determination gas-liquid chemical reaction rate, under guarantee gas volume permanence condition, real time dynamic measurement can be carried out to gas pressure intensity by high-precision pressure sensor by constant volume transformation mode, avoid conventional constant voltage method measurement volumes and cannot realize robotization, add labour cost, be difficult to the drawback of raising the efficiency, there is real-time and reliability.
A kind of device based on volumetric determination gas-liquid chemical reaction rate, utilize constant volume method to adopt buffer container substep meter air or measure the mode of giving vent to anger step by step to control reactant or product, calculate the consumption of reactant or the output speed of product by the change of gas pressure intensity in monitoring chemical reaction in good time, thus calculate rate constant and the rate equation of chemical reaction process.This device is made up of air supply system, vacuum system, gas metering system, gas liquid reaction system, heating system, stirring system, cooling system and data acquisition system (DAS) eight part.
Wherein said air supply system is made up of source of the gas gas cylinder to be measured, reduction valve, source of the gas solenoid valve and source of the gas joint flange.The gas of chemical reaction participated in by source of the gas gas cylinder to be measured for holding, because storage pressure is higher, need, through reduction valve, pressure is reduced to the required pressure of chemical reaction operation, reduction valve is connected with source of the gas gas cylinder to be measured by high pressure sealing screw thread.Source of the gas solenoid valve is opened or closed by programmed control, and enter measurement chamber for the source of the gas to be measured controlled through decompression, source of the gas solenoid valve is connected with source of the gas joint flange with reduction valve by pipeline, and source of the gas joint flange is for connecting air supply system and measurement chamber.
Described vacuum system is made up of bonding in vacuum flange, vacuum solenoid and vacuum pump.Vacuum system is connected with measurement chamber by bonding in vacuum flange, for vacuumizing measurement chamber, gets rid of the impact of residual gas.Vacuum pump, vacuum solenoid are connected by pipeline with bonding in vacuum flange, and vacuum solenoid is opened or closed by programmed control.
Described gas metering system is by measurement chamber, measurement chamber thermocouple sheath, measurement chamber thermopair, all press joint flange, measurement chamber pressure measurement joint flange and measurement chamber pressure transducer to form.Measurement chamber thermopair is placed in measurement chamber thermocouple sheath, and measurement chamber thermocouple sheath stretches in measurement chamber, is linked together by welding technology and measurement chamber, and measurement chamber thermopair is for measuring the temperature of metering intracavity gas.Measurement chamber pressure transducer is connected with measurement chamber by measurement chamber pressure measurement joint flange, for measuring the pressure of metering intracavity gas.Measurement chamber is connected with equal pressure electromagnetic valve by all pressing joint flange.
Described gas liquid reaction system is made up of equal pressure electromagnetic valve, reaction chamber pressure transducer, gas liquid reaction chamber, inlet, the even sleeve pipe of gas thermometric, gas temperature thermocouple, the even sleeve pipe of liquid thermometric and liquid temperature thermocouple; Gas temperature thermocouple is placed in the even sleeve pipe of gas thermometric, and the even sleeve pipe of gas thermometric inserts top, gas liquid reaction chamber, and linked together by welding technology and gas liquid reaction chamber, gas temperature thermocouple is for measuring the temperature of gas liquid reaction chamber headspace gases; Liquid temperature thermocouple is placed in the even sleeve pipe of liquid thermometric, the even sleeve pipe of liquid thermometric inserts bottom, gas liquid reaction chamber, but higher than magnetic stir bar height, linked together by welding technology and gas liquid reaction chamber, liquid temperature thermocouple is for measuring the temperature of gas liquid reaction chamber lower space liquid; Inlet is the pipeline with square nut, is linked together by welding technology with gas liquid reaction chamber, for putting into or pouring liquids, putting into or pouring out magnetic stir bar, during work, by supporting bolt seal; Reaction chamber pressure transducer is arranged on above Y shape cooling worm by screw thread, for measuring the pressure of gas liquid reaction intracavity gas, when gas liquid reaction temperature is higher, cooled by liquid vapour by the heat eliminating medium in cooling jacket, what ensure that reaction chamber pressure transducer records is the pressure of reacting gas; Y shape cooling worm internal diameter is between 4 ~ 7mm, and internal diameter is excessive, and heat transfer cooling effect is poor, and internal diameter is too small, and the liquid of condensation is due to surface tension meeting blocking pipeline;
Described gas heating system is made up of heater strip, the equal backing of metal, temperature-control heat couple, heating cable and temperature control instrument.Heater strip is inner at the equal backing of metal by insulating material uniform winding, is connected with temperature control instrument by heating cable, and it is inner that temperature-control heat couple is placed in the equal backing of metal, with gas liquid reaction chamber close contact, reaches the effect of quick temperature measurement and temperature control.It is peripheral that metal soaking sheet is looped around gas liquid reaction chamber, its bottom is coincide together by metal blank pressing technology, the even heat that heater strip produces is distributed in the outer wall in gas liquid reaction chamber by the equal backing of metal, is heated gas liquid reaction chamber internal-response thing by heat exchange pattern.
Described gas agitating system accelerates knob by magnetic stir bar, magnetic stirring apparatus and stirring and forms.Magnetic stir bar puts into gas liquid reaction chamber by inlet, and magnetic stir bar is by the coated magnetic material of wear-resisting organic material, in the moving magnetic field rotated, carry out circular motion.Magnetic stirring apparatus produces the magnetic field rotated, and accelerates the frequency that knob can change rotating magnetic field, thus change the circular motion speed of magnetic stir bar by regulating to stir.
Described cooling system is made up of cooling jacket, cooling jacket entrance, cooling jacket outlet, Y shape cooling worm and coiled pipe joint flange.Y shape cooling worm top is Y shape bifurcated, makes condensed fluid flow into gas liquid reaction chamber, and bottom is the spiral coiled pipe or spirality pipeline that rise, is connected bottom by coiled pipe joint flange with gas liquid reaction chamber.Heat eliminating medium is flow through in Y shape cooling worm outside, and heat eliminating medium enters from cooling jacket entrance, overflows from cooling jacket outlet.Y shape cooling worm and cooling jacket (16) are by being welded together.
Described data acquisition system (DAS) is made up of data acquisition and valve controling circuit plate and host computer.Host computer is imported into as calculating data after the voltage that measurement chamber thermopair, gas temperature thermocouple, liquid temperature thermocouple, measurement chamber pressure transducer and reaction chamber pressure transducer import into by data acquisition and valve controling circuit plate or current analog signal are converted into digital signal.When pressure condition meet setting require time, host computer sends digital switch instruction to data acquisition and valve controling circuit plate, digital signal is converted into voltage signal by data acquisition and valve controling circuit plate, drive source of the gas solenoid valve, vacuum solenoid or equal pressure electromagnetic valve to open or close, realize the automatic control of program.
It is thinning that processing is passed through in the even sleeve pipe of described measurement chamber thermocouple sheath, gas thermometric and the even sleeve pipe front end of liquid thermometric, strengthen heat-conductive characteristic, its wall thickness is no more than 0.3 mm, thus improves the sensitivity of measurement chamber thermopair, gas temperature thermocouple and survey body temperature thermocouple.
The gas liquid reaction rate test process of the described device based on volumetric determination gas-liquid chemical reaction rate is as follows: first, magnetic stir bar is placed in gas liquid reaction chamber by inlet, the solution prepared is put into gas liquid reaction chamber by funnel through inlet, sealing inlet, gas liquid reaction chamber is placed on magnetic stirring apparatus, open magnetic stirring apparatus switch, Stirring accelerates knob, magnetic stir bar is rotated in a liquid, open temperature control instrument, setting heating-up temperature, temperature control is carried out to gas liquid reaction chamber, open host computer and data acquisition and valve controling circuit plate.Then, open vacuum pump, open vacuum solenoid, equal pressure electromagnetic valve and source of the gas solenoid valve, gas circuit and cavity are vacuumized, remove foreign gas and liquid upper steam, when pressure reaches designated value, close vacuum solenoid, source of the gas solenoid valve and equal pressure electromagnetic valve, open source of the gas gas cylinder to be measured, when reduction valve pressure adjusting is to specified pressure value, open source of the gas solenoid valve, after measurement chamber pressure transducer institute pressure measurement force value and measurement chamber thermopair measured temperature are stablized, record metering intracavity gas force value and temperature value, because metering chamber volume is known, the number of moles of gas entering measurement chamber is calculated according to the equation of gas state.Afterwards, when the liquid temperature thermocouple numerical value in gas liquid reaction chamber and temperature control instrument setting value phase difference constant, the temperature value of the gentle body temperature thermocouple of force value of record reaction chamber pressure transducer, fill liquor capacity calculating gas liquid reaction chamber headspace gases volume according to gas liquid reaction cavity volume and institute, then according to the molal quantity of equation of gas state calculating liquid vapour.Now, open equal pressure electromagnetic valve, because gaseous tension in measurement chamber is higher than vapor pressure in gas liquid reaction chamber, gas in measurement chamber enters gas liquid reaction chamber through equal pressure electromagnetic valve, with liquid generation chemical reaction, when measurement chamber pressure transducer institute measuring pressure numerical value and reaction chamber pressure transducer institute measuring pressure value difference value constant time, close equal pressure electromagnetic valve, be worth over time by data acquisition and valve controling circuit plate record gas liquid reaction cavity pressure, the molal quantity of gas liquid reaction intracavity gas minimizing can be calculated according to Dalton's law (of partial pressures), thus calculate the speed of gas liquid reaction.
In the length of described Y shape cooling worm and cooling jacket, the temperature of heat eliminating medium is determined by actual needs, ensures reaction chamber pressure transducer place frozen-free liquid.
Described temperature-control heat couple can adopt the thermometric components and parts such as thermal resistance, thermistor meeting temperature-controlled precision and require.
The equal backing of described metal adopts the materials such as red copper, aluminium or the stainless steel that heat conductivility is good.
Described measurement chamber thermopair, liquid temperature thermocouple gentle body temperature thermocouple can adopt other thermometric components and parts meeting on-the-spot accuracy requirement respectively, as thermal resistance, thermistor etc. substitute.
The measurement chamber constant volume pressure measurement that the present invention proposes, gas-liquid separation thermometric, endless metal homogeneous heating, external heated for controlling temperature, cooling remove the mode such as liquid, divided dose input reaction gas and ensure that the reliable and stable of this contrive equipment test performance, simple and convenient, study the strong test unit of gas liquid reaction speed, the reaction of various gas and liquid under being applicable to different temperatures, different pressures, can also measure the gas at rest uptake when reaction rate of liquid desorption gas inverse process and gas liquid reaction are in mobile equilibrium as required.
Accompanying drawing explanation
Fig. 1 is the principle of work schematic diagram of apparatus of the present invention;
In Fig. 1: 1. source of the gas gas cylinder to be measured; 2. reduction valve; 3. source of the gas solenoid valve; 4. source of the gas joint flange; 5. measurement chamber; 6. measurement chamber thermocouple sheath; 7. measurement chamber thermopair; 8. all press joint flange; 9. measurement chamber pressure measurement joint flange; 10. measurement chamber pressure transducer; 11. bonding in vacuum flanges; 12. vacuum solenoids; 13. vacuum pumps; 14. equal pressure electromagnetic valves; 15. reaction chamber pressure transducers; 16. cooling jackets; 17. cooling jacket entrances; 18. cooling jacket outlets; 19. Y shape cooling worms; 20. coiled pipe joint flanges; 21. gas liquid reaction chambeies; 22. inlets; The even sleeve pipe of 23. gas thermometrics; 24. gas temperature thermocouples; The even sleeve pipe of 25. liquid thermometrics; 26. liquid temperature thermocouples; 27. heater strips; The equal backing of 28. metal; 29. magnetic stir bars; 30. magnetic stirring apparatuss; 31. stir acceleration knob; 32. temperature-control heat couple; 33. heating cables; 34. temperature control instruments; 35. data acquisitions and valve controling circuit plate; 36. host computers;
Fig. 2 is placed in all thermopairs in container and sleeve pipe sketch thereof in apparatus of the present invention;
6. measurement chamber thermocouple sheath; 7. measurement chamber thermopair; The even sleeve pipe of 23. gas thermometrics; 24. gas temperature thermocouples; The even sleeve pipe of 25. liquid thermometrics; 26. liquid temperature thermocouples.
Embodiment
The embodiment of the present invention measures the chemical reaction rate of monoethanolamine solution (MEA) and carbon dioxide, select 30% MEA solution 500mL, measurement chamber 5 volume is 500mL, gas liquid reaction chamber 21 volume is 1000mL, measurement chamber thermopair 7, gas temperature thermocouple 24 and liquid temperature thermocouple 26 all adopt the T-shaped thermopair of one-level, and its precision is ± 0.5 DEG C.Measurement chamber pressure transducer 10 adopts pressure limit to be 0 ~ 1MPa, and precision is the piezoelectric transducer of ± 0.06%, and reaction chamber pressure transducer 15 adopts working pressure range to be 0 ~ 0.2MPa, maximumly bears pressure 1MPa, and precision is the piezoresistive transducer of ± 0.06%.Vacuum pump 13 speed of exhaust is 0.5L/s, and source of the gas gas cylinder 1 to be measured is the dioxide bottle of 40L, and top pressure is 15MPa, and reduction valve 2 maximum range is 1.4MPa.Cooling jacket 16 is connected with recirculated cooling water, and circulating cooling coolant-temperature gage controls at 1 ± 0.1 DEG C.The temperature of measurement chamber 5 is room temperature 28 DEG C, and temperature control instrument 34 temperature is set to 40 DEG C.
See Fig. 1 and Fig. 2, magnetic stir bar 29 and 30%MEA solution are placed in gas liquid reaction chamber 21 by inlet 22, sealing inlet, gas liquid reaction chamber 21 is placed on magnetic stirring apparatus 30, adjustment is stirred and is accelerated knob 31, make magnetic stir bar 29 Rotating with Uniform in a liquid, open temperature control instrument 34, setting heating-up temperature is 40 DEG C, open host computer 36 and data acquisition and valve controling circuit plate 35, open vacuum pump 13, open vacuum solenoid 12 and equal pressure electromagnetic valve 14, gas circuit and cavity are vacuumized, when pressure instantaneous value is lower than 1Pa, close equal pressure electromagnetic valve 14 and vacuum solenoid 12, open source of the gas gas cylinder 1 to be measured, open reduction valve 2, be adjusted to 1MPa.Open source of the gas solenoid valve 3, be filled with the carbon dioxide of 1.0MPa to measurement chamber 5, after cavity pressure sensor 10 pressure vary stable to be batched, close source of the gas solenoid valve 3, calculate the molal quantity being filled with carbon dioxide in measurement chamber 5 according to the equation of gas state.When the temperature that liquid temperature thermocouple 26 records in gas liquid reaction chamber 21 reaches 40 ± 0.1 DEG C, open equal pressure electromagnetic valve 14, when measurement chamber pressure transducer 10 force value and reaction chamber pressure transducer 15 pressure measurement force value differ meet program setting requirement time, close equal pressure electromagnetic valve 14.Now, the changing value of monitoring reaction chamber pressure transducer 15 pressure, make curve to the time, until when its force value rate of change is less than 120Pa/s, reaction terminates.According to the vapour pressure of the temperature 40 DEG C calculating liquid that gas temperature thermocouple 24 records, then calculate according to the equation of gas state and Dalton's law (of partial pressures) the carbon dioxide molar weight entering gas liquid reaction chamber 21.Calculate carbon dioxide dividing potential drop rate over time by reaction pressure curve, then draw chemical reaction rate by the volume computing in gas liquid reaction chamber 21, thus provide the rate equation of carbon dioxide and 30%MEA solution reaction.
Claims (6)
1., based on a device for volumetric determination gas-liquid chemical reaction rate, it is characterized in that this device is made up of air supply system, vacuum system, gas metering system, gas liquid reaction system, heating system, stirring system, cooling system and data acquisition system (DAS) eight part;
Wherein said air supply system is made up of source of the gas gas cylinder (1) to be measured, reduction valve (2), source of the gas solenoid valve (3) and source of the gas joint flange (4); Source of the gas gas cylinder (1) to be measured participates in the gas of chemical reaction for holding, because storage pressure is higher, need, through reduction valve (2), pressure is reduced to the required pressure of chemical reaction operation, reduction valve (2) is connected with source of the gas gas cylinder (1) to be measured by high pressure sealing screw thread; Source of the gas solenoid valve (3) is opened or closed by programmed control, measurement chamber (5) is entered for the source of the gas to be measured controlled through decompression, source of the gas solenoid valve (3) is connected with source of the gas joint flange (4) with reduction valve (2) by pipeline, and source of the gas joint flange (4) is for the connection of air supply system and measurement chamber (5);
Described vacuum system is made up of bonding in vacuum flange (11), vacuum solenoid (12) and vacuum pump (13); Vacuum system is connected with measurement chamber (5) by bonding in vacuum flange (11), for vacuumizing measurement chamber (5), gets rid of the impact of residual gas; Vacuum pump (13), vacuum solenoid (12) are connected by pipeline with bonding in vacuum flange (11), and vacuum solenoid (12) is opened or closed by programmed control;
Described gas metering system is by measurement chamber (5), measurement chamber thermocouple sheath (6), measurement chamber thermopair (7), all press joint flange (8), measurement chamber pressure measurement joint flange (9) and measurement chamber pressure transducer (10) to form; Measurement chamber thermopair (7) is placed in measurement chamber thermocouple sheath (6), measurement chamber thermocouple sheath (6) stretches in measurement chamber (5), linked together by welding technology and measurement chamber (5), measurement chamber thermopair (7) is for measuring the temperature of measurement chamber (5) interior gas; Measurement chamber pressure transducer (10) is connected with measurement chamber (5) by measurement chamber pressure measurement joint flange (9), for measuring the pressure of measurement chamber (5) interior gas; Measurement chamber (5) is by all pressing joint flange (8) to be connected with equal pressure electromagnetic valve (14);
Described gas liquid reaction system is made up of equal pressure electromagnetic valve (14), reaction chamber pressure transducer (15), gas liquid reaction chamber (21), inlet (22), the even sleeve pipe (23) of gas thermometric, gas temperature thermocouple (24), the even sleeve pipe (25) of liquid thermometric and liquid temperature thermocouple (26); Gas temperature thermocouple (24) is placed in the even sleeve pipe (23) of gas thermometric, the even sleeve pipe (23) of gas thermometric inserts gas liquid reaction chamber (21) top, linked together by welding technology and gas liquid reaction chamber (21), gas temperature thermocouple (24) is for measuring the temperature of gas liquid reaction chamber (21) headspace gases; Liquid temperature thermocouple (26) is placed in the even sleeve pipe (25) of liquid thermometric, the even sleeve pipe (25) of liquid thermometric inserts gas liquid reaction chamber (21) bottom, but higher than magnetic stir bar height, linked together by welding technology and gas liquid reaction chamber (21), liquid temperature thermocouple (26) is for measuring the temperature of gas liquid reaction chamber (21) lower space liquid; Inlet (22) is the pipeline with square nut, being linked together by welding technology with gas liquid reaction chamber (21), for putting into or pouring liquids, putting into or pouring out magnetic stir bar (29), during work, by supporting bolt seal; Reaction chamber pressure transducer (15) is arranged on Y shape cooling worm (19) top, for measuring the pressure of gas liquid reaction chamber (21) interior gas by screw thread; Y shape cooling worm (19) internal diameter is between 4 ~ 7mm;
Described gas heating system is made up of heater strip (27), the equal backing of metal (28), temperature-control heat couple (32), heating cable (33) and temperature control instrument (34); Heater strip (27) is inner at the equal backing of metal (28) by insulating material uniform winding, be connected with temperature control instrument (34) by heating cable (33), it is inner that temperature-control heat couple (32) is placed in the equal backing of metal (28), with gas liquid reaction chamber (21) close contact, reach the effect of quick temperature measurement and temperature control; It is peripheral that the equal backing of metal (28) is looped around gas liquid reaction chamber (21), its bottom is coincide together by metal blank pressing technology, the even heat that heater strip (27) produces is distributed in the outer wall of gas liquid reaction chamber (21) by the equal backing of metal (28), is heated gas liquid reaction chamber (21) internal-response thing by heat exchange pattern;
Described gas agitating system accelerates knob (31) by magnetic stir bar (29), magnetic stirring apparatus (30) and stirring and forms; Magnetic stir bar (29) puts into gas liquid reaction chamber (21) by inlet, and magnetic stir bar (29) is by the coated magnetic material of wear-resisting organic material, in the moving magnetic field rotated, carry out circular motion; Magnetic stirring apparatus (30) produces the magnetic field rotated, and accelerates the frequency that knob (31) can change rotating magnetic field, thus change the circular motion speed of magnetic stir bar (29) by regulating to stir;
Described cooling system is exported (18), Y shape cooling worm (19) and coiled pipe joint flange (20) formed by cooling jacket (16), cooling jacket entrance (17), cooling jacket; Y shape cooling worm (19) top is Y shape bifurcated, condensed fluid is made to flow into gas liquid reaction chamber (21), bottom is the spirality pipeline risen that spirals, and is connected bottom by coiled pipe joint flange (20) with gas liquid reaction chamber (21); Heat eliminating medium is flow through in Y shape cooling worm (19) outside, and heat eliminating medium enters from cooling jacket entrance (17), overflows from cooling jacket outlet (18); Y shape cooling worm (19) and cooling jacket (16) are by being welded together;
Described data acquisition system (DAS) is made up of data acquisition and valve controling circuit plate (35) and host computer (36); Host computer (36) is imported into as calculating data after the voltage that measurement chamber thermopair (7), gas temperature thermocouple (24), liquid temperature thermocouple (26), measurement chamber pressure transducer (10) and reaction chamber pressure transducer (15) import into by data acquisition and valve controling circuit plate (35) or current analog signal are converted into digital signal; When pressure condition meet setting require time, host computer (36) sends digital switch instruction to data acquisition and valve controling circuit plate (35), digital signal is converted into voltage signal by data acquisition and valve controling circuit plate (35), drive source of the gas solenoid valve (3), vacuum solenoid (12) or equal pressure electromagnetic valve (14) to open or close, realize the automatic control of program;
Described measurement chamber thermocouple sheath (6), the even sleeve pipe (23) of gas thermometric and even sleeve pipe (26) front end of liquid thermometric are thinning through processing, and strengthen heat-conductive characteristic, its wall thickness is no more than 0.3mm.
2. one kind adopts as claimed in claim 1 based on the assay method of the device of volumetric determination gas-liquid chemical reaction rate, it is characterized in that gas liquid reaction rate test process is as follows: first, magnetic stir bar is placed in gas liquid reaction chamber by inlet, the solution prepared is put into gas liquid reaction chamber by funnel through inlet, sealing inlet, gas liquid reaction chamber is placed on magnetic stirring apparatus, open magnetic stirring apparatus switch, Stirring accelerates knob, magnetic stir bar is rotated in a liquid, open temperature control instrument, setting heating-up temperature, temperature control is carried out to gas liquid reaction chamber, open host computer and data acquisition and valve controling circuit plate, then, open vacuum pump, open vacuum solenoid, equal pressure electromagnetic valve and source of the gas solenoid valve, gas circuit and cavity are vacuumized, remove foreign gas and liquid upper steam, when pressure reaches designated value, close vacuum solenoid, source of the gas solenoid valve and equal pressure electromagnetic valve, open source of the gas gas cylinder to be measured, when reduction valve pressure adjusting is to specified pressure value, open source of the gas solenoid valve, after measurement chamber pressure transducer institute pressure measurement force value and measurement chamber thermopair measured temperature are stablized, record metering intracavity gas force value and temperature value, because metering chamber volume is known, the number of moles of gas entering measurement chamber is calculated according to the equation of gas state, afterwards, when the liquid temperature thermocouple numerical value in gas liquid reaction chamber and temperature control instrument setting value phase difference constant, the temperature value of the gentle body temperature thermocouple of force value of record reaction chamber pressure transducer, fill liquor capacity calculating gas liquid reaction chamber headspace gases volume according to gas liquid reaction cavity volume and institute, then according to the molal quantity of equation of gas state calculating liquid vapour, now, open equal pressure electromagnetic valve, because gaseous tension in measurement chamber is higher than vapor pressure in gas liquid reaction chamber, gas in measurement chamber enters gas liquid reaction chamber through equal pressure electromagnetic valve, with liquid generation chemical reaction, when measurement chamber pressure transducer institute measuring pressure numerical value and reaction chamber pressure transducer institute measuring pressure value difference value constant time, close equal pressure electromagnetic valve, be worth over time by data acquisition and valve controling circuit plate record gas liquid reaction cavity pressure, the molal quantity of gas liquid reaction intracavity gas minimizing can be calculated according to Dalton's law (of partial pressures), thus calculate the speed of gas liquid reaction.
3., as claimed in claim 1 based on the device of volumetric determination gas-liquid chemical reaction rate, it is characterized in that the temperature of heat eliminating medium in the length of Y shape cooling worm and cooling jacket is determined by actual needs, ensure reaction chamber pressure transducer place frozen-free liquid.
4., as claimed in claim 1 based on the device of volumetric determination gas-liquid chemical reaction rate, it is characterized in that temperature-control heat couple can substitute with thermal resistance, thermistor temperature detecting components and parts.
5., as claimed in claim 1 based on the device of volumetric determination gas-liquid chemical reaction rate, it is characterized in that the equal backing of metal adopts red copper, aluminium or stainless steel that heat conductivility is good.
6., as claimed in claim 1 based on the device of volumetric determination gas-liquid chemical reaction rate, it is characterized in that to substitute with thermal resistance, thermistor at measurement chamber thermopair, the gentle body temperature thermocouple of liquid temperature thermocouple.
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| JP2678635B2 (en) * | 1988-10-19 | 1997-11-17 | 三菱石油株式会社 | Lubricating oil gas absorption rate test method and test equipment |
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| CN101042387A (en) * | 2007-04-23 | 2007-09-26 | 中国科学院广州能源研究所 | Gas hydrate kinetics measuring method and apparatus thereof |
| CN101458241A (en) * | 2008-10-30 | 2009-06-17 | 西南石油大学 | Experimental method for detecting reaction speed of carbonate rock and hydrochloric acid |
| CN203164076U (en) * | 2013-04-08 | 2013-08-28 | 北京科技大学 | Device for determining gas-liquid chemical reaction rate based on volumetric method |
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