CN203561598U - Dissolution reaction dose heat device - Google Patents
Dissolution reaction dose heat device Download PDFInfo
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- CN203561598U CN203561598U CN201320738925.7U CN201320738925U CN203561598U CN 203561598 U CN203561598 U CN 203561598U CN 201320738925 U CN201320738925 U CN 201320738925U CN 203561598 U CN203561598 U CN 203561598U
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 39
- 238000004090 dissolution Methods 0.000 title abstract description 6
- 230000003381 solubilizing effect Effects 0.000 claims description 20
- 238000009413 insulation Methods 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 4
- 230000006978 adaptation Effects 0.000 claims description 3
- 239000011229 interlayer Substances 0.000 claims description 3
- 239000010410 layer Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000003908 quality control method Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000004907 flux Effects 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 238000007707 calorimetry Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The utility model discloses a dissolution reaction dose heat device. The dissolution reaction dose heat device comprises a machine box, a Dewar flask, an inserting unit, a constant-temperature groove and an agitator driving motor, wherein the inserting unit mainly comprises a sample tank, an agitator, a temperature sensor, an electric energy calibrating heater and a push rod through assembly; a dissolution reaction dose heat unit is composed of the Dewar flask and the inserting unit; the dissolution reaction dose heat unit is arranged in the constant-temperature groove and fixedly arranged on a constant-temperature groove cover plate; the agitator driving motor is arranged on the constant-temperature groove cover plate; the machine box is internally provided with a constant-current source circuit, a temperature acquisition circuit, a constant-temperature groove temperature control circuit and a motor power supply; cables are arranged on circuit interfaces, which correspond to the machine box, of the constant-current source circuit, the temperature acquisition circuit and the motor power supply, and are respectively connected with the electric energy calibrating heater, the temperature sensor and the agitator driving motor. The device is simple in structure, low in cost and convenient to use.
Description
Technical field
The utility model relates to and is applicable to chemistry, biology, medical science, pharmaceutical field experiment calorimeter assembly, is specially the experimental provision of the heat that in a kind of dissolving of measurement of species or course of reaction, institute absorbs or discharges.
Background technology
The thermal effect producing when a certain amount of solute is dissolved in a certain amount of solvent is under given conditions called heat of solution; After a chemical reaction occurs in constant voltage and do not make non-volume work in the situation that, if make the temperature of product get back to initial temperature, the heat that at this moment system is emitted or absorbed is called reaction heat.Solubilizing reaction calorimeter assembly is the experimental provision of the thermal change while recording sample dissolution or reaction.According to the principle of calorimetry, meltage hot charging is equipped with three kinds: the first is adiabatic calorimeter, under ideal conditions, between system and environment, there is no exchange heat, and this device is very complicated, and cost is high, seldom uses.The second is isoperibol formula calorimeter, and reaction system is placed in an isoperibol, has heat shield between system and surrounding, and both are reduced as far as possible in heat interchange.This device is fairly simple, and cost is lower, comparatively common.The third is heat-conducted calorimeter, reaction system is also placed in isoperibol, between system and surrounding, by heat flux sensor, separated, heat flux sensor can guarantee to have larger coefficient of heat conductivity between the two, the size of the thermoelectric force that heat flux sensor produces has reflected the dissolving that occurs in system or the neither endothermic nor exothermic speed of course of reaction, is called heat flow rate.By heat flow rate, the time is done to Integral Processing, can calculate calorie value.Such installs commercialization, but expensive, and cost is high.
What the utility model adopted is the calorimetric principle of isoperibol formula.Although the solubilizing reaction calorimeter assembly of the type is more common, some laboratories can oneself be set up, and have commercialization instrument.But all there is complicated operation, the problem such as in use consuming cost is higher.
Utility model content
The purpose of this utility model is to have complicated operation, deficiency that cost is higher for existing isoperibol formula solubilizing reaction calorimeter, and a kind of simple in structure, cost is low, easy to use, precision is high, reliability is high solubilizing reaction calorimeter assembly is provided.
The purpose of this utility model adopts following technical scheme to realize:
A solubilizing reaction calorimeter assembly, comprises cabinet, Dewar flask, plug-in unit, calibration cell and stirrer-driven motor; Plug-in unit is mainly combined by sample cell, stirrer, temperature sensor, energy calibration well heater, push rod; Dewar flask and plug-in unit form solubilizing reaction calorimetric unit, and it is placed in calibration cell, is fixed on calibration cell cover plate; Stirrer-driven motor is arranged on calibration cell cover plate; In cabinet, be provided with constant-current source circuit, temperature collection circuit, calibration cell temperature-control circuit and motor power; At the circuit interface of the corresponding cabinet of constant-current source circuit, temperature collection circuit, motor power, cable being set is connected with energy calibration well heater, temperature sensor, stirrer-driven motor respectively.
Described Dewar flask is Double-layer glass bottle, interlayer vacuum-pumping, and bottleneck top connects the tubulose bottleneck with its bore adaptation, and the upper end of bottleneck is provided with the cover plate of fixed head and calibration cell and fixes.Dewar flask is as reaction vessel, and thermal insulation protection is provided.
Described sample cell is provided with sleeve pipe, and push rod contacts with sample cell through sample cell sleeve pipe, by push rod Quality control container, discharges sample; Sample cell, sample cell sleeve pipe and push rod form a dismountable sample adding device.
Described plug-in unit is also provided with flange, constant temperature cylinder, heat insulation disk, and the corresponding position of three is provided with through hole, and sample cell sleeve pipe and stirrer pass through hole and fix with it; Heat insulation disk is also provided with the through hole of fixed temperature sensor and energy calibration well heater.
Described flange and heat insulation disk outside are provided with groove, groove is embedded with O type circle, the external diameter of this O type circle and the internal diameter of Dewar flask bottleneck are suitable, make plug-in unit can insert smoothly and realize sealing, this structure decrease the heat transmission between reaction system and indoor environment in calorimeter.
The electronic component of described temperature sensor is negative tempperature coefficient thermistor, the electronic component of energy calibration well heater is accurate wire-wound resistor, they are packaged in respectively in thin walled tube, gap-fill between element and tube wall has heat-conducting medium, temperature sensor and well heater are separately fixed in the through hole of heat insulation disk, and connecting cable is connected with circuit interface corresponding on cabinet respectively.
The upper end of described stirrer connects belt pulley, and stirrer-driven motor is connected with belt pulley by driving belt, drives stirrer uniform rotation, below the liquid level that mixing arm submerges in Dewar flask.
The utility model solubilizing reaction calorimetric unit is placed in calibration cell, and is fixed on calibration cell cover plate.Calibration cell provides the isoperibol of high stability for it, be less than ± 0.001K of its temperature fluctuation.The constant temperature cylinder of plug-in unit contacts with the bottleneck of Dewar flask and reaches thermal equilibrium with the thermostatic medium of calibration cell.Heat transmission between reaction system and indoor environment is separated and is split into two sections by constant temperature cylinder.Between heat insulation disk and constant temperature cylinder, between constant temperature cylinder and flange disk, be air, there is heat-blocking action.This structure has reduced the variation that Dewar flask internal temperature brings because of ectocine greatly, effectively raises the accuracy of measurement.
The utility model temperature sensor is connected with temperature collection circuit, this circuit can with computer communication, and by specific program, automatically gather and record the temperature variation of reaction system real-time rendering curve map.The resolution of temperature acquisition is 0.00001K.
The utility model energy calibration well heater is connected with constant-current source circuit, and this constant current source is the constant current source that degree of stability is less than 10 ppm, for well heater provides stable electric current.
The utility model sample cell adopts detachable structure, does not need as glass ampoule bottles, when measuring, is broken, and this structure is reusable, has reduced widely use cost.
The calorimetric principle of this solubilizing reaction calorimeter assembly is: calorimetric unit is placed in calibration cell, between system and surrounding, with adiabatic measure, separate, temperature sensor is converted into electric signal output by the temperature variation of solution in Dewar flask, when occurring dissolve or react, the temperature variation of solution goes on record, and accounting temperature changing value.The thermal capacitance that is multiplied by system by temperature change value, obtains calorie value.And the thermal capacitance of system is calculated by quantitative energy calibration, give the electric current of the logical certain hour of energy calibration resistance, the joule heating effect of its generation changes the temperature of system, record accounting temperature changing value, temperature change value with the calorie value of energy calibration divided by energy calibration process, obtains the thermal capacitance value of system.
The utility model apparatus structure is simple, cost is lower, easy to use.
Accompanying drawing explanation
Fig. 1 is the one-piece construction schematic diagram of embodiment;
Fig. 2 is the structural representation of embodiment Dewar flask;
Fig. 3 is the structural representation of embodiment plug-in unit.
In figure, 1. heat insulation disk 19. O type circle 20. sample cell sleeve pipe 21. sample cell 22. energy calibration well heater 23. push rods of cabinet 1-1. constant-current source circuit 1-2. temperature collection circuit 1-3. motor power 1-4. calibration cell temperature-control circuit 2. Dewar flask 3. plug-in unit 4. calibration cell cover plate 5. driving belt 6. stirrer-driven motor 7. calibration cell 8. Dewar flask bottleneck 9. Dewar flask fixed head 10. stirrer 11. temperature sensor 12. stirrer-driven belt pulley 13. temperature sensor cable 14. energy calibration heater cable line 15. flange 16. O type circle 17. constant temperature cylinder 18..
Embodiment
Below in conjunction with drawings and Examples, the utility model content is further elaborated, but is not to restriction of the present utility model.
Embodiment:
With reference to Fig. 1-3, a kind of solubilizing reaction calorimeter assembly, comprises cabinet 1, Dewar flask 2, plug-in unit 3, calibration cell 7 and stirrer-driven motor 6; Plug-in unit 3 is mainly combined by flange 15, constant temperature cylinder 17, heat insulation disk 18, O type circle 16 and 19, sample cell sleeve pipe 20, sample cell 21, stirrer 10, temperature sensor 11, energy calibration well heater 22, push rod 23; Dewar flask 2 and plug-in unit 3 form solubilizing reaction calorimetric unit; Solubilizing reaction calorimetric unit is placed in calibration cell 7, is fixed on calibration cell cover plate 4; Stirrer-driven motor 6 is arranged on calibration cell cover plate 4; In cabinet 1, be provided with constant-current source circuit 1-1, temperature collection circuit 1-2, calibration cell temperature-control circuit 1-4 and motor power 1-3 etc.; At the circuit interface of the corresponding cabinet 1 of constant-current source circuit 1-1, temperature collection circuit 1-2, motor power 1-3, cable being set is connected with energy calibration well heater 14, temperature sensor 11, drive motor 6 respectively.The circuit interface of the corresponding cabinet 1 of calibration cell temperature-control circuit 1-4 is provided with cable and is connected with temperature sensor, well heater and the circulation motor of calibration cell 7.
With reference to Fig. 2, Dewar flask 2 is Double-layer glass bottle, interlayer vacuum-pumping, and bottleneck top connects the tubulose bottleneck 8 with its bore adaptation, and it is fixing with calibration cell cover plate 4 that the upper end of bottleneck 8 is provided with fixed head 9.
With reference to Fig. 1, Fig. 3, sample cell 21 is provided with sleeve pipe 20, and push rod 23 contacts with sample cell 21 through sample cell sleeve pipe 20, by push rod 23 Quality control containers, discharges sample; Sample cell 21, sample cell sleeve pipe 20 and push rod 23 form a dismountable sample adding device.
With reference to Fig. 3, plug-in unit is also provided with flange 15, constant temperature cylinder 17, heat insulation disk 18, and the corresponding position of three is provided with through hole, and sample cell sleeve pipe 20 and stirrer 10 pass through hole and fix with it; Heat insulation disk 18 is also provided with the through hole of fixed temperature sensor 11 and energy calibration well heater 22.
The electronic component of temperature sensor 11 is negative tempperature coefficient thermistor, is called for short NTC, and the electronic component of energy calibration well heater 22 is accurate wire-wound resistor, and temperature coefficient is about 10ppm.They are packaged in respectively in thin walled tube, gap-fill between device and tube wall has heat-conducting medium, be separately fixed in the through hole of heat insulation disk 18, temperature sensor cable 13 is connected with the interface of temperature collection circuit 1-2, and energy calibration heater cable line 14 is connected with constant-current source circuit 1-1.
The upper end of stirrer 10 connects belt pulley 12, and stirrer-driven motor 6 is connected with belt pulley 12 by driving belt 5, drives stirrer 10 uniform rotation, below the liquid level that stirrer 10 blades submerge in Dewar flask 2.
Concrete test process is as follows:
When the test heat of solution of sample or reaction heat, first make calibration cell 7 temperature reach constant, be less than ± 0.001K of temperature fluctuation.In Dewar flask 2, inject a certain amount of solvent or reaction reagent, and be submerged in calibration cell 7, be fixed on constant temperature cover plate 4.In sample cell 21, accurately add quantitative sample, be then fixed in sample cell sleeve pipe 20 lower ends.Whole plug-in unit 3 is inserted in Dewar flask 2, connect good driving belt 5, start stirrer-driven motor 6, wait for that whole calorimetric unit and calibration cell 7 reach thermal equilibrium.After reaching thermal equilibrium, promote push rod 23, sample cell 21 is depressed, separated with sample cell sleeve pipe 20, falls, and discharges sample.
Sample can discharge or absorb heat in dissolving or course of reaction, causes that the temperature of system raises or reduction.This temperature variation is changed into electric signal by temperature sensor 11 and temperature collection circuit 1-2, and is further converted to digital signal and flows to computer program recorded and real-time rendering temperature-time curve.By processing this temperature-time curve, obtain the temperature change value of this process, the thermal capacitance value of articulated system can calculate the calorie value of this process.And the thermal capacitance value of system is by energy calibration process computation.
Because the resolution of temperature collection circuit 1-2 is 0.00001K, the temperature-coefficient of electrical resistance of energy calibration well heater 22 is 10ppm/K, and the fluctuation 10ppm of constant current source can guarantee accuracy and the repeatability of test result.This example be take potassium chloride as sample, when the temperature of calibration cell 7 is 25 ℃, surveys its heat of solution in water, and the mean value of 5 tests is 17.533 kJ/mol, and mean value standard deviation is 0.012 kJ/mol, coincide in error range with bibliographic reference value.
Claims (7)
1. a solubilizing reaction calorimeter assembly, comprises cabinet, Dewar flask, plug-in unit, calibration cell and stirrer-driven motor; Plug-in unit is mainly combined by sample cell, stirrer, temperature sensor, energy calibration well heater, push rod; It is characterized in that: Dewar flask and plug-in unit form solubilizing reaction calorimetric unit, and it is placed in calibration cell, is fixed on calibration cell cover plate; Stirrer-driven motor is arranged on calibration cell cover plate; In cabinet, be provided with constant-current source circuit, temperature collection circuit, calibration cell temperature-control circuit and motor power; At the circuit interface of the corresponding cabinet of constant-current source circuit, temperature collection circuit, motor power, cable being set is connected with energy calibration well heater, temperature sensor, stirrer-driven motor respectively.
2. solubilizing reaction calorimeter assembly according to claim 1, it is characterized in that: described Dewar flask is Double-layer glass bottle, interlayer vacuum-pumping, bottleneck top connects the tubulose bottleneck with its bore adaptation, and the upper end of bottleneck is provided with the cover plate of fixed head and calibration cell and fixes.
3. solubilizing reaction calorimeter assembly according to claim 1, is characterized in that: described sample cell is provided with sleeve pipe, and push rod contacts with sample cell through sample cell sleeve pipe, by push rod Quality control container, discharges sample; Sample cell, sample cell sleeve pipe and push rod form a dismountable sample adding device.
4. solubilizing reaction calorimeter assembly according to claim 1, is characterized in that: described plug-in unit is also provided with flange, constant temperature cylinder, heat insulation disk, and the corresponding position of three is provided with through hole, and sample cell sleeve pipe and stirrer pass through hole and fix with it; Heat insulation disk is also provided with the through hole of fixed temperature sensor and energy calibration well heater.
5. solubilizing reaction calorimeter assembly according to claim 4, is characterized in that: described flange and heat insulation disk outside are provided with groove, and groove is embedded with O type circle, and the external diameter of this O type circle and the internal diameter of Dewar flask bottleneck are suitable.
6. solubilizing reaction calorimeter assembly according to claim 1, is characterized in that: the electronic component of described temperature sensor is negative tempperature coefficient thermistor; The electronic component of energy calibration well heater is accurate wire-wound resistor, they are packaged in respectively in thin walled tube, gap-fill between element and tube wall has heat-conducting medium, temperature sensor and well heater are separately fixed in the through hole of heat insulation disk, and connecting cable is connected with circuit interface corresponding on cabinet respectively.
7. solubilizing reaction calorimeter assembly according to claim 1, is characterized in that: the upper end of described stirrer connects belt pulley, and stirrer-driven motor is connected with belt pulley by driving belt, drives stirrer uniform rotation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320738925.7U CN203561598U (en) | 2013-11-20 | 2013-11-20 | Dissolution reaction dose heat device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320738925.7U CN203561598U (en) | 2013-11-20 | 2013-11-20 | Dissolution reaction dose heat device |
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| CN203561598U true CN203561598U (en) | 2014-04-23 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105136851A (en) * | 2015-09-22 | 2015-12-09 | 中国石油大学(华东) | Device and method for measuring heat effect in isothermal hot reaction process of carbonaceous macromolecules |
| CN105444910A (en) * | 2015-12-30 | 2016-03-30 | 中国神华能源股份有限公司 | Reaction heat effect measurement device and method |
| CN106404227A (en) * | 2016-09-22 | 2017-02-15 | 李强国 | Multifunctional isothermal calorimeter |
| CN108426655A (en) * | 2018-05-18 | 2018-08-21 | 湘南学院 | Calorimetric reaction vessel for high-precision calorimeter |
| CN111194400A (en) * | 2017-11-06 | 2020-05-22 | 卡尔巴科特公司 | Calorimeter and sample container for calorimeter |
| CN112179527A (en) * | 2019-07-04 | 2021-01-05 | 中国建筑材料科学研究总院有限公司 | Isothermal calorimetry apparatus |
-
2013
- 2013-11-20 CN CN201320738925.7U patent/CN203561598U/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105136851A (en) * | 2015-09-22 | 2015-12-09 | 中国石油大学(华东) | Device and method for measuring heat effect in isothermal hot reaction process of carbonaceous macromolecules |
| CN105136851B (en) * | 2015-09-22 | 2018-06-26 | 中国石油大学(华东) | A kind of device and method for measuring fuel factor in carbonaceous macromolecular isothermal thermal process reactor |
| CN105444910A (en) * | 2015-12-30 | 2016-03-30 | 中国神华能源股份有限公司 | Reaction heat effect measurement device and method |
| CN105444910B (en) * | 2015-12-30 | 2018-01-16 | 中国神华能源股份有限公司 | The measurement apparatus and measuring method of a kind of reaction heat effect |
| CN106404227A (en) * | 2016-09-22 | 2017-02-15 | 李强国 | Multifunctional isothermal calorimeter |
| CN111194400A (en) * | 2017-11-06 | 2020-05-22 | 卡尔巴科特公司 | Calorimeter and sample container for calorimeter |
| CN108426655A (en) * | 2018-05-18 | 2018-08-21 | 湘南学院 | Calorimetric reaction vessel for high-precision calorimeter |
| CN112179527A (en) * | 2019-07-04 | 2021-01-05 | 中国建筑材料科学研究总院有限公司 | Isothermal calorimetry apparatus |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140423 |