CN210774439U - Temperature difference monitoring device of reaction calorimeter - Google Patents
Temperature difference monitoring device of reaction calorimeter Download PDFInfo
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- CN210774439U CN210774439U CN201922272821.1U CN201922272821U CN210774439U CN 210774439 U CN210774439 U CN 210774439U CN 201922272821 U CN201922272821 U CN 201922272821U CN 210774439 U CN210774439 U CN 210774439U
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 82
- 238000012806 monitoring device Methods 0.000 title claims abstract description 23
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- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 8
- 238000009825 accumulation Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
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- 230000004907 flux Effects 0.000 description 2
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- 238000004519 manufacturing process Methods 0.000 description 2
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- 230000003321 amplification Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000007707 calorimetry Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
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Abstract
The utility model discloses a temperature difference monitoring device of a reaction calorimeter, which comprises an end cover, a reaction vessel, a jacket and a temperature difference monitoring device, wherein the jacket is sleeved outside the reaction vessel, the temperature difference monitoring device is used for measuring the temperature difference between the inside of the reaction vessel and the jacket in real time, the temperature difference monitoring device comprises a temperature measuring element, a potential difference measuring device and a controller, wherein the temperature measuring element comprises two paths of thermocouples with the same type, an end cover is provided with a through hole for the temperature difference monitoring device to measure the internal temperature of the reaction container, the end cover is combined and sealed at the top of the reaction container, a cavity filled with a heat-conducting medium is arranged in the end cover, the end cover is provided with an inlet and an outlet which are communicated with the cavity, the end cover and the end cover are connected through the outside to form a loop, the loop is provided with a temperature control circulator for adjusting the temperature of the heat-conducting medium, guide plates are uniformly distributed; the utility model discloses can catch the inside heat signal that presss from both sides the cover and produce of reaction vessel fast, and then acquire the inside difference in temperature change of reaction vessel fast, improve accuracy, environmental suitability and the stability of reaction calorimeter measuring result.
Description
Technical Field
The utility model relates to a reaction process heat survey field, concretely relates to temperature difference monitoring devices of reaction calorimeter.
Background
For a long time, the reaction calorimeter is used as an ideal tool for analyzing chemical reaction, and has wide application in the fields of chemical thermal risk assessment, process safety, process amplification and the like. As a first-choice instrument for reaction process thermal risk research, a reaction calorimeter obtains relevant thermal safety parameters in a reaction process by measuring data such as temperature, pressure, heat flow and the like in a chemical reaction in real time, so that process development and safety production are effectively guided, and matched protective measures are well taken.
The reaction calorimeter mainly measures the heat change in the reaction process, and according to the input heat, i.e. heat accumulation + output heat, the main calorimetric equation in the calorimeter can be represented by the following formula:
(Qr+Qc+Qstir)=Qacc+(Qflow+Qloss+Qdos+Qreflux) (1)
wherein Q isrFor rate of heat of reaction, QcFor calibrating the heater heat flux, QstirTaking off the rate of the heat flow for stirring, QaIs the rate of heat build-up of the reaction system, QiRate of heat accumulation outside the reaction system, QflowIs the rate of heat flux, Q, from the reaction system to the jacketlossThe heat dissipation rate, Q, of the upper part of the reactor and the subsequent part of the apparatus, etc. is outwarddosHeat absorbed for charging, QrefluxThe rate of heat removed for the reflux.
Neglecting the heat lost due to stirring and reflux, the equation can be rewritten as:
Qr=Qacc+Qflow+Qloss+Qdos(2)
wherein,
Qacc=Qa+Qi(3)
Qdos=dmdos/dt*Cpdos*(Tr—Tdos) (4)
the principle of the reaction calorimeter for measurement is that a constant temperature unit is used for quickly adjusting the temperature to control Tr, and the measurement formula is as follows:
Qflow=UA*(Tr—Tj) (5)
wherein Q isflowRefers to the heat flow rate (W) from the reaction system to the jacket. U, A are heat transfer coefficients (W m)-2k-1) And heat transfer area (m)2)。
At present, the reaction calorimeter monitors the temperature (T) of the system in the reaction vessel by temperature sensors respectivelyr) Temperature (T) of jacketj) Then, the difference is calculated according to the formula (1) by calorimetric calculation.
In the prior art, the potential difference measurement mode needs a plurality of probes to measure the temperature and completes the temperature subtraction, which is easy to cause error accumulation. In order to reduce the error in the measurement process, the currently adopted technology is to select a temperature sensor with higher precision so as to reduce the measurement error. However, the technology has extremely high requirements on the manufacturing process and design of the sensor, is difficult to widely obtain and apply, and cannot substantially reduce the problem of error accumulation existing in multiple times of measurement of measuring equipment.
To the inaccurate problem of current commercialized reaction calorimeter calorimetric, the utility model discloses the people relies on many years of industry experience to improve to the end cover structure of reaction calorimeter.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a reaction calorimeter's difference in temperature monitoring devices solves the problem of the accumulated measuring error that the difference leads to is sought again to the temperature of measuring two places respectively earlier among the prior art, improves calorimetric accuracy, environment suitability and stability.
In order to achieve the above object, the technical solution of the present invention is as follows:
the temperature difference monitoring device comprises a temperature measuring element, a potential difference measuring device and a controller, wherein the temperature measuring element comprises two paths of thermocouples with the same model, one path of thermocouple is arranged in a reaction container, the other path of thermocouple is arranged in a jacket, the two paths of thermocouples are connected in series in a reverse direction, the temperature measuring element is connected with the potential difference measuring device, the potential difference measuring device measures the potential difference of the two paths of thermocouples, the potential difference measuring device is connected with the controller, and the controller receives a potential difference signal transmitted by the potential difference measuring device.
The thermocouples are all provided with compensation leads.
The reaction calorimeter also comprises an end cover, the end cover is combined and sealed at the top of the reaction container, the end cover is provided with a through hole, and one path of thermocouple is placed into the reaction container from the through hole.
The jacket is filled with a heat-conducting medium.
The clamp sleeve is provided with an oil inlet and an oil outlet, and the other path of thermocouple is arranged at the oil inlet or the oil outlet of the clamp sleeve.
The reaction calorimeter also comprises a stirrer and a heater which are arranged in the reaction container.
After the scheme is adopted, the utility model discloses a thermocouple has the characteristics that heat capacity and thermal inertia are little, dynamic response is fast, can catch the heat signal that reaction vessel inside and clamp cover produced, and then acquires the inside difference in temperature change of reaction vessel fast for calorimetric is more accurate, and the result is more stable.
Drawings
Fig. 1 is a schematic diagram of the thermocouple reverse series connection potential difference measurement of the present invention.
Fig. 2 is the schematic diagram of the temperature compensation of the end cover of the present invention.
Fig. 3 is a front view of the end cap of the present invention.
Fig. 4 is a top view of the end cap of the present invention.
Wherein Q iscIndicating the heat quantity of the heater, ErRepresents the internal potential of the reaction vessel, EfDenotes the potential of the jacket, QflowIndicating the heat transfer between the jacket and the reaction calorimeter.
Description of reference numerals:
the device comprises an end cover 1, a through hole 11, an inlet 12, an outlet 13, a reaction container 2, a jacket 3, an oil inlet 31, an oil outlet 32, a temperature difference monitoring device 4, a temperature measuring element 41, thermocouples 411 and 412, a potential difference measuring device 42, a controller 43, a stirrer 5 and a heater 6.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without inventive labor, please refer to fig. 1 to 4.
A temperature difference monitoring device 4 of a reaction calorimeter comprises an end cover 1, a reaction vessel 2, a jacket 3, a stirrer 5 and a heater 6, wherein the jacket 3 is sleeved outside the reaction vessel 2, specifically, the jacket 3 is provided with an oil inlet 31 and an oil outlet 32 for heat-conducting media to flow into and out of the jacket 3, so that the jacket 3 can exchange heat with the reaction vessel 2.
The temperature difference monitoring device 4 is used for measuring the temperature difference between the inside of the reaction vessel 2 and the jacket 3 in real time, the end cover 1 is provided with a through hole 11, the through hole 11 is used for the temperature difference monitoring device 4 to measure the temperature inside the reaction vessel 2, and the end cover 1 covers and seals the top of the reaction vessel 2.
The temperature difference monitoring device 4 comprises a temperature measuring element 41, a potential difference measuring device 42 and a controller 43, wherein the temperature measuring element 41 is connected with the potential difference measuring device 42, the potential difference measuring device 42 is used for measuring the potential difference between two ends of the temperature measuring element 41, one end of the temperature measuring element 41 is arranged in the reaction vessel 2 from the through hole 11, the other end of the temperature measuring element 41 is arranged in the jacket 3, and the potential difference measuring device 42 is connected with the controller 43 and transmits a potential difference signal to the controller 43.
The temperature measuring element 41 comprises two thermocouples 411 and 412 with the same model, as shown in fig. 1 and fig. 2, one thermocouple 411 is placed into the reaction material of the reaction container 2 from the through hole 11, the other thermocouple 412 is placed at the oil inlet 31 or the oil outlet 32 of the jacket 3, the two thermocouples 411 and 412 are connected in series in reverse direction, are all provided with compensation wires and are calibrated, the potential difference of the two thermocouples 411 and 412 is obtained through the high-precision potential difference measuring device 42, and the temperature difference between the inside of the reaction container 2 and the jacket 3 is directly obtained by utilizing the corresponding relation between the potential difference and the temperature difference;recording the temperature difference change in real time in the reaction process until the reaction is finished; according to calorimetric equation Qfiow=UA·(Tr-Tj) And carrying out chemical reaction calorimetry to calculate the reaction exotherm. The utility model discloses a thermocouple has the characteristics that heat capacity and thermal inertia are little, dynamic response is fast, can catch the heat signal that the reaction produced rapidly, and the potential difference is got in the direct survey. The temperature difference monitoring device 4 solves the problem of accumulated measurement errors caused by respectively measuring the temperatures at two positions and then calculating the difference in the prior art.
Therefore the utility model discloses be applied to the experiment that reaction temperature has the change in the reaction process, also can realize the quick tracking of end cover 1 department temperature with the same reason, the port is equipped with import 12 and export 13, as long as will place the thermocouple of pressing from both sides the cover and change into place import 12 or export 13 at the end cover can, as shown in fig. 2.
The reaction calorimeter is suitable for reaction in a reaction process under a condition that no obvious gas escapes, and the through hole 11, each inlet, each outlet, each oil inlet and each oil outlet are subjected to sealing treatment, so that the reaction calorimeter is ensured to have good air tightness.
In one embodiment, as shown in fig. 3 and 4, the end cap 1 is circular, and has through holes 11 corresponding to the stirrer 5 for inserting the stirrer 5 and the heater 6, the stirrer 5 is used to accelerate the reaction speed and make the reaction more uniform, and the heater 6 is used to heat the temperature inside the reaction vessel 2.
The basic principles and main features of the invention and the advantages of the invention have been shown and described above. It will be understood by those skilled in the art that the present invention is not limited to the above embodiments, and that the foregoing embodiments and descriptions are provided only to illustrate the principles of the present invention without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The utility model provides a temperature difference monitoring devices of reaction calorimeter, this reaction calorimeter includes reaction vessel and jacket, the jacket cup joints outside reaction vessel, its characterized in that: the temperature difference monitoring device comprises a temperature measuring element, a potential difference measuring device and a controller, wherein the temperature measuring element comprises two paths of thermocouples with the same model, one path of thermocouple is arranged in the reaction container, the other path of thermocouple is arranged in a jacket, the two paths of thermocouples are connected in series in a reverse direction, the temperature measuring element is connected with the potential difference measuring device, the potential difference measuring device measures the potential difference of the two paths of thermocouples, the potential difference measuring device is connected with the controller, and the controller receives a potential difference signal transmitted by the potential difference measuring device.
2. The temperature difference monitoring device for the reaction calorimeter of claim 1, wherein: the thermocouples are all provided with compensation leads.
3. The temperature difference monitoring device for the reaction calorimeter of claim 1, wherein: the reaction calorimeter also comprises an end cover, the end cover is combined and sealed at the top of the reaction container, the end cover is provided with a through hole, and one path of thermocouple is placed into the reaction container from the through hole.
4. The temperature difference monitoring device for the reaction calorimeter of claim 1, wherein: the jacket is filled with a heat-conducting medium.
5. The temperature difference monitoring device for the reaction calorimeter of claim 1, wherein: the clamp sleeve is provided with an oil inlet and an oil outlet, and the other path of thermocouple is arranged at the oil inlet or the oil outlet of the clamp sleeve.
6. The temperature difference monitoring device for the reaction calorimeter of claim 1, wherein: the reaction calorimeter also comprises a stirrer and a heater which are arranged in the reaction container.
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CN201922272821.1U CN210774439U (en) | 2019-12-17 | 2019-12-17 | Temperature difference monitoring device of reaction calorimeter |
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CN201922272821.1U CN210774439U (en) | 2019-12-17 | 2019-12-17 | Temperature difference monitoring device of reaction calorimeter |
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