CN216410454U - Gas production rate measuring device of reaction calorimeter - Google Patents
Gas production rate measuring device of reaction calorimeter Download PDFInfo
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- CN216410454U CN216410454U CN202122494013.7U CN202122494013U CN216410454U CN 216410454 U CN216410454 U CN 216410454U CN 202122494013 U CN202122494013 U CN 202122494013U CN 216410454 U CN216410454 U CN 216410454U
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Abstract
The utility model discloses a gas production rate measuring device of a reaction calorimeter, which comprises a temperature cycle controller, a U-shaped pipe, a first switch valve and a second switch valve, wherein the temperature cycle controller is arranged on the reaction calorimeter and comprises a temperature measuring device arranged in the reaction calorimeter and a temperature control device arranged on the U-shaped pipe, the U-shaped pipe comprises a right branch pipe and a left branch pipe which are mutually communicated, indicating liquid is injected into the U-shaped pipe to form a liquid seal between the right branch pipe and the left branch pipe, the right branch pipe is communicated with the outside, the left branch pipe is provided with a gas inlet and a gas outlet, the gas inlet is communicated with the reaction calorimeter, the gas outlet is communicated with the outside, the first switch valve is arranged on the gas inlet, the second switch valve is arranged on the gas outlet, and the gas inlet and the gas outlet are opened or closed by the first switch valve and the second switch valve. The utility model can synchronously carry out reaction gas production measurement and reaction heat measurement and monitor in real time, and the measurement process is more convenient.
Description
Technical Field
The utility model relates to the technical field of gas production rate measuring devices, in particular to a gas production rate measuring device of a reaction calorimeter.
Background
A reaction calorimeter is a tool used to measure the exothermic or endothermic heat of a chemical or physical reaction during the development of chemicals and pharmaceuticals.
The method is characterized in that the method is used for measuring the gas production volume and the gas production rate in the reaction process through U-shaped tube liquid drainage, but the method is usually carried out after the reaction volume is hot, the device is in a sealed state in the reaction process, the pressure change in the device is large, and the deviation of the experiment and the measurement result is easily caused; therefore, the accuracy of the measurement result obtained by the method is not high, the gas production rate cannot be monitored in real time, and when the gas production rate is excessive in the reaction process, a larger-size U-shaped pipe (measuring device) is needed for accommodating more gas, so that inconvenience is brought to the measurement process.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a gas production rate measuring device of a reaction calorimeter, which overcomes the defects, realizes synchronous reaction gas production measurement and reaction calorimetry and real-time monitoring, and is more convenient and faster in the measuring process.
In order to achieve the above purpose, the solution of the utility model is: the temperature cycle controller comprises a temperature measuring device arranged in the reaction calorimeter and a temperature control device arranged on the U-shaped tube, the U-shaped tube comprises a right branch tube and a left branch tube which are mutually communicated, indicating liquid is injected into the U-shaped tube to form liquid seal between the right branch tube and the left branch tube, the right branch tube is communicated with the outside, the left branch tube is provided with an air inlet and an air outlet, the air inlet is communicated with the reaction calorimeter, the air outlet is communicated with the outside, the first switch valve is arranged on the air inlet, the second switch valve is arranged on the air outlet, and the first switch valve and the second switch valve are opened or closed.
Further, a pressure sensor is arranged in the left branch pipe.
Further, the second switch valve is connected with a counter to record the number of times the second switch valve is opened.
Furthermore, an indicating liquid discharge port is communicated below the U-shaped pipe, a liquid discharge valve is arranged on the indicating liquid discharge port, and the liquid discharge valve is opened or closed to block the indicating liquid in the U-shaped pipe or discharge the indicating liquid along the indicating liquid discharge port.
Further, the temperature control device comprises a heat exchange tube, a temperature control box and a heat conducting medium, the heat exchange tube is wound on the periphery of the U-shaped tube, two ends of the heat exchange tube are communicated with the temperature control box, the heat conducting medium circularly flows between the heat exchange tube and the temperature control box, and the temperature control box heats or cools the heat conducting medium.
Further, the U-shaped pipe is made of glass.
Furthermore, the pipe wall of the left branch pipe is provided with a scale value.
Further, the U-shaped pipe is wrapped with a heat insulation layer.
Further, the inner cavity of the left branch pipe is cylindrical.
Further, the indicating liquid is silicone oil.
After the scheme is adopted, the utility model has the beneficial effects that:
(1) the temperature circulation controller comprises a temperature measuring device arranged in the reaction calorimeter and a temperature control device arranged on the U-shaped pipe, wherein the temperature measuring device measures the temperature in the reaction calorimeter in the reaction process, and the temperature control device heats the U-shaped pipe and the indicating liquid to be equal to the internal temperature of the temperature control device, so that high-temperature gas generated by reaction in the measurement process is prevented from entering the U-shaped pipe and then being liquefied by cooling, and the measurement process is more accurate;
(2) the U-shaped pipe comprises a right branch pipe and a left branch pipe which are communicated with each other, indicating liquid is injected into the U-shaped pipe so as to form a liquid seal between the right branch pipe and the left branch pipe, the right branch pipe is communicated with the outside, the left branch pipe is provided with an air inlet and an air outlet, the air inlet is communicated with a reaction calorimeter, the air outlet is communicated with the outside, a first switch valve is arranged on the air inlet, a second switch valve is arranged on the air outlet, the first switch valve and the second switch valve are opened or closed, the first switch valve is opened, the second switch valve is closed, gas generated by reaction enters the left branch pipe, when the height difference between the liquid levels in the left branch pipe and the right branch pipe reaches a preset difference value, the first switch valve is closed, the second quick switch valve is opened after delaying, and the quantity of substances discharged from the left branch pipe can be calculated by applying a liquid discharge method and an ideal gas state equation, then closing the second switch valve, delaying to open the first switch valve, continuously introducing the gas generated in the reaction calorimeter into the left branch pipe, repeating the process until the reaction is finished, accumulating the amount of the substances discharging the gas after each second switch valve is opened to obtain the total amount of the substances generating the gas in the reaction, and obtaining the gas production rate in the reaction by the time of the reaction; because the gas that measurement was accomplished in the measurement process can directly be discharged, need not store in the U-shaped pipe all the time, so the U-shaped pipe can set up littleer volume, makes the measurement process more convenient.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Description of reference numerals: 1-a reaction calorimeter, 2-a U-shaped pipe, 3-a first switch valve, 4-a second switch valve, 5-a pressure sensor, 6-an upper computer, 7-a temperature cycle controller, 8-a right branch pipe, 9-a left branch pipe, 10-indicating liquid, 11-an air inlet, 12-an air outlet, 13-a temperature measuring device, 14-a temperature control device, 16-a heat insulation layer, 17-an indicating liquid discharge outlet, 18-a liquid discharge valve, 19-a heat exchange pipe and 20-a temperature control box.
Detailed Description
The utility model is described in detail below with reference to the accompanying drawings and specific embodiments.
The utility model provides a gas production rate measuring device of a reaction calorimeter, as shown in fig. 1, comprising a temperature cycle controller 7, a U-shaped tube 2, a first switch valve 3, a second switch valve 4, preferably, for realizing automatic control, a pressure sensor 5, and an upper computer 6, wherein the first fast switch valve 3 and the second switch valve 4 are electromagnetic valves, and the upper computer 6 is not required to be arranged, the first switch valve 3 and the second switch valve 4 are set as manual control valves, without specific limitation, the specific structure of the reaction calorimeter 1 and the principle of the reaction calorimeter 1 for measuring reaction heat are the prior art, in this embodiment, the U-shaped tube 2 is preferably made of glass material, and the U-shaped tube 2 is wrapped with a heat insulating layer 16, and the heat insulating layer 16 can be any one of the prior materials or structures with heat insulating effect, the U-shaped pipe 2 comprises a right branch pipe 8 and a left branch pipe 9 which are communicated with each other, the right branch pipe 8 and the left branch pipe 9 are both vertically arranged, the inner cavity of the left branch pipe 9 is preferably arranged to be cylindrical for facilitating subsequent calculation, an indicating liquid 10 is injected into the U-shaped pipe so as to form a liquid seal between the right branch pipe 8 and the left branch pipe 9, the indicating liquid 10 is a liquid which has low reaction activity with generated gas components and low solubility, preferably, the indicating liquid 10 is made of silicone oil, the material of the indicating liquid 10 is specifically selected according to the type of the generated gas without specific limitation, an indicating liquid discharge port 17 is formed in the lower part of the U-shaped pipe 2, a liquid discharge valve 18 is arranged on the indicating liquid discharge port 17, the liquid discharge valve 18 is opened or closed so as to block the indicating liquid 10 in the U-shaped pipe 2 or discharge along the indicating liquid discharge port 17, and further replace the indicating liquid 10 in the U-shaped pipe 2, the indicating liquid discharge port 17 can also be used for adjusting the liquid level of indicating liquid 10 in the U-shaped tube 2, the right branch tube 8 is communicated with the outside, the left branch tube 9 is opened with an air inlet 11 and an air outlet 12, the air inlet 11 is communicated with the reaction calorimeter 1, the air outlet 12 is communicated with the outside, the first switch valve 3 is arranged on the air inlet 11, the second switch valve 4 is arranged on the air outlet 12, the second switch valve 4 is further connected with a counter, in the embodiment, the counter is integrated on the upper computer 6, the counter is cleared before each measurement is started, the counter records the opening times of the second switch valve 4 in each reaction measurement process, the pressure sensor 5 is arranged in the left branch tube 9, the upper computer 6 is connected with the first switch valve 3, the second switch valve 4 and the pressure sensor 5, the pressure sensor 5 detects the air pressure in the left branch tube 9, the detected air pressure value is transmitted to the upper computer 6 to control the first switch valve 3 and the second switch valve 4 to open or close the air inlet 11 and the air outlet 12, the temperature circulation controller 7 comprises a temperature measuring device 13 arranged in the reaction calorimeter 1 and a temperature control device 14 arranged on a U-shaped tube, the temperature control device 14 comprises a heat exchange tube 19, a temperature control box 20 and a heat conducting medium, the heat exchange tube 19 is wound on the periphery of the U-shaped tube 2, two ends of the heat exchange tube 19 are communicated with the temperature control box 20, the heat conducting medium circularly flows between the heat exchange tube 19 and the temperature control box 20, and the temperature control box 20 heats or cools the heat conducting medium;
the process of measuring the reaction gas production rate by using the device and the further concrete structure in the embodiment are as follows:
step 1: before the reaction starts, the upper computer 6 controls the first switch valve 3 to open the air inlet 11, and controls the second switch valve 4 to close the air outlet 12 to conduct the left branch pipe 9 and the reaction calorimeter 1;
step 2: when the reaction of the reactant to be measured in the reaction calorimeter 1 starts, the temperature measuring device 13 continuously measures the temperature in the reaction calorimeter 1, and the temperature of the U-shaped tube 2 is adjusted in real time through the temperature control device 14, so that the temperature of the U-shaped tube 2 is kept equal to the temperature in the reaction calorimeter 1, and therefore the phenomenon that the high-temperature gas generated by the reaction in the reaction calorimeter 1 enters the left branch tube 9 and is precooled to be liquefied, and the accuracy of the subsequent gas production volume measurement is influenced is prevented;
and step 3: gas generated by reaction of reactants to be tested in the reaction calorimeter 1 is discharged into the left branch pipe 9 along the gas inlet 11, the pressure sensor 5 measures the gas pressure in the left branch pipe 9 to obtain a gas pressure change value in the left branch pipe 9, preferably, the upper computer 6 displays the gas pressure in the left branch pipe 9 in real time, simultaneously, the indicating liquid 10 liquid level height change in the left branch pipe 9 is measured to obtain a gas volume change value in the left branch pipe 9, preferably, scale values can be arranged on the pipe walls of the left branch pipe 9 and the right branch pipe 8, the U-shaped pipe 2 is made of transparent glass, the heat preservation layer 16 is provided with an observation window at a corresponding position, the scale value on the pipe wall of the left branch pipe 9 is used for observing the change value of the liquid level of the indicating liquid 10 in the left branch pipe 9, and then the gas volume change value in the left branch pipe 9 is calculated, or a liquid level meter is arranged in the left branch pipe 9 (the liquid level meter can be any one of the existing liquid level meters, not given in the attached drawing), with the level gauge with host computer 6 is connected, shows in real time on host computer 6 the 10 liquid levels of indicator liquid in the left branch pipe 9, the 9 inner chambers of left branch pipe are cylindrical, and then pass through the height change of the 10 liquid levels of indicator liquid in the left branch pipe 9 reachs the gas volume change value in the left branch pipe 9 is:
wherein d is1Is the diameter of the inner cavity of the left branch pipe 9, R2Is the initial height, R, of the liquid level of the indicating liquid 10 in the left branch pipe 91The actual liquid level height of the indicating liquid 10 in the left branch pipe 9 is the current actual liquid level height; when the air pressure in the left branch pipe 9 reaches a preset value, the pressure sensor 5 controls the second switch valve 4 to close the air inlet 11 and then controls the second switch valve 4 to open the air outlet 12 through the upper computer 6, in the embodiment, a trigger module is arranged on the upper computer 6, the trigger module can be a software program or corresponding hardware equipment, which are the prior art, no specific explanation is provided in the implementation, the pressure sensor 5 transmits the pressure value measured by the pressure sensor to the trigger module, a preset value is arranged on the trigger module, when the pressure value measured by the pressure sensor 5 is equal to the preset value, the upper computer 6 controls the second switch valve 4 to close the air inlet 11, in order to prevent the air inlet 11 and the air outlet 12 from being opened simultaneously, so that the reaction calorimeter 1 is directly communicated with the outside, and the gas which is not measured directly flows out from the outside, the upper computer 6 is provided with a time delay module to delay the opening of the exhaust port 12 from the closing of the air inlet 11, and the amount of substances of single exhaust gas is calculated through an ideal gas state equation:
wherein, P1Controlling the pressure at which the second switching valve 4 opens for the pressure sensor 5Preset value, P0Is the initial air pressure in the left branch, P0The pressure may be atmospheric pressure or a set pressure value, in this embodiment, the atmospheric pressure, R is an ideal gas coefficient, and T is the temperature measured by the temperature measuring device 13;
and 4, step 4: when the pressure sensor 5 detects that the air pressure in the left branch pipe 9 is restored to the initial value, the second switch valve 4 is controlled by the upper computer 6 to close the exhaust port 12, then the first switch valve 3 is controlled to open the air inlet 11, the opening of the air inlet 11 is delayed from the closing of the exhaust port 12, and the unmeasured air is prevented from directly flowing out of the outside;
and 5: repeating the step 3 and the step 4 until the reaction of the reactant to be detected in the reaction calorimeter 1 is terminated, accumulating the amount of the substance of the exhaust gas when the exhaust port 12 is opened each time to obtain the total amount of the substance of the exhaust gas, and after the reaction of the reactant to be detected is terminated, obtaining the total amount of the substance of the exhaust gas by the product of the amount of the substance of the exhaust gas obtained in the step 3 for one time and the opening times of the second switch valve 4 recorded by the counter as follows:
wherein, X is the number of times of opening the second switch valve 4 recorded by the counter, the gas production rate is obtained through the total substance amount and the reaction proceeding time of the reactant, the reaction proceeding time is displayed by the upper computer 6, the calculation process can also adopt the automatic calculation of the upper computer 6 to directly obtain the gas production rate measurement result, which is a conventional technical means, and the explanation is not provided in the embodiment.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the design of the present invention, and all equivalent changes made in the design key point of the present invention fall within the protection scope of the present invention.
Claims (10)
1. A gas production rate measuring device of a reaction calorimeter is characterized in that: including installing temperature cycle controller (7), U-shaped pipe (2), first ooff valve (3), second ooff valve (4) on reaction calorimeter (1), temperature cycle controller (7) is including setting up temperature measuring device (13) in reaction calorimeter (1), temperature regulating device (14) of setting on the U-shaped pipe, U-shaped pipe (2) are including right branch pipe (8) and left branch pipe (9) that switch on each other, the intraductal injection of U has instruction liquid (10), so that form the liquid seal between right branch pipe (8) and left branch pipe (9), right branch pipe (8) switch on the external world, it has air inlet (11), gas vent (12) to open on left branch pipe (9), air inlet (11) switch on reaction calorimeter (1), gas vent (12) switch on the external world, first ooff valve (3) set up on air inlet (11), the second switch valve (4) is arranged on the exhaust port (12), and the first switch valve (3) and the second switch valve (4) open or close the air inlet (11) and the exhaust port (12).
2. The gas generation rate measuring apparatus of a reaction calorimeter of claim 1, wherein: and a pressure sensor (5) is arranged in the left branch pipe (9).
3. The gas generation rate measuring apparatus of a reaction calorimeter of claim 1, wherein: the second switch valve (4) is connected with a counter to record the opening times of the second switch valve (4).
4. The gas generation rate measuring apparatus of a reaction calorimeter of claim 1, wherein: an indicating liquid discharge port (17) is communicated below the U-shaped pipe (2), a liquid discharge valve (18) is arranged on the indicating liquid discharge port (17), and the liquid discharge valve (18) is opened or closed to block the indicating liquid (10) in the U-shaped pipe (2) or discharge the indicating liquid along the indicating liquid discharge port (17).
5. The gas generation rate measuring apparatus of a reaction calorimeter of claim 1, wherein: temperature regulating device (14) include heat exchange pipe (19), accuse temperature case (20), heat-conducting medium, heat exchange pipe (19) are convoluteed U-shaped pipe (2) periphery, heat exchange pipe (19) both ends are switched on accuse temperature case (20), heat-conducting medium circulation flow in heat exchange pipe (19) with between accuse temperature case (20), accuse temperature case (20) heating or cooling heat-conducting medium.
6. The gas generation rate measuring apparatus of a reaction calorimeter of claim 1, wherein: the U-shaped pipe (2) is made of glass.
7. The apparatus for measuring a gas generation rate of a reaction calorimeter of claim 6, wherein: and the pipe wall of the left branch pipe (9) is provided with scale values.
8. The gas generation rate measuring apparatus of a reaction calorimeter of claim 1, wherein: the U-shaped pipe is wrapped by a heat-insulating layer (16).
9. The gas generation rate measuring apparatus of a reaction calorimeter of claim 1, wherein: the inner cavity of the left branch pipe (9) is cylindrical.
10. The gas generation rate measuring apparatus of a reaction calorimeter of claim 1, wherein: the indicating liquid (10) is silicone oil.
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| CN202122494013.7U CN216410454U (en) | 2021-10-15 | 2021-10-15 | Gas production rate measuring device of reaction calorimeter |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113945484A (en) * | 2021-10-15 | 2022-01-18 | 厦门标安科技有限公司 | Gas production rate measuring device of reaction calorimeter |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113945484A (en) * | 2021-10-15 | 2022-01-18 | 厦门标安科技有限公司 | Gas production rate measuring device of reaction calorimeter |
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