CN104655671A - Adiabatic accelerating rate calorimeter and detection method thereof - Google Patents
Adiabatic accelerating rate calorimeter and detection method thereof Download PDFInfo
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- CN104655671A CN104655671A CN201410852696.0A CN201410852696A CN104655671A CN 104655671 A CN104655671 A CN 104655671A CN 201410852696 A CN201410852696 A CN 201410852696A CN 104655671 A CN104655671 A CN 104655671A
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Abstract
The invention discloses an adiabatic accelerating rate calorimeter which comprises a furnace body forming an enclosure space, six heating devices, a reaction basket, a sample furnace, an internal gas circulating device, an external circulating gas supercharging device, a detection fixture, a cooling device and a control system. The provided adiabatic accelerating rate calorimeter has the following advantages that: the external circulating gas supercharging device and the internal gas circulating device are additionally arranged, so that the measurement environment and measurement range of the calorimeter are increased, and six heating devices and a real-time control module are arranged, so that real time heat compensation can be performed on the calorimeter. By detecting a temperature difference between an inlet and an outlet, heat release of a sample can be calculated accurately, and the calorimeter is simple to operate and convenient to use.
Description
Technical field
The invention belongs to material tests field, particularly relate to a kind of adiabatic accelerating calorimeter and detection method.
Background technology
Calorimetry instrument in accelerated speed of the prior art (referred to as: be ARC) a kind of based on the thermal analyzer of thermal insulation away from design, it is away from being adiabatic environment reaction system being placed in ARC, the operation of (H--W--S) and isothermal two kinds of patterns is searched, heat, the pressure hazard of the potential runaway reaction of analogue measurement and some chemicals of quantification and potpourri by heating--wait--.Current, ARC has become one of conventional means of testing evaluating material thermal stability in the world, and progressively to being called standard method of test future development.But this instrument has significant limitation in measurement, the outer circulation can not doing gas participation reaction as AUTO-RC reaction calorimeter can only do " milligram " level sample analysis without gradient reaction, DTA/DSC differential scanning calorimeter, can not do " gram " level sample analysis.Therefore a kind of device can tested under different magnitude, varying environment, different conditions different materials is needed.
Summary of the invention
Therefore, the invention provides and a kind ofly can carry out for different materials the device tested under different magnitude, varying environment, different conditions.
A kind of adiabatic accelerating calorimeter, comprising:
Form the body of heater of enclosure space, comprise top cover, sidewall and base;
Polylith is used for the heating arrangement heated material to be measured in described body of heater, and multiple described heating arrangement is evenly arranged on the inwall of described body of heater;
The reaction basketry reacted for making material to be measured, described reaction basketry is arranged at described furnace interior, downside;
For placing the sample heater of material to be measured, it is inner that described sample heater is suspended in described reaction basketry, and namely the side of described sample heater does not contact with described reaction basketry with bottom surface;
Interior gas-recycling plant, described interior gas-recycling plant is arranged on the upside of described furnace interior, described reaction basketry;
Outer circulation gas pressurized device, described outer circulation gas pressurized device is communicated with described body of heater and forms gas feed and gas vent;
Detect frock;
Cooling device, to be arranged on described body of heater and to form cooling water inlet and coolant outlet with described body of heater;
Control system, described control system is electrically connected with described interior gas-recycling plant, described outer circulation gas pressurized device, described heating arrangement and described detection frock.
The quantity of described heating arrangement is 6 pieces, and wherein, 2 pieces of described heating arrangements are arranged on described top cover, and 2 pieces of described heating arrangements are arranged on described sidewall, and 2 pieces of described heating arrangements are arranged on described base.
Described interior gas-recycling plant is paddle, and described paddle is provided with motor, and described paddle rotates clockwise.
Described body of heater is provided with relief valve port, proximity switch, gate interlock linkage and automatic smoke remover.
Described detection frock comprises 6 groups of temperature-detecting devices, material viscosity pick-up unit and 2 groups of flow detectors, temperature-detecting device described in 6 groups is distributed on described body of heater, described material viscosity pick-up unit is arranged in described sample heater, and flow monitoring device described in 2 groups is arranged at described gas feed and described gas outlet respectively.
Temperature-detecting device described in 3 groups is arranged on described furnace body outer wall, and temperature-detecting device described in 1 group is arranged on described inboard wall of furnace body, and temperature-detecting device described in 1 group is arranged at described relief valve port place, and described in 1 group, temperature-detecting device is for subsequent use.
Described control system comprises real-time control module, power conditioning module, flow-control module and software control module, and described software control module is electrically connected with described real-time control module, described power conditioning module and flow-control module.
Be arranged on the described outer circulation gas pressurized device in described gas feed and described gas vent and be provided with outer circulation pump and reverse checkvalve.
Described gas feed and the position of described gas vent on described body of heater are on same level line.
Utilize a method for the adiabatic accelerating calorimeter test material security according to any one of claim 1-6, comprise the steps:
S1, selection sample heater, weigh and record data;
S2, in sample heater, put into material to be measured, weigh and record data;
S3, the sample heater that material to be measured is housed is put into adiabatic accelerating calorimeter, pick-up unit impermeability;
S4, setup parameter, according to the performance of material to be measured, set initial temperature, final temperature, slope sensitivity, programming rate and the parameter of stand-by period in described control system;
S5, detect and start, start adiabatic accelerating calorimeter, and by control system adiabatic accelerating calorimeter detected and control adiabatic accelerating calorimeter inside and reach equilibrium state, even if the temperature of adiabatic accelerating calorimeter interior point, pressure are homogeneous and stable;
S6, reaction regulate, compare the heating rate of sample and the heating rate of adiabatic accelerating calorimeter, adjust the heating power of heating arrangement described in each, the temperature maintaining adiabatic accelerating calorimeter is consistent with sample temperature, enter the neither endothermic nor exothermic stage by system judgement sample, detect;
S7, record data, in the state of the equilibrium, by the concrete numerical value of control system writing time, temperature, temperature rise rate, pressure and pressure rates;
S8, data analysis, the data analysis that described software control module obtains described detection frock, and draw a diagram;
S9, end are measured, and preserve recorded and chart, cool adiabatic accelerating calorimeter by described cooling device, take out described reaction basketry and described sample heater, and cleaning leaves standstill, again to measure.
Described real-time control module can control separately heating arrangement described in each and carry out real-time heat compensation to adiabatic accelerating calorimeter.
Adiabatic accelerating calorimeter provided by the invention, tool has the following advantages:
1, install outer circulation gas pressurized device and interior gas-recycling plant additional, increase measurement environment and the measurement range of instrument;
2,6 well heaters and real-time control module are set, real-time heat compensation can be carried out to instrument.Poor by detecting out temperature, accurately calculate sample exotherms amount, simple to operate, easy to use.
Figure of description
Fig. 1 is the structural representation of adiabatic accelerating calorimeter provided by the invention;
Fig. 2 is the cut-open view of the body of heater of adiabatic accelerating calorimeter provided by the invention;
Fig. 3 is the temperature and time change curve of adiabatic accelerating calorimeter provided by the invention;
Fig. 4 is the reacting flow chart of adiabatic accelerating calorimeter provided by the invention.
Embodiment
Also the present invention is described in detail by reference to the accompanying drawings below by specific embodiment.
Adiabatic accelerating calorimeter described as shown in Figure 1 to Figure 4, comprising:
Form the body of heater 1 of enclosure space, comprise top cover 11, sidewall 12 and base 13, the volume of described body of heater 1 is preferably 1200cm
3, temperature range is 0 DEG C to 580 DEG C, pressure limit is 0bar to 180bar, controlled heating rate scope is 0 DEG C/min to 150 DEG C/min;
Polylith is used for the heating arrangement 2 heated material to be measured in described body of heater 1, and multiple described heating arrangement 2 is evenly arranged on the inwall of described body of heater 1;
The reaction basketry 3 reacted for making material to be measured, described reaction basketry 3 is arranged at described body of heater 1 inside, downside;
For placing the sample heater 4 of material to be measured, it is inner that described sample heater 4 is suspended in described reaction basketry 3, and namely the side of described sample heater 4 does not contact with described reaction basketry 3 with bottom surface, and the volume range of choices of wherein said sample heater 4 is 100cm
3to 1000cm
3, preferably 100cm
3, 200cm
3, 500cm
3and 1000cm
3;
Interior gas-recycling plant 5, described interior gas-recycling plant 5 is arranged on the upside of described body of heater 1 inside, described reaction basketry 3;
Outer circulation gas pressurized device 6, described outer circulation gas pressurized device 6 is communicated with described body of heater 1 and forms gas feed 61 and gas vent 62;
Detect frock 7;
Cooling device 8, to be arranged on described body of heater 1 and to form cooling water inlet 81 and coolant outlet 82 with described body of heater 1;
Control system, described control system is electrically connected with described interior gas-recycling plant 5, described outer circulation gas pressurized device 6, described heating arrangement 2 and described detection frock 7.
The quantity of described heating arrangement 2 is 6 pieces, and wherein, 2 pieces of described heating arrangements 2 are arranged on described top cover 11, and 2 pieces of described heating arrangements 2 are arranged on described sidewall 12, and 2 pieces of described heating arrangements 2 are arranged on described base 13.
Described interior gas-recycling plant 5 is paddle, described paddle is provided with motor 51, and described paddle rotates clockwise.
Described body of heater 1 is provided with relief valve port, proximity switch, gate interlock linkage and automatic smoke remover.
Described detection frock 7 comprises 6 groups of temperature-detecting devices 71, material viscosity pick-up unit 72 and 2 groups of flow detectors 73, temperature-detecting device 71 described in 6 groups is distributed on described body of heater 1, described material viscosity pick-up unit 72 is arranged in described sample heater 4, flow monitoring device 73 described in 2 groups is arranged at described gas feed 61 and described gas vent 62 place respectively, and the detection sensitivity of described temperature-detecting device 71 is less than 450 DEG C temperature resolutions is 0.005 DEG C.
Temperature-detecting device 71 described in 3 groups is arranged on described body of heater 1 outer wall, temperature-detecting device 71 described in 1 group is arranged on described body of heater 1 inwall, temperature-detecting device 71 described in 1 group is arranged at described relief valve port place, described in 1 group, temperature-detecting device 71 is for subsequent use, and temperature-detecting device 71 described in 6 groups measures cooling water inlet 81 place temperature, coolant outlet 82 place temperature, gas feed 61 place temperature, gas vent 62 place temperature, temperature of reaction equitemperature respectively.
Described control system comprises real-time control module, power conditioning module, flow-control module and software control module, and described software control module is electrically connected with described real-time control module, described power conditioning module and flow-control module, wherein, described control system is EuroARC program, and described software control module is KALDAS software.
Be arranged on the described outer circulation gas pressurized device 6 in described gas feed 61 and described gas vent 62 and be provided with outer circulation pump and reverse checkvalve.
Described gas feed 61 and the position of described gas vent 62 on described body of heater 1 are on same level line.
Utilize a method for adiabatic accelerating calorimeter test material as above security, comprise the steps:
S1, selection sample heater 4, weigh and record data;
S2, in sample heater 4, put into material to be measured, weigh and record data;
S3, the sample heater 4 that material to be measured is housed is put into adiabatic accelerating calorimeter, pick-up unit impermeability;
S4, setup parameter, according to the performance of material to be measured, set initial temperature, final temperature, slope sensitivity, programming rate and the parameter of stand-by period in described control system;
S5, detect and start, start adiabatic accelerating calorimeter, and by control system adiabatic accelerating calorimeter detected and control adiabatic accelerating calorimeter inside and reach equilibrium state, even if the temperature of adiabatic accelerating calorimeter interior point, pressure are homogeneous and stable;
S6, reaction regulate, the heating rate of sample and the heating rate of adiabatic accelerating calorimeter are compared, adjust the heating power of heating arrangement 2 described in each, the temperature maintaining adiabatic accelerating calorimeter is consistent with sample temperature, enter the neither endothermic nor exothermic stage by system judgement sample, detect;
S7, record data, in the state of the equilibrium, by the concrete numerical value of control system writing time, temperature, temperature rise rate, pressure and pressure rates;
S8, data analysis, the data analysis that described software control module obtains described detection frock 7, and draw a diagram;
S9, end are measured, and preserve recorded and chart, cool adiabatic accelerating calorimeter by described cooling device 8, take out described reaction basketry 3 and described sample heater 4, and cleaning leaves standstill, again to measure.
Embodiment
1, choose the sample heater 4 that a quality is M1, in sample heater 4, put into detected sample, and weighing obtains gross mass M2;
2, sample heater 4 is loaded in adiabatic accelerating calorimeter, and check the impermeability of adiabatic accelerating calorimeter;
3, close the door of adiabatic accelerating calorimeter, run EuroARC program, the parameters such as setting initial temperature, final temperature, slope sensitivity, programming rate and stand-by period, preserve Parameter File and name;
4, nominal pressure sensor original pressure is to 1bar, demarcates half range pressure to 153.15bar;
5, experiment is started, by control system adiabatic accelerating calorimeter detected and control described outer circulation pump and described heating arrangement 2 makes adiabatic accelerating calorimeter inside reach equilibrium state, even if the temperature of adiabatic accelerating calorimeter interior point, pressure are homogeneous and stable;
6, the heating rate of sample and the heating rate of adiabatic accelerating calorimeter are compared, the heating power of real-time adjustment heating arrangement 2 described in each, the temperature maintaining adiabatic accelerating calorimeter is consistent with sample temperature, enters the neither endothermic nor exothermic stage, detect by system judgement sample;
7, data are recorded, in the state of the equilibrium, by the concrete numerical value of control system writing time, temperature, temperature rise rate, pressure and pressure rates;
8, data analysis, the data analysis that described KALDAS software obtains described detection frock 7, and draw a diagram, obtain the charts such as graphics primitive data, time and maximum rate chart, thermodynamic model, time and blast chart, and made the comprehensive assessment of above-mentioned detected sample material property by chart;
9, terminate to measure, preserve recorded and chart, cool adiabatic accelerating calorimeter by described cooling device 8, discharge adiabatic accelerating calorimeter internal gas, take out described reaction basketry 3 and described sample heater 4, cleaning, leave standstill, again to measure.
Only the preferred embodiment of the present invention by the above; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (11)
1. an adiabatic accelerating calorimeter, is characterized in that, comprising:
Form the body of heater of enclosure space;
Polylith is used for the heating arrangement heated material to be measured in described body of heater, and multiple described heating arrangement is evenly arranged on the inwall of described body of heater;
The reaction basketry reacted for making material to be measured, described reaction basketry is arranged at described furnace interior, downside;
For placing the sample heater of material to be measured, it is inner that described sample heater is suspended in described reaction basketry, and namely the side of described sample heater does not contact with described reaction basketry with bottom surface;
Interior gas-recycling plant, described interior gas-recycling plant is arranged on the upside of described furnace interior, described reaction basketry;
Outer circulation gas pressurized device, described outer circulation gas pressurized device is communicated with described body of heater and forms gas feed and gas vent;
Detect frock;
Cooling device, to be arranged on described body of heater and to form cooling water inlet and coolant outlet with described body of heater;
Control system, described control system is electrically connected with described interior gas-recycling plant, described outer circulation gas pressurized device, described heating arrangement and described detection frock.
2. adiabatic accelerating calorimeter according to claim 1, it is characterized in that: the quantity of described heating arrangement is 6 pieces, wherein, 2 pieces of described heating arrangements are arranged on described top cover, 2 pieces of described heating arrangements are arranged on described sidewall, and 2 pieces of described heating arrangements are arranged on described base.
3. adiabatic accelerating calorimeter according to claim 1, is characterized in that: described interior gas-recycling plant is paddle, and described paddle is provided with motor, and described paddle rotates clockwise.
4. adiabatic accelerating calorimeter according to claim 1, is characterized in that: described body of heater is provided with relief valve port, proximity switch, gate interlock linkage and automatic smoke remover.
5. adiabatic accelerating calorimeter according to claim 4, it is characterized in that: described detection frock comprises 6 groups of temperature-detecting devices, 1 group of material viscosity pick-up unit and 2 groups of flow detectors, temperature-detecting device described in 6 groups is distributed on described body of heater, described material viscosity pick-up unit is arranged in described sample heater, and flow monitoring device described in 2 groups is arranged at described gas feed and described gas outlet respectively.
6. adiabatic accelerating calorimeter according to claim 5, it is characterized in that: temperature-detecting device described in 3 groups is arranged on described furnace body outer wall, temperature-detecting device described in 1 group is arranged on described inboard wall of furnace body, temperature-detecting device described in 1 group is arranged at described relief valve port place, and described in 1 group, temperature-detecting device is for subsequent use.
7. adiabatic accelerating calorimeter according to claim 1, it is characterized in that: described control system comprises real-time control module, power conditioning module, flow-control module and software control module, and described software control module is electrically connected with described real-time control module, described power conditioning module and flow-control module.
8. adiabatic accelerating calorimeter according to claim 1, is characterized in that: be arranged on the described outer circulation gas pressurized device in described gas feed and described gas vent and be provided with outer circulation pump and reverse checkvalve.
9. adiabatic accelerating calorimeter according to claim 7, is characterized in that: described gas feed and the position of described gas vent on described body of heater are on same level line.
10. utilize a method for the adiabatic accelerating calorimeter test material security according to any one of claim 1-8, it is characterized in that, comprise the steps:
S1, selection sample heater, weigh and record data;
S2, in sample heater, put into material to be measured, weigh and record data;
S3, the sample heater that material to be measured is housed is put into adiabatic accelerating calorimeter, pick-up unit impermeability;
S4, setup parameter, according to the performance of material to be measured, set initial temperature, final temperature, slope sensitivity, programming rate and the parameter of stand-by period in described control system;
S5, detect and start, start adiabatic accelerating calorimeter, and by control system adiabatic accelerating calorimeter detected and control adiabatic accelerating calorimeter inside and reach equilibrium state, even if the temperature of adiabatic accelerating calorimeter interior point, pressure are homogeneous and stable;
S6, reaction regulate, compare the heating rate of sample and the heating rate of adiabatic accelerating calorimeter, adjust the heating power of heating arrangement described in each, the temperature maintaining adiabatic accelerating calorimeter is consistent with sample temperature, enter the neither endothermic nor exothermic stage by system judgement sample, detect;
S7, record data, in the state of the equilibrium, by the concrete numerical value of control system writing time, temperature, temperature rise rate, pressure and pressure rates;
S8, data analysis, the data analysis that described software control module obtains described detection frock, and draw a diagram;
S9, end are measured, and preserve recorded and chart, cool adiabatic accelerating calorimeter by described cooling device, take out described reaction basketry and described sample heater, and cleaning leaves standstill, again to measure.
11. methods according to claim 9, is characterized in that: described real-time control module can control separately heating arrangement described in each and carry out real-time heat compensation to adiabatic accelerating calorimeter.
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Cited By (3)
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| CN105676765A (en) * | 2016-03-11 | 2016-06-15 | 上海应用技术学院 | Chemical engineering process security monitoring system |
| CN107064208A (en) * | 2017-02-04 | 2017-08-18 | 青岛大学 | A kind of universal calorimetric biosensor |
| CN110274929A (en) * | 2019-06-20 | 2019-09-24 | 清华大学深圳研究生院 | Accelerate calorimeter and its system |
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| CN104655671B (en) | 2017-08-25 |
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Granted publication date: 20170825 Termination date: 20191231 |