CN104655671B - Adiabatic accelerating calorimeter and detection method - Google Patents
Adiabatic accelerating calorimeter and detection method Download PDFInfo
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- CN104655671B CN104655671B CN201410852696.0A CN201410852696A CN104655671B CN 104655671 B CN104655671 B CN 104655671B CN 201410852696 A CN201410852696 A CN 201410852696A CN 104655671 B CN104655671 B CN 104655671B
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Abstract
A kind of adiabatic accelerating calorimeter, including：Form the body of heater of closing space；Heater；React basketry；Sample heater；Interior gas-recycling plant；Outer circulation gas pressurized device；Detecting tool；Cooling device；Control system.The adiabatic accelerating calorimeter that the present invention is provided, has the following advantages that：Install outer circulation gas pressurized device and interior gas-recycling plant additional, increase the measuring environment and measurement range of instrument；6 heaters and real-time control module are set, real-time heat compensation can be carried out to instrument.By detecting that out temperature is poor, sample exotherms amount is accurately calculated, it is simple to operate, it is easy to use.
Description
Technical field
The invention belongs to material tests field, more particularly to a kind of adiabatic accelerating calorimeter and detection method.
Background technology
Calorimetry instrument in accelerated speed of the prior art is (referred to as：ARC) it is a kind of heat analysis based on adiabatic remote design
Instrument, it searches (H--W--S) and isothermal away from being that reaction system is placed in ARC adiabatic environment by heating -- wait --
The operation of both of which, the potential runaway reaction of analogue measurement and heat, the pressure hazard for quantifying some chemicals and mixture.When
Before, ARC has become evaluates one of conventional means of testing of material heat endurance in the world, and progressively to referred to as standard testing side
Method direction is developed.But the instrument has significant limitation in terms of measurement, such as AUTO-RC reaction calorimeters can not do gas
" milligram " level sample analysis can only be done without gradient reaction, DTA/DSC differential scanning calorimeters by participating in the outer circulation of reaction, it is impossible to be done
" gram " level sample analysis.Therefore one kind is needed to be surveyed to different materials under different magnitudes, varying environment, different conditions
The device of examination.
The content of the invention
Therefore, the present invention provides one kind and can carried out for different materials under different magnitudes, varying environment, different conditions
The device of test.
A kind of adiabatic accelerating calorimeter, including：
Form the body of heater of closing space, including top cover, side wall and base；
Polylith is used for the heater heated to material to be measured in the body of heater, and multiple heaters are uniform
On the inwall for being arranged at the body of heater；
For the reaction basketry for making material to be measured react, the reaction basketry be arranged at the furnace interior, under
Side；
Sample heater for placing material to be measured, the sample heater is suspended in inside the reaction basketry, i.e., described sample
The side and bottom surface of product stove are not contacted with the reaction basketry；
Interior gas-recycling plant, the interior gas-recycling plant is arranged at the furnace interior, reaction basketry upside；
Outer circulation gas pressurized device, the outer circulation gas pressurized device connects with the body of heater and forms gas feed
And gas vent；
Detecting tool；
Cooling device, is arranged on the body of heater and forms cooling water inlet and coolant outlet with the body of heater；
Control system, it is the control system and the interior gas-recycling plant, the outer circulation gas pressurized device, described
Heater and detecting tool electrical connection.
The quantity of the heater is 6 pieces, wherein, 2 pieces of heaters are arranged on the top cover, described in 2 pieces
Heater is arranged on the side wall, and 2 pieces of heaters are arranged on the base.
The interior gas-recycling plant is agitating paddle, is provided with motor on the agitating paddle, and the agitating paddle is along up time
Pin rotates.
Relief valve port, proximity switch, couplet on the door lock linkage device and automatic smoke remover are provided with the body of heater.
The detecting tool includes 6 groups of temperature-detecting devices, material viscosity detection means and 2 groups of flow detectors, 6 groups
The temperature-detecting device is distributed on the body of heater, and the material viscosity detection means is arranged in the sample heater, 2 groups of institutes
State flow monitoring device and be respectively arranged at the gas feed and the gas outlet.
Temperature-detecting device described in 3 groups is arranged on the furnace body outer wall, and temperature-detecting device described in 1 group is arranged at described
On inboard wall of furnace body, temperature-detecting device described in 1 group is arranged at the relief valve port, and temperature-detecting device described in 1 group is standby.
The control system includes real-time control module, power conditioning module, flow-control module and software control module,
And the software control module is electrically connected with the real-time control module, the power conditioning module and flow-control module.
It is arranged on the outer circulation gas pressurized device in the gas feed and the gas vent outside being provided with
Circulating pump and non-return valve.
The position of the gas feed and the gas vent on the body of heater is in same horizontal line.
A kind of adiabatic accelerating calorimeter using as any one of claim 1-6 detects the side of material safety
Method, comprises the following steps：
S1, selection sample heater, weigh and record data；
S2, material to be measured is put into sample heater, weighed and record data；
S3, the sample heater that will be equipped with material to be measured are put into adiabatic accelerating calorimeter, detection means air-tightness；
S4, setup parameter, according to the performance of material to be measured, set initial temperature, termination in the control system
Temperature, slope sensitivity, programming rate and the parameter of stand-by period；
S5, detection start, and start adiabatic accelerating calorimeter, and adiabatic accelerating calorimeter is detected by control system
And control to reach poised state inside adiabatic accelerating calorimeter, even if the temperature of adiabatic accelerating calorimeter interior point, pressure are equal
One and stably；
S6, reaction regulation, the heating rate of heating rate and adiabatic accelerating calorimeter to sample are compared, and adjustment is every
The heating power of heater described in one, maintains the temperature of adiabatic accelerating calorimeter consistent with sample temperature, is judged by system
Sample enters the neither endothermic nor exothermic stage, is detected；
S7, record data, in the state of the equilibrium, time, temperature, temperature rise rate, pressure and pressure are recorded by control system
The concrete numerical value of power speed；
S8, data analysis, the software control module are analyzed the data obtained by the detecting tool, and are drawn
Chart；
S9, end measurement, preserve recorded and chart, and adiabatic accelerating calorimeter is cooled down by the cooling device,
The reaction basketry and the sample heater are taken out, is cleaned, is stood, to measure again.
It is real-time that the real-time control module can individually control each heater to carry out adiabatic accelerating calorimeter
Heat compensation.
The adiabatic accelerating calorimeter that the present invention is provided, has the following advantages that：
1st, outer circulation gas pressurized device and interior gas-recycling plant are installed additional, increases the measuring environment and measurement model of instrument
Enclose；
The 2nd, 6 heaters and real-time control module are set, real-time heat compensation can be carried out to instrument.By detecting turnover
Mouth temperature difference, accurately calculates sample exotherms amount, simple to operate, easy to use.
Figure of description
Fig. 1 is the structural representation for the adiabatic accelerating calorimeter that the present invention is provided；
Fig. 2 is the sectional view of the body of heater for the adiabatic accelerating calorimeter that the present invention is provided；
Fig. 3 is the temperature and time change curve for the adiabatic accelerating calorimeter that the present invention is provided；
Fig. 4 is the reacting flow chart for the adiabatic accelerating calorimeter that the present invention is provided.
Embodiment
The present invention is described in detail below by specific embodiment and with reference to accompanying drawing.
Described adiabatic accelerating calorimeter as shown in Figure 1 to Figure 4, including：
The body of heater 1 of closing space, including top cover 11, side wall 12 and base 13 are formed, the volume of the body of heater 1 is preferably
1200cm3, temperature range be 0 DEG C to 580 DEG C, pressure limit be that 0bar to 180bar, controllable heating rate scope are 0 DEG C/min
To 150 DEG C/min；
Polylith is used for the heater 2 heated to material to be measured in the body of heater 1, multiple heaters 2
On the inwall for being uniformly arranged on the body of heater 1；
For the reaction basketry 3 for making material to be measured react, it is described reaction basketry 3 be arranged inside the body of heater 1,
Downside；
Sample heater 4 for placing material to be measured, the sample heater 4 is suspended in inside the reaction basketry 3, i.e., described
The side and bottom surface of sample heater 4 are not contacted with the reaction basketry 3, wherein the optional scope of the volume of the sample heater 4 is
100cm3To 1000cm3, preferably 100cm3、200cm3、500cm3And 1000cm3；
Interior gas-recycling plant 5, the interior gas-recycling plant 5 be arranged at the body of heater 1 it is internal, it is described reaction basketry 3
Upside；
Outer circulation gas pressurized device 6, the outer circulation gas pressurized device 6 connects with the body of heater 1 and forms gas
Import 61 and gas vent 62；
Detecting tool 7；
Cooling device 8, is arranged on the body of heater 1 and forms cooling water inlet 81 and coolant outlet with the body of heater 1
82；
Control system, the control system and the interior gas-recycling plant 5, the outer circulation gas pressurized device 6, institute
State heater 2 and the detecting tool 7 is electrically connected.
The quantity of the heater 2 is 6 pieces, wherein, 2 pieces of heaters 2 are arranged on the top cover 11,2 pieces
The heater 2 is arranged on the side wall 12, and 2 pieces of heaters 2 are arranged on the base 13.
The interior gas-recycling plant 5 is agitating paddle, is provided with motor 51 on the agitating paddle, and the agitating paddle is along suitable
Hour hands rotate.
Relief valve port, proximity switch, couplet on the door lock linkage device and automatic smoke remover are provided with the body of heater 1.
The detecting tool 7 includes 6 groups of temperature-detecting devices 71, material viscosity detection means 72 and 2 groups of flow detection dresses
Temperature-detecting device 71 described in putting 73,6 groups is distributed on the body of heater 1, and the material viscosity detection means 72 is arranged at described
In sample heater 4, flow monitoring device 73 described in 2 groups is respectively arranged at the gas feed 61 and the gas vent 62, institute
The detectivity for stating temperature-detecting device 71 is that 450 DEG C of temperature below resolution ratio are 0.005 DEG C.
Temperature-detecting device 71 described in 3 groups is arranged on the outer wall of body of heater 1, and temperature-detecting device 71 is set described in 1 group
In on the inwall of body of heater 1, temperature-detecting device 71 is arranged at the relief valve port described in 1 group, and temperature detection described in 1 group is filled
Put 71 standby, temperature-detecting device 71 described in 6 groups measure respectively temperature at cooling water inlet 81, temperature at coolant outlet 82,
Temperature at gas feed 61, temperature, reaction temperature equitemperature at gas vent 62.
The control system includes real-time control module, power conditioning module, flow-control module and software control module,
And the software control module is electrically connected with the real-time control module, the power conditioning module and flow-control module, its
In, the control system is EuroARC programs, and the software control module is KALDAS softwares.
It is arranged on the outer circulation gas pressurized device 6 in the gas feed 61 and the gas vent 62 and sets
There are outer circulation pump and non-return valve.
The position of the gas feed 61 and the gas vent 62 on the body of heater 1 is in same horizontal line.
A kind of method for detecting material safety using adiabatic accelerating calorimeter as described above, comprises the following steps：
S1, selection sample heater 4, weigh and record data；
S2, material to be measured is put into sample heater 4, weighed and record data；
S3, the sample heater 4 that will be equipped with material to be measured are put into adiabatic accelerating calorimeter, detection means air-tightness；
S4, setup parameter, according to the performance of material to be measured, set initial temperature, termination in the control system
Temperature, slope sensitivity, programming rate and the parameter of stand-by period；
S5, detection start, and start adiabatic accelerating calorimeter, and adiabatic accelerating calorimeter is detected by control system
And control to reach poised state inside adiabatic accelerating calorimeter, even if the temperature of adiabatic accelerating calorimeter interior point, pressure are equal
One and stably；
S6, reaction regulation, the heating rate of heating rate and adiabatic accelerating calorimeter to sample are compared, and adjustment is every
The heating power of heater 2 described in one, maintains the temperature of adiabatic accelerating calorimeter consistent with sample temperature, is judged by system
Sample enters the neither endothermic nor exothermic stage, is detected；
S7, record data, in the state of the equilibrium, time, temperature, temperature rise rate, pressure and pressure are recorded by control system
The concrete numerical value of power speed；
S8, data analysis, the software control module are analyzed the data obtained by the detecting tool 7, and are painted
Charting；
S9, end measurement, preserve recorded and chart, adiabatic accelerating calorimeter are cooled down by the cooling device 8,
The reaction basketry 3 and the sample heater 4 are taken out, is cleaned, is stood, to measure again.
Embodiment
1st, the sample heater 4 that a quality is M1 is chosen, detected sample is put into sample heater 4, and weighing obtains total matter
Measure M2；
2nd, sample heater 4 is fitted into adiabatic accelerating calorimeter, and checks the air-tightness of adiabatic accelerating calorimeter；
3rd, the door of adiabatic accelerating calorimeter is closed, EuroARC programs are run, setting initial temperature, final temperature, slope are quick
The parameters such as sensitivity, programming rate and stand-by period, preserve Parameter File and name；
4th, nominal pressure sensor initial pressure demarcates half range pressure to 153.15bar to 1bar；
5th, start experiment, adiabatic accelerating calorimeter is detected by control system and the outer circulation pump and institute is controlled
Stating heater 2 makes to reach poised state inside adiabatic accelerating calorimeter, even if the temperature of adiabatic accelerating calorimeter interior point,
Pressure is homogeneous and stably；
6th, to sample heating rate and the heating rate of adiabatic accelerating calorimeter is compared, and adjusts each described in real time
The heating power of heater 2, maintains the temperature of adiabatic accelerating calorimeter consistent with sample temperature, is entered by system judgement sample
Enter the neither endothermic nor exothermic stage, detected；
7th, record data, in the state of the equilibrium, time, temperature, temperature rise rate, pressure and pressure is recorded by control system
The concrete numerical value of speed；
8th, data analysis, the KALDAS softwares are analyzed the data obtained by the detecting tool 7, and draw figure
Table, obtains graphics primitive data, time and maximum rate chart, thermodynamic model, time and the charts such as chart that explode, and lead to
Cross the comprehensive assessment that chart makes above-mentioned detected sample material property；
9th, terminate measurement, preserve recorded and chart, adiabatic accelerating calorimeter is cooled down by the cooling device 8,
The adiabatic accelerating calorimeter internal gas of discharge, takes out the reaction basketry 3 and the sample heater 4, cleans, stand, so as to again
Measurement.
By it is described above be only the preferred embodiment of the present invention, it is noted that for the ordinary skill of the art
For personnel, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (11)
1. a kind of adiabatic accelerating calorimeter, it is characterised in that including：
Form the body of heater of closing space, including top cover, side wall and base；
Polylith is used for the heater heated to material to be measured in the body of heater, and multiple heaters are uniformly arranged
In on the inwall of the body of heater；
For the reaction basketry for making material to be measured react, the reaction basketry is arranged at the furnace interior, downside；
Sample heater for placing material to be measured, the sample heater is suspended in inside the reaction basketry, i.e., described sample heater
Side and bottom surface not with it is described reaction basketry contact；
Interior gas-recycling plant, the interior gas-recycling plant is arranged at the furnace interior, reaction basketry upside；
Outer circulation gas pressurized device, the outer circulation gas pressurized device is connected with the body of heater and to form gas feed gentle
Body is exported；
Detecting tool；
Cooling device, is arranged on the body of heater and forms cooling water inlet and coolant outlet with the body of heater；
Control system, the control system and the interior gas-recycling plant, the outer circulation gas pressurized device, the heating
Device and detecting tool electrical connection.
2. adiabatic accelerating calorimeter according to claim 1, it is characterised in that：The quantity of the heater is 6 pieces, its
In, 2 pieces of heaters are arranged on the top cover, and 2 pieces of heaters are arranged on the side wall, are added described in 2 pieces
Thermal is arranged on the base.
3. adiabatic accelerating calorimeter according to claim 1, it is characterised in that：The interior gas-recycling plant is stirring
Motor is provided with oar, the agitating paddle, and the agitating paddle is rotated clockwise.
4. adiabatic accelerating calorimeter according to claim 1, it is characterised in that：Be provided with the body of heater relief valve port,
Proximity switch, couplet on the door lock linkage device and automatic smoke remover.
5. adiabatic accelerating calorimeter according to claim 4, it is characterised in that：The detecting tool includes 6 groups of temperature inspections
Device, 1 group of material viscosity detection means and 2 groups of flow detectors are surveyed, temperature-detecting device described in 6 groups is distributed in the body of heater
On, the material viscosity detection means is arranged in the sample heater, and flow detector described in 2 groups is respectively arranged at the gas
Body import and the gas outlet.
6. adiabatic accelerating calorimeter according to claim 5, it is characterised in that：Temperature-detecting device described in 3 groups is arranged at
On the furnace body outer wall, temperature-detecting device described in 1 group is arranged on the inboard wall of furnace body, and temperature-detecting device described in 1 group is set
It is placed at the relief valve port, temperature-detecting device described in 1 group is standby.
7. adiabatic accelerating calorimeter according to claim 1, it is characterised in that：The control system includes control mould in real time
Block, power conditioning module, flow-control module and software control module, and the software control module and the real-time control mould
Block, the power conditioning module and flow-control module electrical connection.
8. adiabatic accelerating calorimeter according to claim 1, it is characterised in that：It is arranged at the gas feed and the gas
Outer circulation pump and non-return valve are provided with the outer circulation gas pressurized device in body outlet.
9. adiabatic accelerating calorimeter according to claim 7, it is characterised in that：The gas feed and the gas vent
Position on the body of heater is in same horizontal line.
10. adiabatic accelerating calorimeter according to claim 9, it is characterised in that：The real-time control module can be independent
Each heater is controlled to carry out real-time heat compensation to adiabatic accelerating calorimeter.
11. a kind of method for detecting material safety, it is characterised in that comprise the following steps：
S1, selection sample heater, weigh and record data；
S2, material to be measured is put into sample heater, weighed and record data；
S3, the sample heater that will be equipped with material to be measured are put into adiabatic accelerating calorimeter, detection means air-tightness；
S4, setup parameter, according to the performance of material to be measured, set initial temperature, final temperature, slope in the controls
Susceptibility, programming rate and the parameter of stand-by period；
S5, detection start, and start adiabatic accelerating calorimeter, and adiabatic accelerating calorimeter is detected and controlled by control system
Reach poised state inside the adiabatic accelerating calorimeter of system, though the temperature of adiabatic accelerating calorimeter interior point, pressure it is homogeneous and
It is stable；
S6, reaction regulation, the heating rate to the heating rate of sample and adiabatic accelerating calorimeter are compared, adjust it is each plus
The heating power of thermal, maintains the temperature of adiabatic accelerating calorimeter consistent with sample temperature, is entered by system judgement sample
In the neither endothermic nor exothermic stage, detected；
S7, record data, in the state of the equilibrium, time, temperature, temperature rise rate, pressure and pressure speed are recorded by control system
The concrete numerical value of rate；
S8, data analysis, software control module are analyzed the data obtained by detecting tool, and are drawn a diagram；
S9, end measurement, preserve recorded and chart, and adiabatic accelerating calorimeter, taking-up reaction are cooled down by cooling device
Basketry and the sample heater, are cleaned, and are stood, to measure again.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410852696.0A CN104655671B (en) | 2014-12-31 | 2014-12-31 | Adiabatic accelerating calorimeter and detection method |
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|---|---|---|---|
| CN201410852696.0A CN104655671B (en) | 2014-12-31 | 2014-12-31 | Adiabatic accelerating calorimeter and detection method |
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| CN104655671A CN104655671A (en) | 2015-05-27 |
| CN104655671B true CN104655671B (en) | 2017-08-25 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105676765A (en) * | 2016-03-11 | 2016-06-15 | 上海应用技术学院 | Chemical engineering process security monitoring system |
| CN107064208B (en) * | 2017-02-04 | 2019-04-16 | 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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