CN109387537A - Directly measure the device and method of chemicals self-accelerating decomposition temperature - Google Patents
Directly measure the device and method of chemicals self-accelerating decomposition temperature Download PDFInfo
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- CN109387537A CN109387537A CN201710674419.9A CN201710674419A CN109387537A CN 109387537 A CN109387537 A CN 109387537A CN 201710674419 A CN201710674419 A CN 201710674419A CN 109387537 A CN109387537 A CN 109387537A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
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Abstract
The present invention relates to the device and methods that one kind directly measures chemicals self-accelerating decomposition temperature, mainly solve the problems, such as that accuracy is poor in the prior art.The present invention directly measures the device of chemicals self-accelerating decomposition temperature by using one kind, including cabin, hatch door, circulating fan, heater, refrigerator, indoor environment temperature sensor, Data collection and precessing system, cabin and hatch door, Data collection and precessing system, circulating fan, refrigerator is connected, refrigerator is connected with heater, heater is connected with circulating fan, indoor environment temperature sensor is equipped in cabin, the technical solution of sample thermocouple and sample packaging and method preferably solves the above problem, it can be used in the measurement of chemicals self-accelerating decomposition temperature.
Description
Technical field
The present invention relates to the device and methods that one kind directly measures chemicals self-accelerating decomposition temperature.
Background technique
Self-accelerating decomposition temperature (Self Accelerating Decomposition Temperature, abbreviation SADT)
Refer to that the minimum environment temperature that autoacceleration is decomposed occurs in 7 days for the chemicals of certain packaging material and size.It is measurementization
Product are under particular envelope material and size, an important parameter of thermal hazard during its production, transport, storage etc..
SADT is generallyd use in the world at present to evaluate the thermal hazard of autoreaction chemical substance, and the numerical value of SADT can be well in reality
Reflect thermal hazard of the chemical substance in actual production, storage, transport and use process.So SADT is as chemical substance
The characterisitic parameter of thermal hazard evaluation has obtained the classification of the United Nations's dangerous cargo, the coordination of transport Committee of Experts recommends to the utmost.
Currently, the method for solving about reactive chemical SADT, mainly there is empirical assay and two kinds of predication method.
Empirical assay is the reaction fever of the autoreaction chemical substance by measurement standard pack or mock standard packaging
Characteristic determines the SADT of substance.Generally with the autoreaction chemical substance of standard pack or mock standard packaging in one week,
Under a certain environment temperature, the heating of the autoreaction of the substance increases its temperature and minimum when being more than a certain particular value of environment temperature
Environment temperature indicates.The United Nations's danger transports the Committee of Experts and recommends 4 kinds of practical measuring methods: the i.e. U.S. to people
Formula experimental method, insulation storage experimental method, isothermal storage experimental method and accumulation of heat store experimental method.
Isothermal stores experimental method [CN105203592A] and passes through determining chemicals time-varying heat generation rate at a constant temperature,
The heat loss data of heat generation parameter and chemicals packaging are obtained, together for determining that temperature is decomposed in autoacceleration of the substance in its packaging
Degree.This experimental method sample size is few, operating condition is clear, can carry out in routine experimentation room.But this experimental method is most
What is measured eventually is the heat flow data of sample, still needs to series of computation, changes chemicals in specified packet using the mode determination of mapping
The SADT loaded, acquired results inaccuracy, and sample size is small, cannot be directly used to actual shipment situation.Other three kinds of experiment sides
Method has not been reported.
There are many implementation [Xing Xiaoling for predication method；Xue Liang；The thermal analysis systems such as Zhao Fengqi measure energetic material autoacceleration point
Solve the progress chemical propellant and high molecular material 2009 (04) of temperature], it can [Zang Na be based on by differential scanning calorimeter
The reckoning safety and environment journal 2011 (04) of the DCP self-accelerating decomposition temperature of DSC test] sample is carried out under different rates
Heating scan obtains the thermodynamic parameters such as example reaction initial temperature, thermal discharge, obtains instead using thermokinetic analysis method
Kinetic model is answered, the final SADT for calculating sample under particular envelope；It can also be by being insulated Dewar calorimeter [Huang Fei；Wang Zhen
Just；The self-accelerating decomposition temperature and autoreaction process study safety and environment journal of the ammonium persulfates capsule breaker such as Wang Huixin
2010 (03)] heat flow data of test sample under adiabatic conditions, SADT of the sample under particular envelope is calculated using calculating；
Quantitative Structure-Property Relationship correlation research (Quantitative Structure-Property can also be passed through
Relationship, QSPR) [CN102980972B], the structure of a large amount of reflection molecular structure informations is calculated according to molecular structure
Parameter chooses the feature ginseng comprising abundant structural information with characteristic variable screening technique from calculated a large amount of structural parameters
Number is used as molecular descriptor, finally for the inherent quantitative relationship between selected descriptor and studied physicochemical property, adopts
It is associated with suitable statistical modeling method, establishes pervasive prediction model, the final SADT for calculating chemicals.
Summary of the invention
The first technical problem to be solved by the present invention is the problem that accuracy is poor in the prior art, is provided a kind of new
Directly measure the device of chemicals self-accelerating decomposition temperature.The device has the advantages that accuracy is preferable.The present invention to be solved
The technical issues of two be to provide and a kind of corresponding with one of the technical issues of solution directly measure chemicals autoacceleration decomposition
The method of temperature.
One of in order to solve the above problem, The technical solution adopted by the invention is as follows: a kind of directly measure chemicals autoacceleration
The device of decomposition temperature, including cabin, hatch door, circulating fan, heater, refrigerator, indoor environment temperature sensor, data are adopted
Collection and processing system, cabin are connected with hatch door, Data collection and precessing system, circulating fan, refrigerator, refrigerator and heater
It is connected, heater is connected with circulating fan, and indoor environment temperature sensor, sample thermocouple and sample packaging are equipped in cabin.
In order to solve the above problem two, The technical solution adopted by the invention is as follows: a kind of directly measure chemicals autoacceleration
The method of decomposition temperature includes the following steps: that 1. the chemicals of sample packaging is weighed, is subsequently placed in sealing cabin, and protect
Card packaging is kept at a distance from least 100mm with bulkhead, then sample thermocouple is inserted into the center of packaging from package top, note
Lower sample temperature；2. closing hatch door, temperature rises to set temperature, and temperature and sample in continuous survey room in subsequent process control cabin
Product temperature degree writes down sample temperature 2 DEG C of the time lower than indoor environment temperature, as test at the beginning of, then continuous record
Sample temperature and environment temperature, until sample temperature 6 DEG C of the time higher than environment temperature is observed, at the end of test
Between；3. the self-accelerating decomposition temperature of chemicals is corresponding environment when sample temperature is 6 DEG C higher than environment temperature under terms of packing
Temperature.
In above-mentioned technical proposal, it is preferable that cabin is Horizontal cylinder shape, closed at one end, and the other end is to open automatically
The hatch door closed is passed in and out for test specimen and personnel, after hatch door is closed, is realized to the closed of its internal environment.
In above-mentioned technical proposal, it is preferable that the temperature control in temperature control system, which uses, is heated or cooled circulation air
Mode realize that guarantee uniformity of temperature profile in cabin, temperature is able to achieve the consecutive variations in 0 DEG C~100 DEG C in cabin, and guarantees
Accuracy of temperature control is in ± 2 DEG C.
In above-mentioned technical proposal, it is preferable that Data collection and precessing system is mainly by indoor environment temperature sensor, sample
Temperature thermo-coupler, data communication network and touch screen computer composition, data acquisition process and control system are realized to temperature in cabin
Regulation, sample temperature data acquiring and recording and the automatic open and close function of hatch door.
In above-mentioned technical proposal, it is preferable that in cabin space to guarantee up to 220L sample packaging enter after with bulkhead
At least distance of 100mm is kept, cabin inner wall is constituted using insulating materials.
In above-mentioned technical proposal, it is preferable that temperature control recycles air in cabin using outer fan in cabin, simultaneously
Heater and refrigeration unit, and the start and stop of program controlled heater device or refrigeration unit are set in air circulation duct, to realize
Adjusting to temperature in cabin.
In above-mentioned technical proposal, it is preferable that indoor environment temperature sensor records temperature in cabin, and temperature passes through program in cabin
It is controlled；Sample thermocouple records sample temperature.
In above-mentioned technical proposal, it is preferable if from after on-test in continuous 7 days, sample temperature is all not above ring
6 DEG C of border temperature or more, then terminate this time to test, be cooled to room temperature to sample temperature, opens hatch door and take out sample, reuse new
Chemicals under packaging is tested under conditions of high 5 DEG C, until observing sample temperature 6 DEG C of note higher than environment temperature
Record.
The present invention can directly measure the chemicals self-accelerating decomposition temperature under commodity packaging, the matter of used chemicals
Amount, packaging material and size are commodity forms, and therefore, obtained experimental result is the self-accelerating decomposition temperature of chemicals, nothing
It need to be calculated again, ensure that the accuracy of test result, achieve preferable technical effect.
Detailed description of the invention
Fig. 1 is the flow diagram of device of the present invention.
Fig. 2 is cumyl hydroperoxide self-accelerating decomposition temperature trial curve figure.
Fig. 3 is the heat flow versus temperature curve of the CHP of embodiment 1.
In Fig. 1,1- cabin, 2- hatch door, 3- circulating fan, 4- heater, 5- refrigerator, 6- sample thermocouple, in the cabin 7-
Environment temperature sensor, 8- sample packaging, 9- Data collection and precessing system.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific embodiment
[embodiment 1]
The present invention is by having the constant temperature test carried out in temperature controlled security seal cabin to chemicals at one, directly
It connects to obtain self-accelerating decomposition temperature.
(1) the security seal cabin mainly comprises the following steps:
Cabin ontology: use Horizontal cylinder shape, it is closed at one end, the other end be can automatic shutter hatch door, for examination
Sample and personnel's disengaging are tested, it can be achieved that the closed of its internal environment after hatch door is closed.
Temperature control system: temperature control realizes that this temperature control mode is protected by the way of circulation air is heated or cooled
Uniformity of temperature profile in cabin is demonstrate,proved, temperature is able to achieve the consecutive variations in 0 DEG C~100 DEG C in cabin, and guarantees that accuracy of temperature control exists
In ± 2 DEG C.
Data acquisition process and control system: it is main realize to temperature regulation in cabin, sample temperature data acquiring and recording and
The automatic open and close function of hatch door.
Structure drawing of device is as shown in Figure 1.
(2) to the ontology of cabin, temperature control system and data acquisition process control system, details are as follows:
1. the long 5m of cabin, hatch door diameter 3m, space is sufficiently large in cabin, it is ensured that up to the sample packaging of 220L enters
Afterwards, it is kept at a distance from least 100mm with bulkhead, cabin inner wall is constituted using insulating materials, and hatch door can realize automatic shutter；
2. temperature control recycles air in cabin using outer fan in cabin, while being arranged in air circulation duct
Heater and refrigeration unit, and the start and stop of program controlled heater device or refrigeration unit, have realized the adjusting to temperature in cabin；
3. Data collection and precessing system is mainly by indoor environment temperature sensor, sample temperature thermocouple, data communication
Network and touch screen computer composition；
Temperature in indoor environment temperature sensor essential record cabin, temperature can pass through process control in cabin；Sample temperature heat
Galvanic couple records sample temperature；The automatic open and close function of hatch door is also controlled by the system.
(3) specific implementation method of the invention is as follows:
1. the chemicals of commodity packaging is weighed, it is subsequently placed in sealing cabin, and guarantees that packaging is kept at least with bulkhead
The distance of 100mm, then sample thermocouple is denoted as sample temperature from the center of package top insertion packaging；
2. closing hatch door, temperature rises to set temperature, and temperature and sample in continuous survey room in subsequent process control cabin
Temperature writes down sample temperature 2 DEG C of the time lower than indoor environment temperature, as test at the beginning of, then continuously record sample
Product temperature degree and environment temperature, until observe sample temperature 6 DEG C of the time higher than environment temperature, as the end time of test,
If from after on-test in continuous 7 days, sample temperature is all not above 6 DEG C of environment temperature or more, then terminate this time to test, to
Sample temperature is cooled to room temperature, open hatch door take out sample, reuse the chemicals under new packaging under conditions of high 5 DEG C into
Row test, until observing sample temperature 6 DEG C of record higher than environment temperature；
3. the self-accelerating decomposition temperature of chemicals is corresponding when sample temperature is 6 DEG C higher than environment temperature under terms of packing
Environment temperature.
It is tested using the self-accelerating decomposition temperature that this method carries out cumyl hydroperoxide (CHP)
Experimental procedure:
(1) CHP sample 5kg is weighed, is added in the iron flask of 5L, after covering lid, is placed in security seal cabin, from iron flask top
Portion is inserted into thermocouple to sample center, to record sample temperature；
(2) hatch door is closed, temperature rises to 50 DEG C in subsequent process control cabin, temperature and sample temperature in continuous survey room；
(3) sample temperature 2 DEG C of the time lower than indoor environment temperature is write down to continue to test, directly as time on-test
It is 6 DEG C higher than environment temperature to sample temperature, terminate test；
(4) such as from after on-test, in continuous 7 days, sample temperature is less than 6 DEG C of environment temperature or more always, then terminates
Experiment, and to restart to test than high 5 DEG C of temperature before, until measuring the self-accelerating decomposition temperature of sample；
(5) after the test, it is down to room temperature to sample temperature, opens hatch door, take out sample, and properly dispose；
(6) experimental data is exported, analyzes experimental result, as shown in Figure 2.As seen from Figure 2, when environment temperature rises to 40
DEG C when, sample temperature be 41.2 DEG C.By about 5h, sample is by more lenitively decomposition caused heat release, temperature rise to 57 DEG C, have exceeded
17 DEG C of environment temperature, it is believed that the self-accelerating decomposition temperature of the sample is 40 DEG C；
(7) it is directed to typical polymerization initiator CHP, small-scale experiment projectional technique and large scale test side is respectively adopted
Method has obtained SADT value.
Small-scale experiment predication method using heat analysis laboratory facilities measurement reactive chemical at different temperatures
Heat generation characteristic or autoacceleration temperature-raising characteristic are reacted, the chemical kinetics characteristic and thermodynamic behaviour of the self-reactive substance are found out
(order of reaction, activation energy, pre-exponential factor, reaction calorific value of unit mass etc.), according to the characterisitic parameter of packaging material and
Size calculates SADT of the substance under particular envelope material and size.
A. experimental provision
The micro- calorimeter of C600 (French SETARAM company), the measuring principle and differential scanning calorimeter of the micro- calorimeter of C600
(DSC) almost the same, i.e., under program temperature control, measurement is between the sample and reference substance in same temperature region when unit
Between energy difference (or difference power) variation with temperature rule.
B. experiment condition is as shown in table 1:
1 C600 test condition of table
C. experimental result is as shown in Figure 3.
D. process is calculated
When this example calculates SADT, common cylindrical packing cylinder is calculated in outer layer container selection transportational process, is packed
Wood material is irony, and material parameter can be selected directly from the database of software, before the input of internal layer parameter of materials is by calling in
The result of the thermodynamic modeling in face is realized.Analog calculates the SADT of other packing specifications, and the result being calculated is such as
Shown in table 2.
The SADT that table 2 is obtained based on the limited element analysis technique of Thomas model
When CHP now being carried out large scale test, package shape, material, wall thickness and the sample dimension data of actual selection
It brings into the model that the kinetic parameter obtained by small-scale experiment is calculated, obtained SADT data and large scale test is direct
The data obtained compares, and the results are shown in Table 3.
Table 3 calculates that data and test data compare
As can be seen from the data in the table, the SADT value that predication method obtains is compared with the numerical value that packaging test method obtains for AIBN
It is relatively conservative.This is because there are still following problems for the limited element analysis technique computation model based on Thomas model:
A. for calculation amount is greatly reduced, certain simplification has been carried out to the heat transfer of cylindrically shaped packaging, cuboid packaging, will have been passed
Heat is reduced to two-dimentional computation model by Three-dimensional CAD, and cylindrical body, cuboid are considered as endless, only considers the biography of side
Heat, ignore material inside cylindrical body, cuboid to top and bottom heat transfer situation and packaging top and bottom heat radiation
Situation.This simplification is approximate establishment to longer cylindrical body, cuboid, but to the Calculation of Heat Transfer of short cylinder, cuboid
But it will lead to biggish error.
B. for fluid sample, other than heat transfer, the convection current of liquid internal has heat transfer situation and Temperature Distribution
Very important influence, and closer to gasification temperature, it influences since the disturbance that molecule gasification generates can be more significant.The factor
Influence be far below gasification temperature when can approximation ignore.
In conclusion testing predication method relative to small size, need first to carry out a large number of experiments to obtain thermodynamic data, then ask
Kinetic parameter is led, the process finally calculated, it is simple, quick that the present invention tests process, while result also more accurately may be used
It leans on.
Claims (9)
1. one kind directly measures the device of chemicals self-accelerating decomposition temperature, including cabin, hatch door, circulating fan, heater, system
Cooler, indoor environment temperature sensor, Data collection and precessing system, cabin and hatch door, Data collection and precessing system, circulation
Blower, refrigerator are connected, and refrigerator is connected with heater, and heater is connected with circulating fan, and indoor environment temperature is equipped in cabin
Spend sensor, sample thermocouple and sample packaging.
2. the method that one kind directly measures chemicals self-accelerating decomposition temperature, includes the following steps: the chemistry 1. by sample packaging
Product weighing, is subsequently placed in sealing cabin, and guarantee packaging at a distance from bulkhead holding at least 100mm, then by sample thermocouple
From the center of package top insertion packaging, sample temperature is write down；2. closing hatch door, temperature is risen in subsequent process control cabin
Set temperature, and temperature and sample temperature in continuous survey room, write down sample temperature 2 DEG C of the time lower than indoor environment temperature,
At the beginning of as test, sample temperature and environment temperature are then continuously recorded, until observing sample temperature than environment temperature
High 6 DEG C of the time is spent, the end time as test；3. the self-accelerating decomposition temperature of chemicals is sample temperature under terms of packing
Corresponding environment temperature at 6 DEG C higher than environment temperature of degree.
3. directly measuring the method for chemicals self-accelerating decomposition temperature according to claim 2, it is characterised in that cabin is sleeping
Formula cylindrical shape, it is closed at one end, the other end be can automatic shutter hatch door, passed in and out for test specimen and personnel, when hatch door closes
After closing, realize to the closed of its internal environment.
4. directly measuring the method for chemicals self-accelerating decomposition temperature according to claim 2, it is characterised in that temperature control
Temperature in system is controlled to be realized by the way of circulation air is heated or cooled, uniformity of temperature profile in guarantee cabin, in cabin
Temperature is able to achieve the consecutive variations in 0 DEG C~100 DEG C, and guarantees accuracy of temperature control in ± 2 DEG C.
5. directly measuring the method for chemicals self-accelerating decomposition temperature according to claim 2, it is characterised in that data acquisition
Unit is mainly calculated by indoor environment temperature sensor, sample temperature thermocouple, data communication network and touch screen with processing system
Realized at, data acquisition process and control system temperature regulation, sample temperature data acquiring and recording and hatch door in cabin are opened automatically,
Close function.
6. directly measuring the method for chemicals self-accelerating decomposition temperature according to claim 2, it is characterised in that in cabin space
Guarantee to keep at a distance from least 100mm after the sample packaging of up to 220L enters with bulkhead, cabin inner wall uses insulation material
Material is constituted.
7. directly measuring the method for chemicals self-accelerating decomposition temperature according to claim 2, it is characterised in that temperature in cabin
Control recycles air in cabin using outer fan, while heater and refrigeration unit being arranged in air circulation duct,
And the start and stop of program controlled heater device or refrigeration unit, to realize the adjusting to temperature in cabin.
8. directly measuring the method for chemicals self-accelerating decomposition temperature according to claim 2, it is characterised in that indoor environment
Temperature sensor records temperature in cabin, and temperature is controlled by program in cabin；Sample thermocouple records sample temperature.
9. directly measuring the method for chemicals self-accelerating decomposition temperature according to claim 2, it is characterised in that if from trying
It tests after beginning in continuous 7 days, sample temperature is all not above 6 DEG C of environment temperature or more, then terminates this time to test, to sample temperature
It being cooled to room temperature, opens hatch door and take out sample, the chemicals reused under new packaging is tested under conditions of high 5 DEG C,
Until observing sample temperature 6 DEG C of record higher than environment temperature.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113740372A (en) * | 2020-05-28 | 2021-12-03 | 应急管理部化学品登记中心 | Method for rapidly calculating self-accelerating decomposition temperature of substance and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113740372A (en) * | 2020-05-28 | 2021-12-03 | 应急管理部化学品登记中心 | Method for rapidly calculating self-accelerating decomposition temperature of substance and application thereof |
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Application publication date: 20190226 |