CN105301045B - Method of testing for thick liquid and low melting point solid self-heating property - Google Patents
Method of testing for thick liquid and low melting point solid self-heating property Download PDFInfo
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- CN105301045B CN105301045B CN201510664779.1A CN201510664779A CN105301045B CN 105301045 B CN105301045 B CN 105301045B CN 201510664779 A CN201510664779 A CN 201510664779A CN 105301045 B CN105301045 B CN 105301045B
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Abstract
The present invention relates to a kind of method of testing for thick liquid and low melting point solid self-heating property, mainly solves the problems, such as that being not suitable for the solid self-heating property of liquid and fusing point less than 140 DEG C in the prior art tests.The present invention is by using a kind of method of testing for thick liquid and low melting point solid self-heating property, the technical scheme being made up of method of testing program, infrared ray flame detector, the chamber equipped with safety valve and oxygen concentration analyzer, the shuttle with air transmitting device, self-extinguishing accessory system preferably solves above mentioned problem, in the test available for thick liquid and low melting point solid self-heating property.
Description
Technical field
The present invention relates to a kind of method of testing for thick liquid and low melting point solid self-heating property.
Background technology
Whether the present invention is evaluation thick liquid and low melting point solid with the method for testing from thermal hazard.Experiment at present
What room was used to testing chemicals and goods has GB/T 21612-2008 from the method for thermal hazard《Dangerous material inflammable solid self-heating
Test method》、GB19521.5-2004《The solid hazardous goods Tests on Hazardous Properties safety standard of spontaneous combustion》And the United Nations《On
The recommendation of Dangerous Goods Transport --- experiment and manual of standards》(hereinafter referred to as《Experiment and manual of standards》) on self-heating thing
The method of testing of matter.The above-mentioned impartial mark of two national standard method of test uses《Experiment and manual of standards》It is interior on self-heating material
Method of testing, and it is exactly the same for the program description of self-heating substance testing and the design of instrument and equipment in three methods, without any
Difference.Pair and in above-mentioned standard method there are the following problems：
1) length of side 25mm and 100mm the test cube container used in method, is manufactured, aperture is using stainless (steel) wire
0.05mm, and the aperture steel mesh can not contain thick liquid, liquid.
2) intra-method testing temperature is 100 DEG C, 120 DEG C and 140 DEG C, and fusing point is less than the solid sample of test temperature, is not having
It is liquid all to melt when reaching test temperature, is flowed out out of 0.05mm stainless (steel) wire, such as sulphur.
3) it is uneven with air contact after sample fills stainless steel cloth side's cage.
4) method requires that the test period is 24 hours, if sample temperature should suitably prolong still in ascent stage after 24 hours
The long testing time.Once the sample self-heating in test process, temperature is up to several Baidu, temperature control, or even spontaneous combustion of catching fire；
And tester can not the moment scene stare at experimentation, and equipment does not possess the functions such as self-extinguishing, cooling in method, the lighter
There is the phenomenon of damage thermocouple, occur laboratory when serious and the accident such as catch fire, explode.
The present invention targetedly solves the problem.
The content of the invention
The technical problems to be solved by the invention are to be not suitable for liquid and fusing point in existing standard method less than 140 DEG C
A kind of the problem of solid self-heating property is tested, there is provided new method of testing for being used for thick liquid and low melting point solid self-heating property.Should
Method is used in the test of thick liquid and low melting point solid self-heating property, has and is suitable for liquid and fusing point consolidating less than 140 DEG C
The advantages of body self-heating property is tested.
1st, to solve the above problems, the technical solution adopted by the present invention is as follows：One kind is used for thick liquid and eutectic solid point
The method of testing of body self-heating property,
2nd, comprise the following steps：
1) testing sample is loaded in glass container；
2) the stainless steel tube insertion that will act as air peptizaiton is filled in the container of testing sample；
3) air disperser is assembled：Air bottle is connected into the first check valve, flowmeter, is connected with the stainless steel tube；
4) extinguishment control system is assembled：At least two carbon dioxide extinguishers are symmetrically arranged on experiment baking oven both sides, peace
For machinery claw of installing at fire extinguisher handle, installation infrared ray flame detector is electric by the 3rd in the symmetrical both sides of experiment baking oven, manipulator
Magnet valve controls；Installation nitrogen nozzle at the top of baking oven is tested, the nitrogen of the nitrogen cylinder for being connected to the second check valve and experiment baking oven is sprayed
Mouth connects, and nitrogen pipeline is equipped with second solenoid valve, for controlling being passed through for nitrogen；
5) test baking oven be temperature control test baking oven, experiment oven interior be made of refractory material, temperature control ±
0.5℃；Oxygen concentration analyzer equipped with real-time online, installation control system and the computer of data collecting system are dried with experiment
Case connects；
6) will be at least in 5 thermocouple insertion testing samples；
7) by after above-mentioned part all connection, computer is opened, control system and data collecting system relevant parameter are set, is led to
Cross data collecting system and test temperature is set, assign instruction and give experiment baking oven；Mass air flow sensor parameter is set, sets magnetic valve to open
Dynamic parameter；After on-test, it may appear that following three kinds of test situations, control system will make different move according to different situations
Instruct；
If a) five thermocouples inserted in sample are not detected by sample temperature rise, the experiment of setting is maintained always
Baking oven test temperature, then show that self-heating or spontaneous combustion do not occur for sample, after test period reaches, control system is automatically stopped experiment
The heating of baking oven simultaneously carries out air blast cooling, and control system closes the input that the first magnetic valve cut off air automatically；
If b) piece thermocouple of any of which detects sample temperature higher than 60 degree of the test temperature set, baking oven is automatic
Stop heating, open and take cooling mode, when sample temperature reaches 300 degree, then control system automatically turns on second solenoid valve, performs
Nitrogen pours password, until oxygen concentration analyzer output result is reduced to less than 5%, is automatically stopped and pours nitrogen；Rush nitrogen process
In, when tank pressure is more than 150kPa, control system starts the 4th magnetic valve and performs pressure release instruction, when tank pressure is reduced to one
Individual atmospheric pressure, it is automatic to close the 4th magnetic valve；
If c) infrared ray flame detector detects that involuntary ignition occurs for sample, control system automatically turns on the 3rd electromagnetism
Valve, start manipulator and carry out fire extinguisher spraying operation, until flame detector blackout, automatic to close the 3rd magnetic valve.
The present invention has following several big advantages：The shuttle in original method of testing is changed so as to fit in viscous fluid
Body or low melting point solid；Circular beaker is changed into by original stainless steel cloth, and adds air dispersion device, make sample with
The contact of air evenly, carry out slowly oxidation autothermal reaction.The air disperser inserted in sample, sky is passed through with constant rate of speed
Gas, avoid the problem of sample is uneven with air contact, and sample causes oxygen concentration reduction in casing after slowly aoxidizing.Automatically go out
The design of fiery system, after avoiding sample spontaneous combustion or self-heating, and then the possibility of accident is developed into, improve the peace from Thermal test
Overall coefficient.Solve the problems, such as that tester needs to stare at for 24 hours to keep experiment, also fundamentally solve the problems, such as to fire safe.
Full-automatic control system, automatic fire extinguishing system are introduced into from Thermal test by the method, substantially increase safety coefficient and work effect
Rate, and test sample container is improved, solve and be not suitable for the solid of liquid and fusing point less than 140 DEG C in existing method certainly
The problem of hot test, achieve preferable technique effect.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the method for the invention.
1 is computer control and monitor, and 2,3 be check valve, and 4 be the first magnetic valve, and 5 be second solenoid valve, and 6 be the 3rd
Magnetic valve, 7 be air bottle, and 8 be nitrogen cylinder, and 9 be carbon dioxide extinguisher, and 10 be flowmeter, and 11 be that carbon dioxide extinguisher sprays
Mouth, 12 be shuttle, and 13 be the temperature-controlled cabinet with oxygen analyzer, and 14 be nitrogen nozzle, and 15 be air disperser, and 16 be heat
Galvanic couple, 17 be infrared ray flame detector, and 18 be the 4th magnetic valve, and 19 be pressure relief opening.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Embodiment
【Embodiment 1】
The present invention is by method of testing program, infrared ray flame detector, the temperature equipped with safety valve and oxygen concentration analyzer
Control cabinet, the shuttle with air transmitting device, self-extinguishing accessory system composition.As shown in Figure 1.
Shuttle：Internal diameter is 100mm pyroceram beaker.
Air disperser：It is made up of air bottle, check valve, 5 stainless steel tube air dispersers.Stainless steel tube overall diameter is
Two row's apertures are punched on 1.8mm, wall thickness 0.4mm, the relative both sides of stainless steel tube, and small pitch of holes is 0.1mm.
Automatic fire extinguishing system：It is made up of nitrogen cylinder, fire extinguisher, automatic extruder tool torch magnet valve.
Each part and system are as follows：
1st, testing sample is loaded in internal diameter 100mm glass container, filling height is 100mm.
2nd, the stainless steel tube insertion that will act as air peptizaiton is filled in the container of testing sample.
3rd, air disperser is assembled.By oxygen concentration be 21% air bottle connect check valve, flowmeter, with step 2 not
Rust fastener for connection.Air is conveyed with 50ml/min speed in test process, and a whole set of gas circuit is controlled by the first magnetic valve
System.
4th, extinguishment control system is assembled.Two carbon dioxide extinguishers are symmetrically arranged on chamber both sides, installation machinery
Pawl is at fire extinguisher handle, and installation infrared ray flame detector is in the symmetrical both sides of chamber, and manipulator is by the 3rd solenoid valve control；
Installation nitrogen nozzle at the top of chamber, will be connected to the nitrogen cylinder of check valve and the nitrogen nozzle of experiment casing connects, nitrogen pipeline
Equipped with second solenoid valve, for controlling being passed through for nitrogen.
5th, test is temperature control experiment baking oven with casing, and box house is made of refractory material, and temperature control is ± 0.5
℃；Oxygen concentration analyzer equipped with real-time online, by installation control system and the computer and experiment casing of data collecting system
Connection.Control system is used for the heating and cooling of Control experiment casing and each magnetic valve.
6th, 5 thermocouples are inserted in testing sample.
7th, experiment baking oven is temperature control baking oven, the oxygen concentration analyzer equipped with real-time online, the 4th solenoid valve control casing
Pressure release.
Method of testing is described in detail：
After above-mentioned part all connection, computer is opened, control system and data collecting system relevant parameter are set, passed through
Data collecting system sets test temperature, assigns instruction to test oven；Set air mass flow to be calculated as 50ml/min, electromagnetism is set
Valve start-up parameter；After on-test, in fact it could happen that following three kinds of test situations, control system will be made not according to different situations
Same action command.
If 1) five thermocouples inserted in sample are not detected by sample temperature rise, the baking oven of setting is maintained always
Temperature, then show that self-heating or spontaneous combustion do not occur for sample, after experiment reaches in this world, control system is automatically stopped adding for experiment baking oven
Heat simultaneously carries out air blast cooling, and control system closes the input that the first magnetic valve cut off air automatically.
2) if piece thermocouple of any of which detects sample temperature higher than 60 degree of the test temperature set, baking oven is automatic
Stop heating, open and take cooling mode, when sample temperature reaches 300 degree, then control system automatically turns on second solenoid valve, performs
Nitrogen pours password, until oxygen concentration analyzer output result is reduced to less than 5%, is automatically stopped and pours nitrogen.Rush nitrogen process
In, when tank pressure is more than 150kPa, control system starts the 4th magnetic valve and performs pressure release instruction, when tank pressure is reduced to one
Individual atmospheric pressure, it is automatic to close the 4th magnetic valve.
3) if infrared ray flame detector detects that involuntary ignition occurs for sample, control system automatically turns on the 3rd electromagnetism
Valve, start manipulator and carry out fire extinguisher spraying operation, until flame detector blackout, automatic to close the 3rd magnetic valve.
Claims (1)
1. a kind of method of testing for thick liquid and low melting point solid self-heating property, comprise the following steps：
1) testing sample is loaded in glass container；
2) the stainless steel tube insertion that will act as air peptizaiton is filled in the container of testing sample；
3) air disperser is assembled：Air bottle is connected into the first check valve, flowmeter, is connected with the stainless steel tube；
4) extinguishment control system is assembled：At least two carbon dioxide extinguishers are symmetrically arranged on experiment baking oven both sides, fitting machine
Machinery claw is at fire extinguisher handle, and installation infrared ray flame detector is testing the symmetrical both sides of baking oven, and manipulator is by the 3rd magnetic valve
Control；Installation nitrogen nozzle at the top of baking oven is tested, the nitrogen nozzle of the nitrogen cylinder for being connected to the second check valve and experiment baking oven is connected
Connect, nitrogen pipeline is equipped with second solenoid valve, for controlling being passed through for nitrogen；
5) it is that baking oven is tested in temperature control to test baking oven, and experiment oven interior is made of refractory material, and temperature control is ± 0.5
℃；Oxygen concentration analyzer equipped with real-time online, by installation control system and the computer of data collecting system and experiment baking oven
Connection；
6) will be at least in 5 thermocouple insertion testing samples；
7) by after above-mentioned part all connection, computer is opened, control system and data collecting system relevant parameter are set, pass through number
Test temperature is set according to acquisition system, instruction is assigned and gives experiment baking oven；Mass air flow sensor parameter is set, sets magnetic valve to start ginseng
Number；After on-test, it may appear that following three kinds of test situations, control system will be made different actions and refer to according to different situations
Order；
If a) five thermocouples inserted in sample are not detected by sample temperature rise, the experiment baking oven of setting is maintained always
Test temperature, then show that self-heating or spontaneous combustion do not occur for sample, after test period reaches, control system is automatically stopped experiment baking oven
Heating and carry out air blast cooling, control system close automatically the first magnetic valve carry out cut off air input；
If b) piece thermocouple of any of which detects sample temperature higher than 60 degree of the test temperature set, baking oven is automatically stopped
Heating, opens and takes cooling mode, and when sample temperature reaches 300 degree, then control system automatically turns on second solenoid valve, performs nitrogen
Password is poured, until oxygen concentration analyzer output result is reduced to less than 5%, is automatically stopped and pours nitrogen；Rush during nitrogen, case
When body pressure is more than 150kPa, control system starts the 4th magnetic valve and performs pressure release instruction, when tank pressure is reduced to one greatly
Air pressure, it is automatic to close the 4th magnetic valve；
If c) infrared ray flame detector detects that involuntary ignition occurs for sample, control system automatically turns on the 3rd magnetic valve,
Start manipulator and carry out fire extinguisher spraying operation, until flame detector blackout, automatic to close the 3rd magnetic valve.
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| CN105301045B true CN105301045B (en) | 2017-12-12 |
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| CN109387539A (en) * | 2017-08-09 | 2019-02-26 | 中国石油化工股份有限公司 | Mutability is the solid of liquid from thermal hazard test method |
| CN111781230A (en) * | 2019-04-04 | 2020-10-16 | 应急管理部化学品登记中心 | Method for grading danger of thermal decomposition of nitro compound fertilizer |
| CN113262408A (en) * | 2021-04-30 | 2021-08-17 | 中广核新奇特(扬州)电气有限公司 | Fire retardant device for mica tape production and method thereof |
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| CN103808543A (en) * | 2014-01-29 | 2014-05-21 | 南京工业大学 | Self-heating substance thermal reaction test system |
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Patent Citations (6)
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| DE102009013264A1 (en) * | 2009-03-10 | 2010-09-16 | Technische Universität Ilmenau | Magnetic field thermal analyzer for executing e.g. differential thermal analysis, of energetic property of e.g. metallic substance, has positioning system designed, such that end layer is arranged in magnetic and temperature field |
| CN102192924A (en) * | 2010-03-15 | 2011-09-21 | 中华人民共和国上海出入境检验检疫局 | Self-heating test device for flammable solids of dangerous materials |
| CN102928465A (en) * | 2012-10-17 | 2013-02-13 | 中国石油化工股份有限公司 | Full-automatic Koenen test system |
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