CN103076363B - Method for determining critical pressure range for explosive decomposition of pressure sensitive gas - Google Patents

Method for determining critical pressure range for explosive decomposition of pressure sensitive gas Download PDF

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Publication number
CN103076363B
CN103076363B CN201210406009.3A CN201210406009A CN103076363B CN 103076363 B CN103076363 B CN 103076363B CN 201210406009 A CN201210406009 A CN 201210406009A CN 103076363 B CN103076363 B CN 103076363B
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pressure
gas
compressor
sensibility
autoclave
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CN103076363A (en
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王振刚
江美丽
孟庭宇
郑俊鹤
黄飞
孙峰
姜杰
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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Abstract

The invention provides a pressure sensitive explosive testing device based method for determining a critical pressure range for explosive decomposition of pressure sensitive gas without participation of oxygen. The method comprises steps of: step 1, vacuumizing; step 2, preheating the pressure sensitive gas to be tested; and step 3, compressing the pressure sensitive gas to be tested, and determining the critical pressure range for explosive decomposition of the pressure sensitive gas without participation of oxygen. The test method can determine the critical pressure range for explosive decomposition of pressure sensitive gas without participation of oxygen, and has advantages of wide test range for the critical pressure range, precise controlled temperature in the test process, and examination on stability of pressure sensitive gas under high temperature and high pressure for a long time.

Description

The method of the emergent pressure scope of test pressure susceptibility gas generation decomposition explosion
Technical field
The invention belongs to technical field of petrochemical industry, particularly relate to a kind of method of emergent pressure scope of test pressure susceptibility gas generation decomposition explosion.
Background technology
In petrochemicals production and transportation, due to acetylene, butadiene, vinylacetylene, the gases such as methyl nitrite are comparatively responsive to pressure, after pressure exceedes certain value, even if also can decomposition explosion be there is under the condition participated in not having oxygen, the safety its blast characteristics research being ensured to production and transport is needed in operating mode production and transport process, this just needs to test it to issue raw decomposition explosion emergent pressure in the condition not having oxygen to participate in, therefore, to the system of the airtight compressible controllable temperature of blast characteristics test needs one of this type of gas, the pressure of pressure sensibility gas is changed by the volume changing system, thus realize the test of emergent pressure.
Current gas phase fires the proving installation of parameter, all carry out firing test for " inflammable gas+oxidant combustion gas " system or " inflammable gas+oxidizing gas+inert gas " system, proving installation is airtight incompressible device, and all need the participation of oxygen, the requirement of the emergent pressure this type of pressure sensibility gas being measured under the condition not having oxygen to participate in its decomposition explosion cannot be met.
The applicant of the application is measure the emergent pressure that pressure sensibility gas acetylene measures its decomposition explosion under the condition not having oxygen to participate at the patent acetylene gas pressure sensitivity explosion testing device (patent publication No. CN101995449A) applied for before, but the defect adopting this device to exist is that its test pressure scope is narrow, only can test emergent pressure when there is the emergent pressure scope of the decomposition explosion pressure sensibility gas generation decomposition explosion close with acetylene, and cannot obtain the test to pressure sensibility gas of other emergent pressure scopes, in addition, adopt this device cannot investigate the stability of pressure sensibility gas under long-time high-temperature and high-pressure conditions.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method adopting pressure-sensitive explosion test device to test emergent pressure scope pressure sensibility gas being issued to raw decomposition explosion in the condition not having oxygen to participate in, adopt this method of testing can measure emergent pressure scope pressure sensibility gas being issued to raw decomposition explosion in the condition not having oxygen to participate in, the emergent pressure scope of its test is wide, accurately can control the temperature of test process, the stability of pressure sensibility gas under long-time high-temperature and high-pressure conditions can be investigated simultaneously.
For solving the problems of the technologies described above, the invention provides a kind of method adopting pressure-sensitive explosion test device to test emergent pressure scope pressure sensibility gas being issued to raw decomposition explosion in the condition not having oxygen to participate in, it comprises:
The first step, vacuumizes;
Second step, to pressure sensibility air preheat to be tested;
3rd step, to pressure sensibility gas compression to be tested, measures it issues raw decomposition explosion emergent pressure scope in the condition not having oxygen to participate in;
Described pressure-sensitive explosion test device comprises:
Compressor, Detonation Tube, pressure-detecting device, temperature-detecting device, vacuum pump, chromatograph and Computer Control Unit, described temperature-detecting device is positioned on described Detonation Tube, described Detonation Tube is connected by pipeline with described compressor, described pressure-detecting device is positioned on described compressor, described vacuum pump is connected with described compressor, and described chromatograph is also connected with described compressor.
Wherein, the described first step is specially further before experiment starts and first rinses described Detonation Tube, described compressor and described autoclave with nitrogen, then uses vacuum pump evacuation for subsequent use.
Wherein, described second step is specially further and carries out preheating by pressure sensibility gas to be tested feeding Detonation Tube, temperature required under obtaining high temperature and high pressure condition condition, preheated pressure sensibility gas to be tested enters into the air intake opening of described compressor by connecting line.
Wherein, described 3rd step is specially described pressure sensibility gas to be tested further and carries out two stages of compression in described compressor, first the pressure in described compressor is risen to 0.5MPa through one stage of compression by normal pressure, 3MPa is being risen to by 0.5MPa through two-stage compression, opening pressure record during gas compression, pressure data is presented on Computer Control Unit in real time, if gas does not react under set pressure condition, pressure curve slope is 0, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure.
Present invention also offers a kind of method adopting pressure-sensitive explosion test device to test emergent pressure scope pressure sensibility gas being issued to raw decomposition explosion in the condition not having oxygen to participate in, described pressure-sensitive explosion test device comprises compressor, Detonation Tube, autoclave, pressure-detecting device, temperature-detecting device, vacuum pump, chromatograph and Computer Control Unit, described temperature-detecting device is positioned on described Detonation Tube, described Detonation Tube is connected by pipeline with described compressor, described pressure-detecting device is positioned on described compressor, described autoclave is connected with described compressor, described vacuum pump is connected with described autoclave, described chromatograph is connected with described autoclave with described compressor, described method of testing comprises:
The first step, vacuumizes;
Second step, to pressure sensibility air preheat to be tested;
3rd step, to pressure sensibility gas compression to be tested, measures it issues raw decomposition explosion emergent pressure scope in the condition not having oxygen to participate in;
4th step, for the transient pressure susceptibility gas not recording critical decomposition pressure, after it is compressed by described compressor, pass into the autoclave after vacuumizing airtight, autoclave temp setting is identical with working temperature, gas is chromatograph instrument gas phase composition at set intervals, judges that gas decomposes situation.
Wherein, the described first step is specially further before experiment starts and first rinses described Detonation Tube, described compressor and described autoclave with nitrogen, then uses vacuum pump evacuation for subsequent use.
Wherein, described second step is specially further and carries out preheating by pressure sensibility gas to be tested feeding Detonation Tube, temperature required under obtaining high temperature and high pressure condition condition, preheated pressure sensibility gas to be tested enters into the air intake opening of described compressor by connecting line.
Wherein, described 3rd step is specially described pressure sensibility gas to be tested further and carries out two stages of compression in described compressor, first the pressure in described compressor is risen to 0.5MPa through one stage of compression by normal pressure, 3MPa is being risen to by 0.5MPa through two-stage compression, opening pressure record during gas compression, pressure data is presented on Computer Control Unit in real time, if gas does not react under set pressure condition, pressure curve slope is 0, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure.
Present invention also offers a kind of method adopting pressure-sensitive explosion test device to test emergent pressure scope pressure sensibility gas being issued to raw decomposition explosion in the condition not having oxygen to participate in, described pressure-sensitive explosion test device comprises compressor, Detonation Tube, autoclave, pressure-detecting device, temperature-detecting device, vacuum pump, chromatograph and Computer Control Unit, described temperature-detecting device is positioned on described Detonation Tube, described Detonation Tube is connected by pipeline with described compressor, described pressure-detecting device is positioned on described compressor, described autoclave is connected with described compressor, described vacuum pump is connected with described autoclave, described chromatograph is connected with described autoclave with described compressor, described method of testing comprises:
The first step, first rinses described Detonation Tube, described compressor and described autoclave with nitrogen before experiment starts, then uses vacuum pump evacuation for subsequent use;
Second step, sends into pressure sensibility gas to be tested in Detonation Tube and carries out preheating, temperature required under obtaining high temperature and high pressure condition condition, and preheated pressure sensibility gas to be tested enters into the air intake opening of described compressor by connecting line;
3rd step, described pressure sensibility gas to be tested carries out two stages of compression in described compressor, first the pressure in described compressor is risen to 0.5MPa through one stage of compression by normal pressure, 3MPa is being risen to by 0.5MPa through two-stage compression, opening pressure record during gas compression, pressure data is presented on Computer Control Unit in real time, if gas does not react under set pressure condition, pressure curve slope is 0, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure,
4th step, for the transient pressure susceptibility gas not recording critical decomposition pressure, after it is compressed by described compressor, pass into the autoclave after vacuumizing airtight, autoclave temp setting is identical with working temperature, gas is chromatograph instrument gas phase composition at set intervals, judges that gas decomposes situation.
Present invention also offers the above-mentioned application of method in petrochemical complex safety in production pressure sensibility gas being issued to the emergent pressure scope of raw decomposition explosion in the condition not having oxygen to participate in.
The technique effect that the present invention is useful is:
Employing pressure-sensitive explosion test device test provided by the invention issues the emergent pressure scope of raw decomposition explosion in the condition not having oxygen to participate in method to pressure sensibility gas can measure emergent pressure scope pressure sensibility gas being issued to raw decomposition explosion in the condition not having oxygen to participate in, the emergent pressure scope of its test is wide, accurately can control the temperature of test process, the stability of pressure sensibility gas under long-time high-temperature and high-pressure conditions can be investigated simultaneously.
Accompanying drawing explanation
Fig. 1 is pressure-sensitive explosion test device structural drawing provided by the invention;
Fig. 2 is the structural drawing of the Detonation Tube in pressure-sensitive explosion test device provided by the invention.
Reference numeral is as follows: 1-compressor one stage of compression part; 2-compressor two-stage compression part; 3-1 level rain glass; 4-2 level rain glass; 5-autoclave; 6-tensimeter; 7-thermometer; 8-vacuum pump; 9-Computer Control Unit; 10-compressor; 11-1 level temperature sensor; 12-2 level temperature sensor; 13-1 level oil pressure gauge; 14-2 level oil pressure gauge; 15-rupture disk;
Detonation Tube mark is as follows: 1A-vacuum pump; 2A-surge tank; 3A-vacuum pump ball valve; 4A-needle-valve; 5A-retaining valve; 6A-sample introduction needle-valve; 7A-detonation body; 8A-view window; 9A-attemperating unit; 10A-circulating fan; 11A-tail gas discharging pipe; 12A-digital pressure gauge; 13A-compressor inlet needle-valve; 14A-safety valve.
Embodiment
The invention provides one and carry out pressure-sensitive explosion test device to pressure sensibility gas, it comprises:
Compressor, Detonation Tube, pressure-detecting device, temperature-detecting device, vacuum pump, chromatograph and Computer Control Unit;
Described Detonation Tube is used for carrying out preheating to pressure sensibility gas, temperature required under obtaining high temperature and high pressure condition condition;
Described temperature-detecting device is positioned on described Detonation Tube, for detecting the temperature of carrying out pressure sensibility air preheat in Detonation Tube, and by temperature feedback to Computer Control Unit, according to Computer Control Unit feedack, control the preheat temperature in Detonation Tube;
Described Detonation Tube is connected by pipeline with described compressor, and the pressure sensibility gas through Detonation Tube preheating enters into described compressor;
Described compressor is used for compressing pressure sensibility gas, thus measures pressure sensibility gas issues solution explosion time estranged emergent pressure in the condition not having oxygen to participate in;
Described pressure-detecting device is positioned on described compressor, for detecting the pressure in compressor in real time, and by information feed back to Computer Control Unit, Computer Control Unit feedack, controls compressor to the compression of the pressure sensibility gas be positioned at wherein and stopping;
Described vacuum pump is connected with described compressor, for vacuumizing described compressor and Detonation Tube;
Whether described chromatograph is also connected with described compressor, decompose, thus judge whether to arrive emergent pressure for detecting the pressure sensibility gas after stopping compression in described compressor;
Described Computer Control Unit is used for monitoring the temperature in described Detonation Tube and compressed the produced pressure of described pressure sensibility gas in described compressor in real time.
Further, described pressure-sensitive explosion test device can be only made up of above-mentioned parts.
Required temperature range is normal temperature ~ 200 DEG C.
Some unstable gas does not record critical decomposition pressure in compression process, but can slowly decompose under the condition having certain temperature and pressure, decompose and release energy, when energy accumulation to a certain extent after can accelerated decomposition, thus it is explosion caused, in storage process, autoacceleration decomposition explosion whether is there is for investigating unstable gas, described pressure-sensitive explosion test device further comprises autoclave, described autoclave is arranged between described compressor and described vacuum pump, while be connected with described compressor, while be connected with described vacuum pump, through compressor compresses but the pressure sensibility gas not recording critical decomposition pressure enters into autoclave investigates the stability of pressure sensibility gas under long-time high-temperature and high-pressure conditions (i.e. working condition), the test specification of High Temperature High Pressure is normal pressure ~ 3MPa, temperature: normal temperature ~ 200 DEG C, described vacuum pump is also for vacuumizing described autoclave, described chromatograph is also connected with described autoclave, for judging the decomposition situation under high-temperature and high-pressure conditions of this kind of pressure sensibility gas.
Described autoclave is also provided with pressure-detecting device and temperature-detecting device, and described pressure-detecting device can be tensimeter, and described temperature-detecting device can be thermometer.
The pipeline be connected between described Detonation Tube and described vacuum pump is provided with companion's heat, the setting of its temperature sets identical with the temperature on described Detonation Tube, the i.e. temperature to be tested of gas, for making described pressure sensibility gas at whole test period and the temperature remained constant testing link, to record gas emergent pressure at such a temperature accurately, the material of described connecting line can be steel.
Described compressor mainly comprises cylinder and promotes piston, by realizing the compression of pressure sensibility gas volume to the propelling of piston, thus improve the pressure of compressor, compressor temperature and pressure signal is monitored at any time in compressor pressure elevation process, when pressure signal raises suddenly, illustrate that pressure sensibility gas there occurs decomposition, create blast.
The cylinder skin of described compressor has chuck, carries out temperature control by conduction oil.
Described pressure-detecting device is positioned on the cylinder of described compressor, it can be pressure transducer, pressure transducer connects Computer Control Unit, by the pressure information on Real-time Feedback compressor, thus pressure curve is recorded on Computer Control Unit, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph instrument gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure.
Described compressor comprises one stage of compression part and two-stage compression part, connected by pipeline between the exhausr port of described one stage of compression part and the air intake opening of two-stage compression part, described one stage of compression part have two retaining valves, when the piston is moving down, air intake opening retaining valve is opened, gas outlet closed check valve, completes air-breathing; When the piston is moving up, air intake opening closed check valve, gas outlet retaining valve is opened, complete compression exhaust, the gas after compression enters two-stage compression part, described two-stage compression part has two retaining valves, when the piston is moving down, air intake opening retaining valve is opened, and gas outlet closed check valve, completes air-breathing; When the piston is moving up, air intake opening closed check valve, gas outlet retaining valve is opened, complete compression exhaust, one stage of compression part makes the pressure of gas rise to 0.5MPa by normal pressure, two-stage compression part makes the pressure of gas by the most promotion of 0.5MPa to 3MPa, and the M2V-5/200 that this compressor is produced by Dandong Jin Ding compressor company limited gets through transformation.
Further, described compressor is only made up of one stage of compression part and two-stage compression part.
Described compressor there are 4 tensimeters and 2 temperature sensors, four tensimeters are 1 grade of oil pressure gauge respectively, 1 grade of rain glass and 2 grades of oil pressure gauges, 2 grades of rain glasss, oil pressure gauge display be the pressure of compressor oil, what rain glass showed is current gaseous tension to be compressed, oil pressure gauge and rain glass by the force information back that obtains to Computer Control Unit, 1 grade of oil pressure gauge and 1 grade of rain glass are positioned in the one stage of compression part of described compressor, 2 grades of oil pressure gauges and 2 grades of rain glasss are positioned in the two-stage compression part of described compressor, 2 temperature sensors lay respectively at one stage of compression part and the two-stage compression part of described compressor, be respectively used to the temperature measuring one stage of compression part and two-stage compression part, and the temperature information of acquisition is fed back to Computer Control Unit.
Gas to be measured from Detonation Tube through be preheating to treat testing temperature laggard enter compressor one stage of compression part, gaseous tension after compression enters secondary compressing portion and divides after 1 grade of oil pressure gauge and 1 grade of rain glass detect, gas after two-stage compression enters autoclave after 2 grades of oil pressure gauges and 2 grades of rain glasss detect, close compressor and autoclave air intake valve after pressure in autoclave rises to testing pressure, the temperature of autoclave is recorded by thermometer, and pressure is recorded by tensimeter.
Preferably, the escape pipe of described one stage of compression part and the escape pipe of described two-stage compression part are provided with rupture disk, when being fallen by pressure releasing in time after pressure sensibility gas generation decomposition explosion superpressure, prevent superpressure from causing damage to instrument.
Further, described compressor is only made up of above-mentioned parts.
The test pressure scope of described pressure-sensitive explosion test device is normal pressure ~ 3MPa, and Range of measuring temp is normal temperature ~ 200 DEG C.
Present invention also offers one and carry out pressure-sensitive explosion test device to pressure sensibility gas, it comprises:
Compressor, Detonation Tube, autoclave, pressure-detecting device, temperature-detecting device, vacuum pump, chromatograph and Computer Control Unit;
Described Detonation Tube is used for carrying out preheating to pressure sensibility gas, temperature required under obtaining high temperature and high pressure condition condition;
Described temperature-detecting device is positioned on described Detonation Tube, for detecting the temperature of carrying out pressure sensibility air preheat in Detonation Tube, and by temperature feedback to Computer Control Unit, according to Computer Control Unit feedack, control the preheat temperature in Detonation Tube;
Described Detonation Tube is connected by pipeline with described compressor, and the pressure sensibility gas through Detonation Tube preheating enters into described compressor;
The pipeline be connected between described Detonation Tube and described vacuum pump is provided with companion's heat, the setting of its temperature sets identical with the temperature on described Detonation Tube, the i.e. temperature to be tested of gas, for making described pressure sensibility gas at whole test period and the temperature remained constant testing link, to record gas emergent pressure at such a temperature accurately;
Described compressor is used for compressing pressure sensibility gas, thus measures pressure sensibility gas issues solution explosion time estranged emergent pressure in the condition not having oxygen to participate in;
Described pressure-detecting device is positioned on described compressor, for detecting the pressure in compressor in real time, and by information feed back to Computer Control Unit, according to Computer Control Unit feedack, control compressor to the compression of the pressure sensibility gas be positioned at wherein and stopping;
Described compressor mainly comprises cylinder and promotes piston, by realizing the compression of pressure sensibility gas volume to the propelling of piston, thus improve the pressure of compressor, compressor temperature and pressure signal is monitored at any time in compressor pressure elevation process, when pressure signal raises suddenly, illustrate that pressure sensibility gas there occurs decomposition, create blast;
The cylinder skin of described compressor has chuck, carries out temperature control by conduction oil;
Described compressor comprises one stage of compression part and two-stage compression part, divided by one stage of compression part and secondary compressing portion and carry out two-stage compression, one stage of compression part makes the pressure of described compressor rise to 0.5MPa by normal pressure, and two-stage compression part makes the pressure of described compressor by the most promotion of 0.5MPa to 3MPa;
Described compressor there are 4 tensimeters and 2 temperature sensors, four tensimeters are 1 grade of oil pressure gauge respectively, 1 grade of rain glass and 2 grades of oil pressure gauges, 2 grades of rain glasss, oil pressure gauge display be the pressure of compressor oil, what rain glass showed is current gaseous tension to be compressed, oil pressure gauge and rain glass by the force information back that obtains to Computer Control Unit, 1 grade of oil pressure gauge and 1 grade of rain glass are positioned in the one stage of compression part of described compressor, 2 grades of oil pressure gauges and 2 grades of rain glasss are positioned in the two-stage compression part of described compressor, 2 temperature sensors lay respectively at one stage of compression part and the two-stage compression part of described compressor, be respectively used to the temperature measuring one stage of compression part and two-stage compression part, and the temperature information of acquisition is fed back to Computer Control Unit,
Described autoclave is connected with described compressor, through compressor compresses but the pressure sensibility gas not recording critical decomposition pressure enters into autoclave investigates the stability of this kind of pressure sensibility gas under long-time high-temperature and high-pressure conditions (i.e. working condition);
Described autoclave is also provided with described pressure-detecting device and described temperature-detecting device;
Described vacuum pump is connected with described autoclave, for vacuumizing described compressor, Detonation Tube and autoclave;
Described chromatograph is connected with described autoclave with described compressor, when detecting the pressure sensibility gas in described compressor, whether decompose for detecting the pressure sensibility gas after stopping compression in described compressor, thus judge whether to arrive emergent pressure, when detecting the pressure sensibility gas in described autoclave, for detecting the stability of this kind of pressure sensibility gas under long-time high-temperature and high-pressure conditions (i.e. working condition);
Described Computer Control Unit is used for monitoring the temperature in described Detonation Tube and compressed the produced pressure of described pressure sensibility gas in described compressor in real time.
Described pressure-detecting device is positioned on the cylinder of described compressor, it can be pressure transducer, pressure transducer connects Computer Control Unit, by the pressure information on Real-time Feedback compressor, thus pressure curve is recorded on Computer Control Unit, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph instrument gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure.
Further, described pressure-sensitive explosion test device is preferably only made up of above-mentioned parts.
The test pressure scope of described pressure-sensitive explosion test device is normal pressure ~ 3MPa, and Range of measuring temp is normal temperature ~ 200 DEG C.
Present invention also offers the method adopting the test of above-mentioned pressure-sensitive explosion test device pressure sensibility gas to be issued to the emergent pressure scope of raw decomposition explosion in the condition not having oxygen to participate in, it comprises:
The first step, vacuumizes;
Second step, to pressure sensibility air preheat to be tested;
3rd step, to pressure sensibility gas compression to be tested, measures it issues raw decomposition explosion emergent pressure scope in the condition not having oxygen to participate in.
The described first step is specially further before experiment starts and first rinses described Detonation Tube, described compressor and described autoclave with nitrogen, then uses vacuum pump evacuation for subsequent use.
Described second step is specially further and carries out preheating by pressure sensibility gas to be tested feeding Detonation Tube, temperature required under obtaining high temperature and high pressure condition condition, preheated pressure sensibility gas to be tested enters into the air intake opening of described compressor by connecting line, required temperature range is normal temperature ~ 200 DEG C.
Described 3rd step is specially described pressure sensibility gas to be tested further and carries out two stages of compression in described compressor, first the pressure in described compressor is risen to 0.5MPa through one stage of compression by normal pressure, 3MPa is being risen to by 0.5MPa through two-stage compression, opening pressure record during gas compression, pressure data is presented on Computer Control Unit in real time, if gas does not react under set pressure condition, pressure curve slope is 0, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure.
Described method of testing further comprises the 4th step, for the transient pressure susceptibility gas not recording critical decomposition pressure, after it is compressed by described compressor, pass into the autoclave after vacuumizing airtight, autoclave temp setting is identical with working temperature, gas is chromatograph instrument gas phase composition at set intervals, judges that gas decomposes situation.
Present invention also offers the method adopting the test of above-mentioned pressure-sensitive explosion test device pressure sensibility gas to be issued to the emergent pressure scope of raw decomposition explosion in the condition not having oxygen to participate in, it comprises:
The first step, first rinses described Detonation Tube, described compressor and described autoclave with nitrogen before experiment starts, then uses vacuum pump evacuation for subsequent use;
Second step, pressure sensibility gas to be tested is sent in Detonation Tube and carries out preheating, temperature required under obtaining high temperature and high pressure condition condition, preheated pressure sensibility gas to be tested enters into the air intake opening of described compressor by connecting line, required temperature range is normal temperature ~ 200 DEG C;
3rd step, described pressure sensibility gas to be tested carries out two stages of compression in described compressor, first the pressure in described compressor is risen to 0.5MPa through one stage of compression by normal pressure, 3MPa is being risen to by 0.5MPa through two-stage compression, opening pressure record during gas compression, pressure data is presented on Computer Control Unit in real time, if gas does not react under set pressure condition, pressure curve slope is 0, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure,
4th step, for the transient pressure susceptibility gas not recording critical decomposition pressure, after it is compressed by described compressor, pass into the autoclave after vacuumizing airtight, autoclave temp setting is identical with working temperature, gas is chromatograph instrument gas phase composition at set intervals, judges that gas decomposes situation.
Present invention also offers above-mentioned pressure-sensitive explosion test device and adopt this device to test pressure sensibility gas to be issued to the application of method in petrochemical complex safety in production of the emergent pressure scope of raw decomposition explosion in the condition not having oxygen to participate in.
Describe embodiments of the present invention in detail below with reference to embodiment, to the present invention, how application technology means solve technical matters whereby, and the implementation procedure reaching technique effect can fully understand and implement according to this.
As shown in Figure 2, Detonation Tube comprises with lower component: vacuum pump 1A, surge tank 2A, vacuum pump ball valve 3A, needle-valve 4A, retaining valve 5A, sample introduction needle-valve 6A, detonation body 7A, view window 8A, attemperating unit 9A, circulating fan 10A, tail gas discharging pipe 11A, digital pressure gauge 12A, compressor inlet needle-valve 13A, safety valve 14A, and each parts connect as shown in Figure 2.
As shown in Figure 1, of the present invention pressure-sensitive explosion test device is carried out to pressure sensibility gas, it comprises: compressor 10, Detonation Tube, autoclave 5, vacuum pump 8, chromatograph and Computer Control Unit 9, described Detonation Tube has attemperating unit 9A for controlling to carry out in Detonation Tube the temperature of pressure sensibility gas, and temperature signal is fed back to Computer Control Unit 9, according to Computer Control Unit feedack, control the preheat temperature in Detonation Tube, Detonation Tube is connected by pipeline with compressor 10, pressure sensibility gas through Detonation Tube preheating enters into compressor 10, the pipeline be connected between described Detonation Tube and described vacuum pump 8 is provided with companion's heat, the setting of its temperature sets identical with the temperature on described Detonation Tube, the i.e. temperature to be tested of gas, for making described pressure sensibility gas at whole test period and the temperature remained constant testing link, to record gas emergent pressure at such a temperature accurately, described compressor comprises one stage of compression part 1 and two-stage compression part 2, one stage of compression part 1 has retaining valve, two-stage compression part 2 has retaining valve, two-stage compression is carried out by one stage of compression part 1 and two-stage compression part 2, one stage of compression part 1 makes the pressure of described compressor rise to 0.5MPa by normal pressure, two-stage compression part 2 makes the compression pressure of described compressor by the most promotion of 0.5MPa to 3MPa, described compressor there are 4 tensimeters and 2 temperature sensors, four tensimeters are 1 grade of oil pressure gauge 13 respectively, 1 grade of rain glass 3 and 2 grades of oil pressure gauges 14, 2 grades of rain glasss 4, oil pressure gauge display be the pressure of compressor oil, what rain glass showed is current gaseous tension to be compressed, oil pressure gauge and rain glass by the force information back that obtains to Computer Control Unit, 1 grade of oil pressure gauge 13 and 1 grade of rain glass 3 are positioned in the one stage of compression part 1 of described compressor, 2 grades of oil pressure gauges 14 and 2 grades of rain glasss 4 are positioned in the two-stage compression part 2 of described compressor, 2 temperature sensors, 1 grade of temperature sensor 11 and 2 grades of temperature sensors 12 lay respectively at one stage of compression part 1 and the two-stage compression part 2 of described compressor, be respectively used to the temperature measuring one stage of compression part 1 and two-stage compression part 2, and the temperature information of acquisition is fed back to Computer Control Unit 9, the escape pipe of described one stage of compression part 1 and the escape pipe of described two-stage compression part 2 are provided with rupture disk 15, described compressor 10 mainly comprises cylinder and promotes piston, by realizing the compression of pressure sensibility gas volume to the propelling of piston, thus improve the pressure of compressor, compressor temperature and pressure signal is monitored at any time in compressor pressure elevation process, when pressure signal raises suddenly, illustrate that pressure sensibility gas there occurs decomposition, create blast, the cylinder skin of described compressor 10 has chuck, temperature control is carried out by conduction oil, described autoclave 5 is connected with described compressor 10, to compress but the pressure sensibility gas not recording critical decomposition pressure enters into autoclave 5 investigates the stability of this kind of pressure sensibility gas under long-time high-temperature and high-pressure conditions (i.e. working condition) through compressor 10, described autoclave is provided with tensimeter 6 and thermometer 7, described vacuum pump 8 is connected with described autoclave 5, for to described compressor 10, Detonation Tube and autoclave 5 vacuumize, described chromatograph is connected with described autoclave with described compressor, when detecting the pressure sensibility gas in described compressor, whether decompose for detecting the pressure sensibility gas after stopping compression in described compressor, thus judge whether to arrive emergent pressure, when detecting the pressure sensibility gas in described autoclave, for detecting the stability of this kind of pressure sensibility gas under long-time high-temperature and high-pressure conditions (i.e. working condition), described Computer Control Unit 9 is for monitoring the temperature in described Detonation Tube and compressed the produced pressure of described pressure sensibility gas in described compressor in real time, the test pressure scope of this pressure-sensitive explosion test device is normal pressure ~ 3MPa, Range of measuring temp is normal temperature ~ 200 DEG C.
The pressure-sensitive explosion test device shown in Fig. 1 of the present invention is adopted pressure sensibility gas to be issued to the method for the emergent pressure scope of raw decomposition explosion in the condition not having oxygen to participate in, experiment start before first with nitrogen to described Detonation Tube, described compressor 10 and described autoclave 5 rinse, then vacuumize for subsequent use with vacuum pump 8, pressure sensibility gas to be tested is sent in Detonation Tube and carries out preheating, preheated pressure sensibility gas to be tested enters into the air intake opening of described compressor 10 by connecting line, described pressure sensibility gas to be tested carries out two stages of compression in described compressor, first the pressure in described compressor is risen to 0.5MPa through one stage of compression part 1 by normal pressure, 3MPa is being risen to by 0.5MPa through two-stage compression part 2, opening pressure record during gas compression, pressure data is presented on Computer Control Unit 9 in real time, if gas does not react under set pressure condition, pressure curve slope is 0, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure, for the transient pressure susceptibility gas not recording critical decomposition pressure, after it is compressed by described compressor 10, pass into the autoclave after vacuumizing 5 airtight, autoclave temp setting is identical with working temperature, gas is every 8 hours chromatograph instrument gas phase composition, judge that gas decomposes situation.
Example: test methyl nitrite at 80 DEG C, the stability under pressure 2MPa condition.
Changing 15 rupture disks before experiment starts is the rupture disk of 2MPa, once methyl nitrite decomposition pressure is more than 2MPa in compression process, rupture disk breaks, and methyl nitrite gas is by outside rupture disk discharge chamber.
Vacuumize with Detonation Tube vacuum pump 1A and compressor vacuum pump 8 pairs of devices before experiment starts.
By methyl nitrite steel cylinder access Detonation Tube air inlet gas cylinder mouth, methyl nitrite gas is by 4A needle-valve, and 5A retaining valve and 6A needle-valve enter Detonation Tube, and pressure value is shown by 12A tensimeter, and pouring sub-ester gaseous tension is normal pressure.
Close 6A needle-valve, 9A to 80 DEG C, opening temp. control device, open 10A circulating fan, prepare to open 13A at 80 DEG C after one hour until temperature stabilization and enter compressor valve.
Unlatching Detonation Tube and compressor pipeline accompany heat to 80 DEG C, open compressor jacket temperature to 80 DEG C, prepare compression after temperature stabilization.
Open compressor, open 13A and enter compressor valve, methyl nitrite gas enters 10 compressors from Detonation Tube, 2 compressor two-stage compressions are entered after 1 compressor one stage of compression, by 11 temperature sensor 12 temperature sensor records on computers, after the compression of compressor I and II, pressure by 3 tensimeter 4 tensimeter records on computers for compressor I and II compression chamber temperature.
Real Time Observation pressure curve changes, the close compressor when autoclave pressure is 2MPa, opens gas chromatography and analyzes gas sample.Known methyl nitrite is at 80 DEG C by analysis, does not decompose under pressure 2MPa condition.
To the every 8 hours chromatographs of methyl nitrite gas in autoclave gas phase composition, judge that gas decomposes situation, draw the resolving time.
All above-mentioned this intellecture properties of primary enforcement, not setting restriction this new product of other forms of enforcement and/or new method.Those skilled in the art will utilize this important information, and foregoing is revised, to realize similar implementation status.But all modifications or transformation belong to the right of reservation based on new product of the present invention.
The above is only preferred embodiment of the present invention, and be not restriction the present invention being made to other form, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But everyly do not depart from technical solution of the present invention content, any simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.

Claims (8)

1. the method adopting pressure-sensitive explosion test device to test emergent pressure scope pressure sensibility gas being issued to raw decomposition explosion in the condition not having oxygen to participate in, it is characterized in that described pressure-sensitive explosion test device comprises compressor, Detonation Tube, autoclave, pressure-detecting device, temperature-detecting device, vacuum pump, chromatograph and Computer Control Unit, described temperature-detecting device is positioned on described Detonation Tube, described Detonation Tube is connected by pipeline with described compressor, described pressure-detecting device is positioned on described compressor, described vacuum pump is connected with described compressor, described chromatograph is also connected with described compressor, comprise:
The first step, vacuumizes;
Second step, to pressure sensibility air preheat to be tested;
3rd step, to pressure sensibility gas compression to be tested, measure it issues raw decomposition explosion emergent pressure scope in the condition not having oxygen to participate in, be specially described pressure sensibility gas to be tested and carry out two stages of compression in described compressor, first the pressure in described compressor is risen to 0.5MPa through one stage of compression by normal pressure, 3MPa is risen to by 0.5MPa again through two-stage compression, opening pressure record during gas compression, pressure data is presented on Computer Control Unit in real time, if gas does not react under set pressure condition, pressure curve slope is 0, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure.
2. the method for claim 1, is characterized in that: the described first step is specially further before experiment starts and first rinses described Detonation Tube, described compressor and described autoclave with nitrogen, then uses vacuum pump evacuation for subsequent use.
3. the method for claim 1, it is characterized in that: described second step is specially further and carries out preheating by pressure sensibility gas to be tested feeding Detonation Tube, temperature required under obtaining high temperature and high pressure condition condition, preheated pressure sensibility gas to be tested enters into the air intake opening of described compressor by connecting line.
4. the method adopting pressure-sensitive explosion test device to test emergent pressure scope pressure sensibility gas being issued to raw decomposition explosion in the condition not having oxygen to participate in, described pressure-sensitive explosion test device comprises compressor, Detonation Tube, autoclave, pressure-detecting device, temperature-detecting device, vacuum pump, chromatograph and Computer Control Unit, described temperature-detecting device is positioned on described Detonation Tube, described Detonation Tube is connected by pipeline with described compressor, described pressure-detecting device is positioned on described compressor, described autoclave is connected with described compressor, described vacuum pump is connected with described autoclave, described chromatograph is connected with described autoclave with described compressor, it is characterized in that, described method comprises:
The first step, vacuumizes;
Second step, to pressure sensibility air preheat to be tested;
3rd step, to pressure sensibility gas compression to be tested, measure it issues raw decomposition explosion emergent pressure scope in the condition not having oxygen to participate in, be specially described pressure sensibility gas to be tested and carry out two stages of compression in described compressor, first the pressure in described compressor is risen to 0.5MPa through one stage of compression by normal pressure, 3MPa is risen to by 0.5MPa again through two-stage compression, opening pressure record during gas compression, pressure data is presented on Computer Control Unit in real time, if gas does not react under set pressure condition, pressure curve slope is 0, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure,
4th step, for the transient pressure susceptibility gas not recording critical decomposition pressure, after it is compressed by described compressor, pass into the autoclave after vacuumizing airtight, autoclave temp setting is identical with working temperature, gas is chromatograph instrument gas phase composition at set intervals, judges that gas decomposes situation.
5. method as claimed in claim 4, is characterized in that: the described first step is specially further before experiment starts and first rinses described Detonation Tube, described compressor and described autoclave with nitrogen, then uses vacuum pump evacuation for subsequent use.
6. method as claimed in claim 4, it is characterized in that: described second step is specially further and carries out preheating by pressure sensibility gas to be tested feeding Detonation Tube, temperature required under obtaining high temperature and high pressure condition condition, preheated pressure sensibility gas to be tested enters into the air intake opening of described compressor by connecting line.
7. the method adopting pressure-sensitive explosion test device to test emergent pressure scope pressure sensibility gas being issued to raw decomposition explosion in the condition not having oxygen to participate in, described pressure-sensitive explosion test device comprises compressor, Detonation Tube, autoclave, pressure-detecting device, temperature-detecting device, vacuum pump, chromatograph and Computer Control Unit, described temperature-detecting device is positioned on described Detonation Tube, described Detonation Tube is connected by pipeline with described compressor, described pressure-detecting device is positioned on described compressor, described autoclave is connected with described compressor, described vacuum pump is connected with described autoclave, described chromatograph is connected with described autoclave with described compressor, it is characterized in that, described method comprises:
The first step, first rinses described Detonation Tube, described compressor and described autoclave with nitrogen before experiment starts, then uses vacuum pump evacuation for subsequent use;
Second step, sent in Detonation Tube by pressure sensibility gas to be tested and carry out preheating, preheated pressure sensibility gas to be tested enters into the air intake opening of described compressor by connecting line;
3rd step, described pressure sensibility gas to be tested carries out two stages of compression in described compressor, first the pressure in described compressor is risen to 0.5MPa through one stage of compression by normal pressure, 3MPa is being risen to by 0.5MPa through two-stage compression, opening pressure record during gas compression, pressure data is presented on Computer Control Unit in real time, if gas does not react under set pressure condition, pressure curve slope is 0, if gas there occurs decomposition reaction, pressure curve slope can change to some extent, recording curve flex point pressure, stop pressure gas, chromatograph gas phase forms, judge that whether this force value is the critical decomposition pressure of this gas, if gas composition does not change, illustrate that gas decomposition explosion does not occur, continue pressure gas until find critical decomposition pressure,
4th step, for the transient pressure susceptibility gas not recording critical decomposition pressure, after it is compressed by described compressor, pass into the autoclave after vacuumizing airtight, autoclave temp setting is identical with working temperature, gas is chromatograph instrument gas phase composition at set intervals, judges that gas decomposes situation.
8. described in any one of claim 1 to 7, pressure sensibility gas is issued to the application of method in petrochemical complex safety in production of the emergent pressure scope of raw decomposition explosion in the condition not having oxygen to participate in.
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