CN101968457B - Explosion danger testing device for gas-phase reaction system and using method thereof - Google Patents

Explosion danger testing device for gas-phase reaction system and using method thereof Download PDF

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CN101968457B
CN101968457B CN 201010280536 CN201010280536A CN101968457B CN 101968457 B CN101968457 B CN 101968457B CN 201010280536 CN201010280536 CN 201010280536 CN 201010280536 A CN201010280536 A CN 201010280536A CN 101968457 B CN101968457 B CN 101968457B
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gas
reactor
phase
pressure
oxygen content
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CN101968457A (en
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谢传欣
孙峰
石宁
黄飞
王振刚
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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 discloses an explosion danger testing device for a gas-phase reaction system and a using method thereof. The device comprises a gas-phase feeding system, a reaction kettle, a high-pressure ignition system and a dynamic pressure collection system, wherein the gas-phase feeding system is connected with the reaction kettle, and is used for feeding a raw gas to be tested into the reaction kettle; the high-pressure ignition system is arranged on the reaction kettle, and is used for igniting the reaction kettle; and the dynamic pressure collection system is arranged on the reaction kettle, and is used for dynamically testing pressure in the reaction kettle in real time. The device of the invention can observe and study gas-phase explosion dangers by forcible ignition, and collect real-time data to observe and study gas-phase oxygen content controllability under different conditions so as to test the explosion dangers in gas-phase reaction by gas-phase ignition experiments.

Description

A kind of gas-phase reaction system fires the using method of dangerous proving installation
Technical field
The present invention relates to the petrochemical technology field, particularly a kind of gas-phase reaction system fires dangerous proving installation and using method thereof.
Background technology
In petrochemical industry, such class reaction is arranged, the gas phase organism generation target product that reacts to each other, wherein gaseous oxidizing agent can be air, oxygen rich gas, oxygen etc., the following safety problem of this class reaction ubiquity: 1, when gas speed is too fast, may blast; Under the static ignition condition, may blast and the forming energy propagation; 2, because reaction conditions control is improper, cause reaction not carried out as scheduled, oxygenant enters gas phase, and unreacted enters the oxygenant of gas phase fully and the organism mixing of gas phase causes having gas phase to fire risk.
At present, the optimum process condition of the main just reaction of researcher and mechanism etc. are studied, and lack the concern to secure context, and the test of explosion limits and providing of critical dissolved oxygen content are also be provided in the research of secure context on a small quantity.Along with domestic concern to secure context, for the dangerous characteristics of gas phase oxidation, investigates by positive ignition that gas phase fires danger, when gathering real time data investigation different condition, gas phase oxygen content controllability etc. becomes the trouble free service person furthers investigate the work that gas phase oxidation danger must be carried out.
Summary of the invention
Technical matters to be solved by this invention is, provides a kind of gas-phase reaction system to fire dangerous proving installation and using method thereof.Reactor, high-voltage ignition device, dynamic pressure harvester, tail oxygen content detector that apparatus of the present invention are equipped with can be simulated the gas-phase reaction condition, observation changes the variation of gas phase ability to take oxygen with reaction conditions, by the igniting experiments in gas phase, the test gas-phase reaction fires danger.
For solving the problems of the technologies described above, the invention provides a kind of gas-phase reaction system and fire dangerous proving installation, comprising: gas-phase feed system, reactor, high-tension ignition system and dynamic pressure acquisition system.
Described gas-phase feed system is connected with described reactor, is used for input unstrpped gas to be tested in the reactor;
Described high-tension ignition system is arranged on described reactor, is used to described reactor igniting;
Described dynamic pressure acquisition system is arranged on described reactor, is used for the pressure in the described reactor of real-time dynamic test.
Described device can go on foot and comprise tail oxygen content detector; Described tail oxygen content detector is for detection of the tail gas oxygen content, thus the ability to take oxygen of judgement gas phase.
Described reactor preferably is provided with safety valve, rupture disk, stirrer, cooling coil and electrical heating chuck.
Gaseous phase outlet place, described reactor upper end preferably is provided with gas-liquid separator and water trap.
Described device preferably further is provided with temperature-controlling system and voltage-regulating system;
Described temperature-controlling system is connected with described reactor, is used for controlling the temperature of reaction in described reactor;
Described voltage-regulating system is connected with described reactor, is used for controlling the reaction pressure in described reactor.
Described reactor maximum operation (service) temperature is preferably 200 ℃, and maximum operating pressure is preferably 3MPa.
Can be provided with view window on the still wall of described reactor, be used for firing and the flame propagation situation in the observation still;
In described reactor, the liquid level of gas-phase reaction generation solution is controlled automatically by pneumatic valve.
For solving the problems of the technologies described above, the present invention also provides a kind of gas-phase reaction system to fire the using method of dangerous proving installation, comprises the following steps:
A. start the gas-phase feed system to reactor air inlet phase raw material, stop charging when setting volume when charging reaches;
B. pass through temperature-controlling system conditioned reaction still temperature to design temperature;
C. pass through voltage-regulating system conditioned reaction still pressure to set pressure;
D. pass into setting gas, regulate voltage-regulating system and make reactor pressure maintain set pressure;
E. repeating step a~d, realize the gaseous phase materials circulation;
F. detect the tail gas oxygen content by tail oxygen content detector, thus the ability to take oxygen of judgement gas phase; By dynamic pressure data after fighting the collection point fire at reactor differing heights point, the judgement gas-phase reaction system fires danger.
Described step f can also for: tail oxygen content detector is measured the tail gas oxygen content, and reads by control panel, the transformationreation condition, fire trial is repeatedly carried out in the differing heights position in reactor; Adopt its blasting process of video camera Taking Pictures recording, pressure and time data, by charge amplifier, data collecting card is sent on PC.
Apparatus of the present invention can investigate by positive ignition that gas phase fires danger, gas phase oxygen content controllability when gathering real time data and investigating different condition, and by the igniting experiments in gas phase, the test gas-phase reaction fires danger.
Description of drawings
Fig. 1 is that the described gas-phase reaction system of the embodiment of the present invention fires dangerous proving installation schematic diagram.
Embodiment
Describe embodiments of the present invention in detail below with reference to drawings and Examples, how the application technology means solve technical matters to the present invention whereby, and the implementation procedure of reaching technique effect can fully understand and implement according to this.
As shown in Figure 1, fire dangerous proving installation schematic diagram for the described gas-phase reaction system of the embodiment of the present invention.Wherein, the title of all parts is respectively: 1, oxygen tank, 2, nitrogen pot, 3, head tank, 4, gas distributor, 5, oxygen analyzer, 6, igniter head, 7, reactor, 8, gas-liquid separator, 9, oxygen analyzer, 10, water trap, 11, observation window, 12, dynamic pressure transducer, 13, the rewinding tank.
In one embodiment of the invention, device mainly is comprised of gas-phase feed system, reactor, high-tension ignition and dynamic pressure acquisition system, tail oxygen content detector etc.; Reactor is furnished with safety valve, rupture disk, stirrer, cooling coil, electrical heating chuck etc., gaseous phase outlet place, still upper end is furnished with gas-liquid separator and water trap, the still wall is furnished with glass window, fire in the Observable still and the flame propagation situation, the reactor liquid level is controlled automatically by pneumatic valve, 200 ℃ of reactor maximum operation (service) temperatures, maximum operating pressure 3MPa.Control temperature of reaction kettle and pressure well by temperature-controlling system and tail gas counterbalance valve, the gas for preparing enters reactor by reactor bottom gas distributor and participates in reaction, can detect the tail gas oxygen content by tail oxygen content detector, thus the ability to take oxygen of judgement gas phase; By dynamic pressure data after fighting the collection point fire at reactor differing heights point, the judgement gas-phase reaction system fires danger.
In another embodiment of the present invention, the using method of device is:
1, gaseous phase materials is added head tank, start feeder pump to the reactor charging, stop charging when reactor reaches designated volume;
2, by temperature-controlling system conditioned reaction still temperature to assigned temperature, by voltage-regulating system conditioned reaction still pressure to specified pressure;
3, pass into designated gas, regulate counterbalance valve and make reactor pressure maintain specified pressure;
4, can start the gaseous phase materials feeder pump to the reactor charging, automatically regulate discharging to control stable gas pressure by pneumatic valve, realize the gaseous phase materials circulation;
5, the tail gas oxygen content can be measured and be read by control panel by tail oxygen content detector, the high-tension ignition test is carried out in the various conditions of conversion differing heights position in still, its blasting process of video camera Taking Pictures recording, the data such as pressure are by charge amplifier, and data collecting cards etc. are sent on PC.
In yet another embodiment of the invention, device comprises: gas-phase feed system, reactor, high-tension ignition system and dynamic pressure acquisition system.
Described gas-phase feed system is connected with described reactor, is used for input unstrpped gas to be tested in the reactor;
Described high-tension ignition system is arranged on described reactor, is used to described reactor igniting;
Described dynamic pressure acquisition system is arranged on described reactor, is used for the pressure in the described reactor of real-time dynamic test.
Described device can go on foot and comprise tail oxygen content detector; Described tail oxygen content detector is for detection of the tail gas oxygen content, thus the ability to take oxygen of judgement gas phase.
Described reactor preferably is provided with safety valve, rupture disk, stirrer, cooling coil and electrical heating chuck.
Gaseous phase outlet place, described reactor upper end preferably is provided with gas-liquid separator and water trap.
Described device preferably further is provided with temperature-controlling system and voltage-regulating system;
Described temperature-controlling system is connected with described reactor, is used for controlling the temperature of reaction in described reactor;
Described voltage-regulating system is connected with described reactor, is used for controlling the reaction pressure in described reactor.
Described reactor maximum operation (service) temperature is preferably 200 ℃, and maximum operating pressure is preferably 3MPa.
Can be provided with view window on the still wall of described reactor, be used for firing and the flame propagation situation in the observation still;
In described reactor, the liquid level of gas-phase reaction generation solution is controlled automatically by pneumatic valve.
In another embodiment of the present invention, also provide a kind of gas-phase reaction system to fire the using method of dangerous proving installation, comprised the following steps:
A. start the gas-phase feed system to reactor air inlet phase raw material, stop charging when setting volume when charging reaches;
B. pass through temperature-controlling system conditioned reaction still temperature to design temperature;
C. pass through voltage-regulating system conditioned reaction still pressure to set pressure;
D. pass into setting gas, regulate voltage-regulating system and make reactor pressure maintain set pressure;
E. repeating step a~d, realize the gaseous phase materials circulation;
F. detect the tail gas oxygen content by tail oxygen content detector, thus the ability to take oxygen of judgement gas phase; By dynamic pressure data after fighting the collection point fire at reactor differing heights point, the judgement gas-phase reaction system fires danger.
Described step f can also for: tail oxygen content detector is measured the tail gas oxygen content, and reads by control panel, the transformationreation condition, fire trial is repeatedly carried out in the differing heights position in reactor; Adopt its blasting process of video camera Taking Pictures recording, pressure and time data, by charge amplifier, data collecting card is sent on PC.
In embodiment of the present invention cyclohexane non-catalyst oxidation preparing cyclohexanone device, oxide isolation is oxygen-enriched air, this system take oxygen-enriched air as oxide isolation can cause the reactor gas phase to fire dangerous increasing, and the explosive characteristic of therefore studying cyclohexane-oxygen under process conditions-nitrogen systems is very valuable, significant.
With apparatus of the present invention, pimelinketone device reactor gas phase cyclohexane-oxygen-nitrogen systems explosive characteristic is studied.Experimental procedure is as follows:
A. before advancing raw material, logical nitrogen replacement system;
B. advance cyclohexane to reactor and specify liquid level;
C. passing into nitrogen to pressure is the 1MPa left and right, opens heating, and controlling temperature in the kettle is 160 ℃ of left and right, and makes the still internal gas pressure be stabilized in the 1MPa left and right;
D. pass into the gas of different oxygen (20.9%, 30%, 40%) by the reactor bottom gas distributor;
E. press feeder pump pushbutton enable feeder pump to reactor feed, control discharging by the bottoms level variable valve.
F. can record the tail oxygen content by the tail oxygen conten analyser, thus the judgement reaction process;
G. pass into the gas that flow is 4L/min, the various conditions of conversion gas phase in still is utilized high-tension ignition, and pressure data is by charge amplifier, and data collecting card etc. are sent on PC.
Acquired results is as follows:
Table 1 cyclohexane-oxygen-nitrogen systems explosive characteristic result of study
Figure BSA00000268006800061
As can be seen from Table 1:
A. under the pimelinketone device working condition (1MPa, 155 ℃), the ventilation oxygen content is lower than 30% the time, and the reactor gas phase does not fire danger;
If when fluctuation of operating conditions b., temperature reduced and pressure raises, gas phase fired dangerous increasing, the ventilation oxygen content also may fire danger when being 30%;
If c. fluctuation of operating conditions, when temperature raises, also fire danger without gas phase even lead to 40% oxygen rich gas;
D. logical which kind of gas no matter, if with the tail Control for Oxygen Content below 20%, the reactor gas phase is just without dangerous under the nominal situation condition;
E., the quick-fried danger of sudden strain of a muscle when passing into air, the cyclohexane liquid phase is arranged under normal temperature and pressure.
By above research, grasp rule and condition that reactor gas phase cyclohexane-oxygen-nitrogen systems may fire, thereby can take corresponding measure, prevent that effectively pimelinketone device reactor generation gas phase from firing danger.
The above is only preferred embodiment of the present invention, is not to be the present invention to be done the restriction of other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away from according to any simple modification, equivalent variations and the remodeling that technical spirit of the present invention is done above example, still belongs to the protection domain of technical solution of the present invention.
All are above-mentioned is primary device for carrying out said and/or the method for this intellecture property, does not set restriction and implements this new device and/or method with other form.Those skilled in the art will utilize this important information, foregoing be revised, to realize similar implementation status.But all belong to the right of reservation based on modification of the present invention or transformation new product and/or method.

Claims (2)

1. a gas-phase reaction system fires the using method of dangerous proving installation, it is characterized in that,
Described gas-phase reaction system fires dangerous proving installation, comprising: gas-phase feed system, reactor, high-tension ignition system and dynamic pressure acquisition system;
Described gas-phase feed system is connected with described reactor, is used for input unstrpped gas to be tested in the reactor;
Described high-tension ignition system is arranged on described reactor, is used to described reactor igniting;
Described dynamic pressure acquisition system is arranged on described reactor, is used for the pressure in the described reactor of real-time dynamic test;
Described device further comprises tail oxygen content detector; Described tail oxygen content detector is for detection of the tail gas oxygen content, thus the ability to take oxygen of judgement gas phase;
Described reactor is provided with safety valve, rupture disk, stirrer, cooling coil and electrical heating chuck;
Gaseous phase outlet place, described reactor upper end is provided with gas-liquid separator and water trap;
Described device further is provided with temperature-controlling system and voltage-regulating system;
Described temperature-controlling system is connected with described reactor, is used for controlling the temperature of reaction in described reactor;
Described voltage-regulating system is connected with described reactor, is used for controlling the reaction pressure in described reactor;
The using method that described gas-phase reaction system fires dangerous proving installation comprises the following steps:
A. start the gas-phase feed system to reactor air inlet phase raw material, stop charging when setting volume when charging reaches;
B. pass through temperature-controlling system conditioned reaction still temperature to design temperature;
C. pass through voltage-regulating system conditioned reaction still pressure to set pressure;
D. pass into setting gas, regulate voltage-regulating system and make reactor pressure maintain set pressure;
E. repeating step a ~ d, realize the gaseous phase materials circulation;
F. detect the tail gas oxygen content by tail oxygen content detector, thus the ability to take oxygen of judgement gas phase; By dynamic pressure data after fighting the collection point fire at reactor differing heights point, the judgement gas-phase reaction system fires danger.
2. using method according to claim 1, is characterized in that, described step f is: tail oxygen content detector is measured the tail gas oxygen content, and reads by control panel, the transformationreation condition, and fire trial is repeatedly carried out in the differing heights position in reactor; Adopt its blasting process of video camera Taking Pictures recording, pressure and time data, by charge amplifier, data collecting card is sent on PC.
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