CN107219256B - Method for evaluating safe operation boundary of reaction temperature of oxidation reactor - Google Patents
Method for evaluating safe operation boundary of reaction temperature of oxidation reactor Download PDFInfo
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- CN107219256B CN107219256B CN201610165005.9A CN201610165005A CN107219256B CN 107219256 B CN107219256 B CN 107219256B CN 201610165005 A CN201610165005 A CN 201610165005A CN 107219256 B CN107219256 B CN 107219256B
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 30
- 230000003647 oxidation Effects 0.000 title claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 44
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000001301 oxygen Substances 0.000 claims abstract description 35
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 35
- 238000004880 explosion Methods 0.000 claims abstract description 15
- 239000000945 filler Substances 0.000 claims abstract description 10
- 239000003063 flame retardant Substances 0.000 claims abstract description 10
- 238000011156 evaluation Methods 0.000 claims abstract description 7
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- 229920005830 Polyurethane Foam Polymers 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 239000011496 polyurethane foam Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/50—Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility
- G01N25/54—Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility by determining explosibility
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention relates to an evaluation method for a safe operation boundary of reaction temperature of an oxidation reactor, which mainly solves the problem that the explosion danger of the oxidation reactor cannot be effectively detected in the prior art. The invention adopts a technical scheme that the method comprises an oxygen mixer, a reactor with temperature control and a vacuum pump, an oxygen pipeline and a combustible gas pipeline are respectively connected with the oxygen mixer, fire-retardant and explosion-proof filler is filled in the oxygen mixer, an outlet of the oxygen mixer is divided into two paths, the first path is connected with an inlet of a metering pump, the second path is connected with an outlet of the reactor with temperature control, an outlet of the metering pump is connected with an inlet of the reactor with temperature control, the reactor with temperature control is provided with a safety valve, a rupture disk and at least one thermocouple, the thermocouple is connected with a computer, and the vacuum pump is connected with the outlet of the reactor with temperature control.
Description
Technical Field
The invention relates to an evaluation method of a safe operation boundary of reaction temperature of an oxidation reactor.
Background
The oxidation reaction is an exothermic dangerous chemical reaction, and when the temperature, the material residence time, the oxygen concentration and the initial pressure of the reactor are not well controlled in the reaction process of combustible gas and oxygen in the oxidizer, complete oxidation (namely combustion) is likely to occur, so that the temperature runaway of the reactor is caused, and further, a combustion explosion accident occurs.
CN201510185390.9 relates to a survey device of gas phase blasting characteristic in the reaction process, including reactor, ignition head, temperature and pressure sensor, feed system, temperature and pressure acquisition system, ignition control system and extrinsic cycle heat extraction system.
The existing detection means cannot meet the requirements of working conditions, the design of key parameters of the oxidation reactor can only be estimated through simulation means and thermodynamic calculation, and the existing simulation means cannot accurately obtain the key parameters due to the fact that four changes of 'three-pass-one-reverse' are involved in the oxidation reactor.
The invention solves the problem in a targeted way.
Disclosure of Invention
The invention aims to solve the technical problem that the explosion danger of an oxidation reactor cannot be effectively detected in the prior art, and provides a novel evaluation method for the safe operation boundary of the reaction temperature of the oxidation reactor. The method is used for evaluating the safe operation boundary of the reaction temperature of the oxidation reactor, and has the advantages of effectively detecting the explosion danger of the oxidation reactor and providing data.
In order to solve the problems, the technical scheme adopted by the invention is as follows: a method for evaluating the safe operation boundary of the reaction temperature of an oxidation reactor comprises the following steps of evaluating the reaction temperature on an evaluation device of the oxidation reactor, uniformly mixing oxygen and combustible gas in an oxygen mixer, feeding the mixture into a reactor with temperature control through a metering pump, installing a thermocouple on the reactor, transmitting a temperature signal to a computer by the thermocouple, judging whether the mixed combustible gas is combusted or not by the computer according to the temperature change condition, opening a safety valve or a rupture disk once the gas is combusted and exploded, and discharging tail gas out of a room through a tail gas discharge pipe; if the explosion does not occur, the mixed combustible gas returns to the inlet of the metering pump, if the pressure of the mixed combustible gas does not reach the preset pressure, the mixed combustible gas is continuously injected into the metering pump, and the mixed combustible gas is circulated for many times until the explosion occurs, and various states of the mixed combustible gas during the explosion occur are recorded, so that the safety critical parameters of the oxidation reaction are obtained; the oxidation reactor evaluation device comprises an oxygen mixer, a reactor with temperature control and a vacuum pump, wherein an oxygen pipeline and a combustible gas pipeline are respectively connected with the oxygen mixer, fire-retardant and explosion-proof filler is filled in the oxygen mixer, an outlet of the oxygen mixer is divided into two paths, the first path is connected with an inlet of a metering pump, the second path is connected with an outlet of the reactor with temperature control, an outlet of the metering pump is connected with an inlet of the reactor with temperature control, a safety valve, a rupture disk and at least one thermocouple are arranged on the reactor with temperature control, the thermocouple is connected with a computer, and the vacuum pump is connected with an outlet of the reactor with temperature control.
In the above technical solution, preferably, the outlet of the oxygen mixer is divided into two paths after passing through a back pressure valve and a check valve, the first path is connected with the inlet of the metering pump, and the second path is connected with the outlet of the reactor with temperature control after passing through the check valve.
In the above technical solution, preferably, the safety valve and the outlet of the rupture disk are both connected to a tail gas exhaust pipeline.
In the above technical solution, preferably, a valve is disposed on a pipeline connecting the vacuum pump and the temperature-controlled reactor.
In the above technical scheme, preferably, the fire-retardant and explosion-proof filler is a porous spherical non-metallic organic material.
In the above technical solution, more preferably, the porous spherical non-metallic organic material is a polyurethane foam sponge or a polyether porous sphere.
This patent surveys the safe critical value of reactor temperature to the explosive danger that exists in the oxidation reaction reactor through testing conditions such as different material dwell time, oxygen concentration and initial pressure, provides the basis for the oxidation reaction formulates the reaction condition, has obtained better technological effect.
Drawings
FIG. 1 is a schematic view of the structure of the device of the present invention.
In fig. 1, 1 oxygen line; 2 combustible gas pipeline; 3 fire-retardant and explosion-proof filler; 4, oxygen mixing device; 5a back pressure valve; 5b a valve; 6a/b check valve; 7a metering pump; 7b a vacuum pump; 8, a computer; 9, a reactor with temperature control; 10 thermocouple; 11 a safety valve; 12 rupture discs; 13 tail gas discharge pipe.
The present invention will be further illustrated by the following examples, but is not limited to these examples.
Detailed Description
[ example 1 ]
An assessment method of a safe operation boundary of reaction temperature of an oxidation reactor is carried out on an assessment device of the oxidation reactor, as shown in figure 1, the assessment device of the oxidation reactor comprises an oxygen mixer, a reactor with temperature control and a vacuum pump, an oxygen pipeline and a combustible gas pipeline are respectively connected with the oxygen mixer, fire-retardant and explosion-proof filler and porous spherical non-metallic organic material of the fire-retardant and explosion-proof filler are filled in the oxygen mixer. The outlet of the oxygen mixer is divided into two paths, the first path is connected with the inlet of the metering pump, the second path is connected with the outlet of the reactor with temperature control, the outlet of the metering pump is connected with the inlet of the reactor with temperature control, the reactor with temperature control is provided with a safety valve, a rupture disk and a thermocouple, the thermocouple is connected with a computer, and the vacuum pump is connected with the outlet of the reactor with temperature control.
After oxygen and combustible gas are uniformly mixed in an oxygen mixer, the oxygen and the combustible gas enter a metering pump through a back pressure valve 6a and a one-way valve, the metering pump flushes the mixed gas into a reactor with temperature control, thermocouples are uniformly arranged on the reactor at intervals, the total number of the thermocouples is 6, the thermocouples transmit temperature signals to a computer, the computer judges whether the mixed combustible gas is combusted or not according to the temperature change condition, once the gas is combusted and exploded, a safety valve or a rupture disk acts, and tail gas is discharged out of a room through a tail gas discharge pipe; if the mixed combustible gas is not exploded, the mixed combustible gas returns to the metering pump through the one-way valve 6b to be circulated, if the pressure of the mixed combustible gas does not reach the preset pressure, the mixed combustible gas is continuously injected into the metering pump through the back pressure valve, and after the mixed combustible gas is circulated for many times until the mixed combustible gas is exploded, various states of the mixed combustible gas during explosion are recorded, so that the safety critical parameters of the oxidation reaction are obtained.
In addition, before the device samples, a vacuum pump needs to be started to vacuumize the system, and a valve is arranged on a pipeline connecting the vacuum pump and the reactor.
Take a reactor for preparing ethylene oxide by partial oxidation of ethylene as an example.
The ethylene concentration, material residence time and initial pressure were fixed and the safe operating boundaries for reaction temperature were investigated.
The operation method comprises the following steps:
1. starting a vacuum pump and a valve 5b to vacuumize the system;
2. introducing ethylene and oxygen in proportion;
3. adjusting the back pressure valve to a target pressure;
4. setting the reactor to a reaction temperature;
5. adjusting the metering pump to a proper flow rate;
6. recording the temperature rise change condition after circulation, if no explosion occurs, discharging tail gas, cleaning the system, raising the temperature of the reactor, and repeating the steps 1-6 until explosion occurs;
7. the reaction temperature at which the detonation occurred was recorded.
Through industrial amplification, reference basis can be provided for the design of an industrial oxidation reactor.
[ example 2 ]
According to the conditions and the steps described in the example 1, the total number of the thermocouples is 2, and the fire-retardant and explosion-proof filler is polyurethane foam sponge, so that the burning and explosion risks of the oxidation reactor can be effectively detected and design data can be provided.
[ example 3 ]
According to the conditions and the steps described in the example 1, only 8 thermocouples are used in total, and the fire-retardant and explosion-proof filler is a polyether type porous ball, so that the explosion risk of the oxidation reactor can be effectively detected and design data can be provided.
Claims (1)
1. A method for evaluating the safe operation boundary of the reaction temperature of an oxidation reactor comprises the steps of evaluating the safe operation boundary of the reaction temperature on an evaluation device of the oxidation reactor, uniformly mixing oxygen and combustible gas in an oxygen mixer, then feeding the mixture into the reactor with temperature control through a metering pump, mounting a thermocouple on the reactor, transmitting a temperature signal to a computer by the thermocouple, judging whether the mixed combustible gas is combusted or not by the computer according to the temperature change condition, opening a safety valve or a rupture disk once the gas is combusted and exploded, and discharging tail gas out of the room through a tail gas discharge pipe; if the explosion does not occur, the mixed combustible gas returns to the inlet of the metering pump, if the pressure of the mixed combustible gas does not reach the preset pressure, the mixed combustible gas is continuously injected into the metering pump, and the mixed combustible gas is circulated for many times until the explosion occurs, and the reaction temperature of the explosion occurs is recorded; the oxidation reactor evaluation device comprises an oxygen mixer, a reactor with temperature control and a vacuum pump, wherein an oxygen pipeline and a combustible gas pipeline are respectively connected with the oxygen mixer, fire-retardant and explosion-proof filler is filled in the oxygen mixer, an outlet of the oxygen mixer is divided into two paths, the first path is connected with an inlet of a metering pump, the second path is connected with an outlet of the reactor with temperature control, an outlet of the metering pump is connected with an inlet of the reactor with temperature control, the reactor with temperature control is provided with a safety valve, a rupture disk and at least one thermocouple, the thermocouple is connected with a computer, and the vacuum pump is connected with an outlet of the reactor with temperature control; the safety valve and the outlet of the rupture disk are connected with a tail gas discharge pipeline; a valve is arranged on a pipeline connecting the vacuum pump and the reactor with the temperature control function; the thermocouples are uniformly arranged along the axial direction of the reactor with temperature control; the fire-retardant and explosion-proof filler is porous spherical polyurethane foam sponge or polyether porous balls; the outlet of the oxygen mixer is divided into two paths after passing through a back pressure valve and a one-way valve, the first path is connected with the inlet of a metering pump, and the second path is connected with the outlet of a reactor with temperature control after passing through the one-way valve.
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| CN201610165005.9A CN107219256B (en) | 2016-03-22 | 2016-03-22 | Method for evaluating safe operation boundary of reaction temperature of oxidation reactor |
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| CN201610165005.9A CN107219256B (en) | 2016-03-22 | 2016-03-22 | Method for evaluating safe operation boundary of reaction temperature of oxidation reactor |
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|---|---|---|---|---|
| JPH08145921A (en) * | 1994-11-18 | 1996-06-07 | Lion Corp | Measuring equipment of flammability limits |
| CN102369591A (en) * | 2009-04-03 | 2012-03-07 | 中央硝子株式会社 | System for in-situ mixing and diluting fluorine gas |
| CN101968457A (en) * | 2010-09-14 | 2011-02-09 | 中国石油化工股份有限公司 | Explosion danger testing device for gas-phase reaction system and using method thereof |
| CN102558831A (en) * | 2011-10-22 | 2012-07-11 | 上海华篷防爆科技有限公司 | Organic barrier and explosion-proof material and preparation method for same |
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Effective date of registration: 20211220 Address after: Yanan City, Shandong province Qingdao City three road 266071 No. 218 Applicant after: CHINA PETROLEUM & CHEMICAL Corp. Applicant after: Sinopec Safety Engineering Research Institute Co., Ltd Address before: Yanan City, Shandong province Qingdao City three road 266071 No. 218 Applicant before: CHINA PETROLEUM & CHEMICAL Corp. Applicant before: Qingdao Safety Engineering Research Institute of Sinopec |
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