CN107219253B - Method for evaluating safety operation boundary of residence time of oxidation reactor - Google Patents
Method for evaluating safety operation boundary of residence time of oxidation reactor Download PDFInfo
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- CN107219253B CN107219253B CN201610163830.5A CN201610163830A CN107219253B CN 107219253 B CN107219253 B CN 107219253B CN 201610163830 A CN201610163830 A CN 201610163830A CN 107219253 B CN107219253 B CN 107219253B
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 30
- 230000003647 oxidation Effects 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 43
- 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 16
- 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 3
- 239000000463 material Substances 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- 229920005830 Polyurethane Foam Polymers 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 239000011496 polyurethane foam Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 description 7
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene 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
- 238000007599 discharging Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000000203 mixture Substances 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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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to an evaluation method for a residence time safe operation boundary 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 assessment method of the residence time safe operation boundary of the oxidation reactor 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 the outlet of the reactor with temperature control.
Description
Technical Field
The invention relates to a method for evaluating the residence time safety operation boundary 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 assessment method for the residence time safety operation boundary of the oxidation reactor. The method is used for evaluating the safe operation boundary of the residence time of the oxidation reactor, and has the advantages of effectively detecting the explosion danger of the oxidation reactor and providing corresponding parameter data.
In order to solve the problems, the technical scheme adopted by the invention is as follows: a assessment method of a residence time safe operation boundary of an oxidation reactor is carried out on an assessment device of the oxidation reactor, oxygen and combustible gas are uniformly mixed in an oxygen mixer and then enter the reactor with temperature control through a metering pump, a thermocouple is installed on the reactor and transmits a temperature signal to a computer, the computer judges whether the mixed combustible gas is burnt or not according to the temperature change condition, once the gas is burnt and exploded, a safety valve or a rupture disk is opened, and tail gas is discharged 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, the mixed combustible gas is circulated for many times until the explosion occurs, the flow of the metering pump with the explosion occurs is recorded, and the retention time of the material is calculated; 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 solution, preferably, the thermocouples are uniformly arranged along the axial direction of the reactor with temperature control.
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 dwell time's safe critical value through testing conditions such as different reaction temperature, oxygen concentration and initial pressure to the explosive danger that exists in the oxidation reaction reactor, provides the basis for oxidation reaction formulation 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 residence time safe operation boundary 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 is filled in the oxygen mixer, and the fire-retardant and explosion-proof filler is made of porous spherical non-metallic organic materials. 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, reaction temperature and initial pressure were fixed and the safe operating boundaries for material residence time 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. and recording the flow of the metering pump with the explosion and calculating the retention time of the material.
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 assessment method of a residence time safe operation boundary of an oxidation reactor is carried out on an assessment device of the oxidation reactor, oxygen and combustible gas are uniformly mixed in an oxygen mixer and then enter the reactor with temperature control through a metering pump, a thermocouple is installed on the reactor and transmits a temperature signal to a computer, the computer judges whether the mixed combustible gas is burnt or not according to the temperature change condition, once the gas is burnt and exploded, a safety valve or a rupture disk is opened, and tail gas is discharged 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, the mixed combustible gas is circulated for many times until the explosion occurs, the flow of the metering pump with the explosion occurs is recorded, and the retention time of the material is calculated; 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 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; 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.
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| CN201610163830.5A CN107219253B (en) | 2016-03-22 | 2016-03-22 | Method for evaluating safety operation boundary of residence time of oxidation reactor |
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| CN201610163830.5A CN107219253B (en) | 2016-03-22 | 2016-03-22 | Method for evaluating safety operation boundary of residence time of oxidation reactor |
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| CN103256786B (en) * | 2013-06-08 | 2015-09-09 | 中煤科工集团重庆研究院有限公司 | Flame-suppression explosion-suppression type low-concentration coal bed gas cryogenic liquefaction device |
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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 |
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| 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: 20211209 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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