CN107286045A - The colourity alarm of cyclohexanone oxamidinating technique and interlocking method under the conditions of fresh catalyst - Google Patents
The colourity alarm of cyclohexanone oxamidinating technique and interlocking method under the conditions of fresh catalyst Download PDFInfo
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- CN107286045A CN107286045A CN201610190329.8A CN201610190329A CN107286045A CN 107286045 A CN107286045 A CN 107286045A CN 201610190329 A CN201610190329 A CN 201610190329A CN 107286045 A CN107286045 A CN 107286045A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C249/00—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton
- C07C249/04—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of oximes
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Abstract
The present invention relates to a kind of colourity alarm of cyclohexanone oxamidinating technique under the conditions of fresh catalyst and interlocking method, the problem of security is poor in the prior art is mainly solved.Colourity alarm and interlocking method of the present invention by using cyclohexanone oxamidinating technique under the conditions of a kind of fresh catalyst, in the process unit of hydrogen peroxide oxidation Cyclohexanone Production cyclohexanone, under the conditions of using fresh catalyst, during catalyst is inactivated, the alarming value of Ammoximation reaction clear liquid colourity is located at 100 ° 200 °, and interlocking value is located at 200 ° 400 °；When Ammoximation reaction clear liquid colourity reaches alarming value; operated using fresh catalyst is added; when Ammoximation reaction clear liquid colourity reaches interlocking value; control system interlocks action launching; cut off hydrogen peroxide, cyclohexanone and ammonia charging; the technical scheme that reactor carries out nitrogen filled protection preferably solves above mentioned problem, available in cyclohexanone oxamidinating technique.
Description
Technical field
The present invention relates to a kind of colourity alarm of cyclohexanone oxamidinating technique under the conditions of fresh catalyst and interlocking method.
Background technology
Caprolactam is the monomer of synthetic fibers and engineering plastics, is always market important industrial chemicals in short supply in China.Mesh
Before, most of production of caprolactam changes into cyclohexanone oxime using cyclohexanone, then is rearranged into the process route of caprolactam.
It is a kind of environmental protection that the direct ammoxidation of cyclohexanone that conversion from cyclohexanone to cyclohexanone oxime is used, which prepares cyclohexanone oxime technique,
The technique of low energy consumption.Cyclohexanone oxamidinating synthesizing cyclohexane 1 ketoxime new technology is in lower pressure using cyclohexanone, ammonia and hydrogen peroxide
Under, the tert-butyl alcohol is solvent, using titanium-silicon molecular sieve catalyst, the one-step synthesis cyclohexanone oxime in continuous slurry bed reactor,
Its reaction equation is (1)：
NH3+H2O2+C6H10O=C6H11ON+2H2O
This method directly prepares cyclohexanone oxime, instead of traditional azanol preparation technology, substantially reduces technological process, saves
Investment, not producing ammonium sulfate byproduct, it is to avoid the production of nitrogen oxides and oxysulfide, great to environment protection significance, application prospect is wide
It is general, receive extensive attention.
Under normal operation, Ammoximation reaction is carried out under high conversion, high selectivity, but when raw material proportioning it is improper and/or
During catalyst activity reduction, main reaction speed declines, main to occur following side reaction：
4H2O2+2NH3=N2O+7H2O
3H2O2+2NH3=N2+6H2O
2H2O2=2H2O+O2
During catalyst inactivation, other side reactions can cause the colourity rise for reacting clear liquid, simultaneously, reaction end gas
The content of middle hazardous gas oxygen, laughing gas and ammonia can also increase, and may cause to form explosive mixed gas in reactor,
Blast will be produced by such as running into burning things which may cause a fire disaster, high temperature or electrostatic spark.
This technology method is by colourity changing rule in the cyclohexanone oxamidinating course of reaction under the conditions of fresh catalyst, to reflect
The degree of Ammoximation reaction catalyst inactivation state and gas phase risk, and corresponding security alarm and interlocking method are set, keep away
Exempt from gas phase and occur blast accident, it is ensured that the safety and steady operation of device.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of new fresh catalyst for the problem of security is poor in the prior art
The colourity alarm of cyclohexanone oxamidinating technique and interlocking method under the conditions of agent.This method has the preferable advantage of security.
To solve the above problems, the technical solution adopted by the present invention is as follows：Cyclohexanone oxamidinating under the conditions of a kind of fresh catalyst
The colourity alarm of technique and interlocking method, in the process unit of hydrogen peroxide oxidation Cyclohexanone Production cyclohexanone, using fresh
Under catalysts conditions, catalyst inactivate during there is provided the alarm of the colourity of safe and reliable Ammoximation reaction clear liquid,
Interlocking value and corresponding safety control measures, to ensure the security of Ammoximation reaction, prevent gas phase and fire；Wherein,
The alarming value of Ammoximation reaction clear liquid colourity is located at 100 ° -200 °, and interlocking value is located at 200 ° -400 °；When oximes anti-
Answer clear liquid colourity reach alarming value when, using add fresh catalyst operation, the fresh catalyst added be reaction system in urge
The 10%-50% of agent；When Ammoximation reaction clear liquid colourity reaches interlocking value, control system interlocking action launching, cut-out is double
Oxygen water, cyclohexanone and ammonia charging, reactor carry out nitrogen filled protection.
In above-mentioned technical proposal, it is preferable that when Ammoximation reaction clear liquid colourity reaches interlocking value, control system interlocking action
Start, cut-out hydrogen peroxide, cyclohexanone and ammonia charging, reactor carries out nitrogen charging (herein referring to nitrogen) protection, and keeps tertiary fourth
Alcohol is circulated.
In above-mentioned technical proposal, it is preferable that the fresh catalyst added is the 20%-30% of catalyst in reaction system.
Patent of the present invention is on the basis of the changing rule of fresh catalyst inactivation colourity, it is proposed that the report of corresponding colourity
Alert and interlocking control method, is effectively ensured Ammoximation reaction security, prevents blast accident, it is to avoid unplanned parking,
Achieve preferable technique effect.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Embodiment
【Embodiment 1】
The colourity alarm of cyclohexanone oxamidinating technique and interlocking method, are urged using HTS under the conditions of a kind of fresh catalyst
Agent, in fresh catalyst inactivation, Ammoximation reaction device clear liquid colourity alarming value is 150 °, and interlocking value is 250 °.
When colourity reaches 150 ° of alarming value, operating personnel should carry out fresh makeup catalyst behaviour in 60 minutes to reaction system
Make, magnitude of recruitment is 20% of catalytic amount in reaction system, can effectively reduce the colourity of reaction clear liquid；When colourity reaches interlocking
During 250 ° of value, control system should start interlocked control measure, emergency cut-off hydrogen peroxide and fed cyclohexanone immediately, urgent anti-
Nitrogen charging in device is answered, and keeps the tert-butyl alcohol to circulate.
【Embodiment 2】
The colourity alarm of cyclohexanone oxamidinating technique and interlocking method, are urged using HTS under the conditions of a kind of fresh catalyst
Agent, in fresh catalyst inactivation, Ammoximation reaction device clear liquid colourity alarming value is 200 °, and interlocking value is 280 °；
When colourity reaches 200 ° of alarming value, operating personnel should carry out fresh makeup catalyst behaviour in 30 minutes to reaction system
Make, magnitude of recruitment is 30% of catalytic amount in reaction system, can effectively reduce the colourity of reaction clear liquid；When colourity reaches interlocking
During 280 ° of value, control system should start interlocked control measure, emergency cut-off hydrogen peroxide and fed cyclohexanone immediately, urgent anti-
Nitrogen charging in device is answered, and keeps the tert-butyl alcohol to circulate.
【Embodiment 3】
The colourity alarm of cyclohexanone oxamidinating technique and interlocking method, are urged using HTS under the conditions of a kind of fresh catalyst
Agent, in fresh catalyst inactivation, Ammoximation reaction device clear liquid colourity alarming value is 100 °, and interlocking value is 200 °；
When colourity reaches 100 ° of alarming value, operating personnel should carry out fresh makeup catalyst operation in 1 hour to reaction system,
Magnitude of recruitment is 10% of catalytic amount in reaction system, can effectively reduce the colourity of reaction clear liquid；When colourity reaches interlocking value
At 200 °, control system should start interlocked control measure, emergency cut-off hydrogen peroxide and fed cyclohexanone, alarm reaction immediately
Nitrogen charging in device, and keep the tert-butyl alcohol to circulate.
【Embodiment 4】
The colourity alarm of cyclohexanone oxamidinating technique and interlocking method, are urged using HTS under the conditions of a kind of fresh catalyst
Agent, in fresh catalyst inactivation, Ammoximation reaction device clear liquid colourity alarming value is 200 °, and interlocking value is 400 °；
When colourity reaches 200 ° of alarming value, operating personnel should carry out fresh makeup catalyst operation interior immediately to reaction system,
Magnitude of recruitment is 20% of catalytic amount in reaction system, can effectively reduce the colourity of reaction clear liquid；When colourity reaches interlocking value
At 400 °, control system should start interlocked control measure, emergency cut-off hydrogen peroxide and fed cyclohexanone, alarm reaction immediately
Nitrogen charging in device, and keep the tert-butyl alcohol to circulate.
Obviously, using method of the present invention, under the conditions of using fresh catalyst, effective monitoring Ammoximation reaction situation,
Prevent because reaction deteriorates and causes gas phase to be exploded, it is ensured that the safety and steady operation of device, achieve preferable technique effect.
Claims (3)
1. the colourity alarm of cyclohexanone oxamidinating technique and interlocking method under the conditions of a kind of fresh catalyst, in hydrogen peroxide oxidation hexamethylene
In the process unit of ketone production cyclohexanone, using under the conditions of fresh catalyst, catalyst inactivate during there is provided
Alarm, interlocking value and the corresponding safety control measures of the colourity of safe and reliable Ammoximation reaction clear liquid, it is oximes to ensure
The security of reaction, prevents gas phase and fires；Wherein, the alarming value of Ammoximation reaction clear liquid colourity is located at 100 ° -200 °,
Interlocking value is located at 200 ° -400 °；When Ammoximation reaction clear liquid colourity reaches alarming value, grasped using fresh catalyst is added
Make, the fresh catalyst added is the 10%-50% of catalyst in reaction system；Interlocked when Ammoximation reaction clear liquid colourity is reached
During value, control system interlocking action launching, cut-out hydrogen peroxide, cyclohexanone and ammonia charging, reactor carries out nitrogen filled protection.
2. the colourity of cyclohexanone oxamidinating technique is alarmed and interlocking method under the conditions of fresh catalyst according to claim 1, its
It is characterised by when Ammoximation reaction clear liquid colourity reaches interlocking value, control system interlocking action launching, cut-out hydrogen peroxide, ring
Hexanone and ammonia charging, reactor carries out nitrogen filled protection, and keeps the tert-butyl alcohol to circulate.
3. the colourity of cyclohexanone oxamidinating technique is alarmed and interlocking method under the conditions of fresh catalyst according to claim 1, its
It is characterised by the 20%-30% that the fresh catalyst added is catalyst in reaction system.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610190329.8A CN107286045B (en) | 2016-03-30 | 2016-03-30 | Chroma alarm and interlocking method of cyclohexanone ammoximation process under fresh catalyst condition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610190329.8A CN107286045B (en) | 2016-03-30 | 2016-03-30 | Chroma alarm and interlocking method of cyclohexanone ammoximation process under fresh catalyst condition |
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| CN107286045A true CN107286045A (en) | 2017-10-24 |
| CN107286045B CN107286045B (en) | 2020-03-31 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103949191A (en) * | 2014-05-13 | 2014-07-30 | 湖北三宁化工股份有限公司 | Device and method for continuously adding catalysts in cyclohexanone oximation reaction |
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- 2016-03-30 CN CN201610190329.8A patent/CN107286045B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103949191A (en) * | 2014-05-13 | 2014-07-30 | 湖北三宁化工股份有限公司 | Device and method for continuously adding catalysts in cyclohexanone oximation reaction |
Non-Patent Citations (2)
| Title |
|---|
| 刘卫东: "氨肟化法制备环己酮肟的工艺条件的优化", 《广州化工》 * |
| 彭湘潍: ""氨肟化装置安全性及控制方案研究"项目通过鉴定", 《安全、健康和环境》 * |
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Effective date of registration: 20190816 Address after: 100728 Beijing, Chaoyangmen, North Street, No. 22, No. Applicant after: Sinopec Corp. Applicant after: Qingdao Safety Engineering Research Institute of Sinopec Co., Ltd. Applicant after: SINOPEC Research Institute of Petroleum Processin Address before: Yanan City, Shandong province Qingdao City three road 266071 No. 218 Applicant before: Sinopec Corp. Applicant before: Qingdao Safety Engineering Research Institute of Sinopec Co., Ltd. |
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