CN106824301B - A kind of benzene hydrogenating catalyst regenerative system and technique - Google Patents

A kind of benzene hydrogenating catalyst regenerative system and technique Download PDF

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Publication number
CN106824301B
CN106824301B CN201611208943.9A CN201611208943A CN106824301B CN 106824301 B CN106824301 B CN 106824301B CN 201611208943 A CN201611208943 A CN 201611208943A CN 106824301 B CN106824301 B CN 106824301B
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catalyst
aeration
catalyst regeneration
tank
regeneration
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CN106824301A (en
Inventor
张庆喜
刘福青
孙立平
张鑫
王士波
魏传奇
朱士超
李怀增
谢培建
郭平
袁东立
王彤
李海滨
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Liaocheng Luxi polyamide New Material Technology Co., Ltd
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Liaocheng Meisi New Material Technology Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

Abstract

The invention discloses a kind of benzene hydrogenating catalyst regenerative system and techniques, including sequentially connected catalyst regeneration stripper, catalyst regeneration aeration tank, aeration and catalyzing agent delivery pump, catalyst regeneration boiling pot and regenerated catalyst delivery pump, vapor tight tank is equipped at the suction line of the aeration and catalyzing agent delivery pump, sealed storage raw catelyst in the vapor tight tank, need regenerated catalyst after catalyst regeneration stripper deoils, the hydrogen that aeration removal needs to adhere in regenerated catalyst is carried out into catalyst regeneration aeration tank, raw catelyst in catalyst and vapor tight tank after catalyst regeneration aeration tank removal hydrogen is delivered to catalyst regeneration boiling pot and carries out heating purification by regenerated catalyst delivery pump, finally pass through regenerated catalyst delivery pump for the catalyst transport in catalyst regeneration boiling pot to reactor.The additive amount of raw catelyst had not only been reduced using system and technique of the invention, but also has reduced power consumption.

Description

A kind of benzene hydrogenating catalyst regenerative system and technique
Technical field
The present invention relates to benzene hydrogenation production system and techniques, and in particular to a kind of benzene hydrogenating catalyst regenerative system and work Skill.
Background technique
Cyclohexanone is important industrial chemicals, is the main intermediate for manufacturing nylon, caprolactam and adipic acid.It is also important Industrial solvent especially contain nitrocellulose, vinyl chloride-base polymer and its copolymer or methyl for those such as painting Acrylate polymer paint etc..In industrial production, often using benzene as raw material, production cyclohexanone is carried out.In the work of benzene preparing cyclohexanone In skill and system, ruthenium is the catalyst of partial hydrogenation of benzene cyclohexene, and the core catalyst of entire technique and system.Catalysis The performance of agent determines performance, cost, quality and the safety of technique and system.When the ruthenium catalyst in catalyst slurry reaches the longevity When life, catalyst will fail, and be embodied in the conversion ratio of technique and system, selectivity is greatly lowered.Need to technique and Catalyst in system is replaced.According to the conversion ratio of reaction, yield in actual production, it is interrupted and is added into technique and system Catalyst is constant with the activity for guaranteeing catalyst slurry in technique and system, and device runs smoothly.Ruthenium catalyst is nanometer grade gold Belong to microcrystal grain, thermodynamically unstable, many impurity contents can all make a big impact to catalyst in reaction environment, especially It is the pH value of reaction system, reaction mother liquor ingredient, (benzene, hydrogen, high purity water etc.) sulfide and ammonia state compound contain in raw material Amount, content of beary metal etc. can all cause the active and selective fluctuation of catalyst.Therefore ruthenium catalyst is in technique and system In addition seem extremely important.
Benzene hydrogenating catalyst regeneration technology in traditional benzene preparing cyclohexanone technique, as shown in Figure 1, its capital equipment includes Catalyst regeneration stripper 1, catalyst regeneration aeration tank 2, aeration and catalyzing agent delivery pump 3, catalyst regeneration boiling pot 4, regeneration Catalyst transport pump 5, raw catelyst bucket 6 and barrel pump 7 need regenerated catalyst to need by the removal of catalyst regeneration stripper 1 The oil in regenerated catalyst is wanted, is oxidized away subsequently into catalyst regeneration aeration tank 2 using oxygen denuded air and needs regenerated urge The hydrogen adhered in agent, using aeration and catalyzing agent delivery pump 3 by catalyst regeneration aeration tank 2 treated need it is regenerated Catalyst transport is to catalyst regeneration boiling pot 4 and carries out boiling purification, finally by regenerated catalyst delivery pump 5 effect with Circulation slurry is sent together to hydrogenator;Meanwhile the raw catelyst in raw catelyst bucket 7 is delivered to and urges by barrel pump 7 or nitrogen Agent regenerated aeration tank 2, to complete the supplement of catalyst.Since catalyst regeneration aeration tank is normal pressure tank, the work of boiling pot Pressure is 0.4MPaG, under normal circumstances, it is safer that raw catelyst is added to regenerated aeration tank.
But the problem is that, firstly, catalyst regeneration aeration tank 2 is the oxygen deprivation being made by instrument wind and nitrogen Air oxidation removes the hydrogen and entrained oil point for needing depth absorption on regenerated catalyst particle, and raw catelyst is added to catalysis Agent regenerated aeration tank 2 is mixed with regenerated catalyst, the oil pollution being easily removed, while being exposed in oxygen denuded air and can also be made It is aoxidized at nanometer ruthenium crystallite, to reduce the activity of catalyst, so that the activity of catalyst reduces, causes raw catelyst additive amount Increase increase production cost to waste noble metal catalyst ruthenium.
Secondly, the addition of raw catelyst generally requires to carry out pressurized delivered by barrel pump 7 or nitrogen, increases power and disappear Consumption, to further increase production cost.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention provides a kind of benzene hydrogenating catalyst regenerative system and techniques, both Reduce the additive amount of raw catelyst, and reduces power consumption.
To achieve the above object, the technical solution of the present invention is as follows:
A kind of benzene hydrogenating catalyst regenerative system, including sequentially connected catalyst regeneration stripper, catalyst regeneration expose Gas tank, aeration and catalyzing agent delivery pump, catalyst regeneration boiling pot and regenerated catalyst delivery pump are conveyed in the aeration and catalyzing agent Vapor tight tank is equipped at the suction line of pump, sealed storage raw catelyst in the vapor tight tank, the aeration and catalyzing agent delivery pump will The regenerated catalyst transport of needs in raw catelyst and catalyst regeneration aeration tank in the vapor tight tank is to catalyst regeneration Boiling pot, then by regenerated catalyst delivery pump by the defeated of the raw catelyst in catalyst regeneration boiling pot and the catalyst after regeneration Send reactor.
The present invention is not necessarily to raw catelyst catalyst regeneration aeration tank is added, and is pumped by vapor tight tank from aeration catalyst transport Inlet pipeline on be added, be mixed into catalyst regeneration boiling pot with by the regenerated catalyst of needs of Air Exposure, pass through It crosses and boils, purifies, the reaction temperature of the temperature and subsequent reactor that make catalyst is consistent, and has both prevented the dirt of aeration tank Dye ensure that raw catelyst performance and active stabilization, and be directly the defeated of raw catelyst by aeration and catalyzing agent delivery pump Offer power is provided, the quantity pumped in system is reduced, reduces power consumption, improves power utilization rate.
Preferably, the catalyst regeneration boiling pot is equipped with blender.Guarantee what raw catelyst was mixed with regenerated catalyst Uniformity.
Preferably, the pipeline between the vapor tight tank and the aeration and catalyzing agent delivery pump is equipped with valve.Pass through valve Switch can be realized the timing addition of raw catelyst;It can be realized the quantitative addition of raw catelyst by the aperture of valve simultaneously.
It is further preferred that the entrance of the vapor tight tank is equipped with the pipeline that raw catelyst is added.For adding into vapor tight tank Add raw catelyst.
Aeration and catalyzing agent delivery pump and regenerated catalyst delivery pump are all diaphragm pump.
Preferably, the oxygen denuded air entrance of the catalyst regeneration aeration tank is provided with catalyst regeneration aeration pot sidewall bottom Portion.The time of contact of oxygen denuded air and catalyst can be increased.
Heretofore described catalyst regeneration stripper is commonly to flash stripper in chemical company.
Heretofore described catalyst regeneration aeration tank is common aeration tank in chemical company.
Heretofore described catalyst regeneration boiling pot is that steam coil heated boiling is commonly utilized in chemical company Tank is risen, to guarantee the uniformity of boiling pot temperature.
Heretofore described vapor tight tank is the atmospheric storage tank of favorable sealing property, and catalyst passes through desalted water in hermetically sealed can It seals, the catalyst being added in tank is added under desalted water water seal state, and the presence of desalted water prevents hermetically sealed can be pumped into negative pressure.
A kind of above system is preparing the application in cyclohexanone system.
A kind of benzene hydrogenating catalyst regeneration technology provides catalyst regeneration stripper, catalyst regeneration aeration tank, aeration and urges Agent delivery pump, catalyst regeneration boiling pot, regenerated catalyst delivery pump and vapor tight tank, sealed storage is newly urged in the vapor tight tank Agent needs regenerated catalyst after catalyst regeneration stripper deoils, and is aerated into catalyst regeneration aeration tank After removal needs the hydrogen adhered in regenerated catalyst, regenerated catalyst delivery pump that catalyst regeneration aeration tank is removed hydrogen Catalyst and vapor tight tank in raw catelyst be delivered to catalyst regeneration boiling pot and carry out heating purification, finally urged by regeneration Agent delivery pump is by the catalyst pressurized delivered in catalyst regeneration boiling pot to reactor.
Preferably, the pipeline of raw catelyst can be provided for vapor tight tank by providing one.
Preferably, oxygen denuded air is passed through the bottom of catalyst regeneration aeration tank, and oxygen denuded air is made to need regenerated catalysis Agent provides oxygen, with the hydrogen adhered in the catalyst of oxidation regeneration.
Heretofore described oxygen denuded air is the gaseous mixture of instrument air and nitrogen according to a certain percentage.Keep addition Gas oxygen content is in 3vol% hereinafter, to guarantee that oxygen concentration is lower than the explosive range of hydrogenation reaction.
A kind of above-mentioned technique is preparing the application in cyclohexanone technique.
The advantages of this technique is compared with traditional handicraft:
1, traditional handicraft is added by aeration tank equipment, needs to be pressed into tank by pump or nitrogen;It is changed to aeration tank delivery pump A vapor tight tank is fixed in the upper surface of inlet pipeline in entry position, opens the valve of tank when addition every time, passes through the self-priming of pump Addition can be completed in pipeline, reduces power consumption.
2, fresh catalyst does not add catalyst regeneration aeration tank, by vapor tight tank from aeration catalyst transport pump into It is added, is mixed by the catalyst of Air Exposure, catalyst regeneration boiling pot has blender, can guarantee on mouth pipeline The uniformity that raw catelyst is mixed with regenerated catalyst.The working principle of catalyst regeneration boiling pot is boiled to regenerated catalyst Boiling, purification keep consistent with the temperature of reactor, then send together with recycling catalyst to hydrogenator.It is urged due to fresh Agent does not pass through the pollution of aeration tank, ensure that raw catelyst performance and active stabilization.
Detailed description of the invention
Fig. 1 is conventional process flow figure;
Fig. 2 is process flow chart of the invention;
Wherein, 1. catalyst regeneration stripper, 2. catalyst regeneration aeration tanks, 3. aeration and catalyzing agent delivery pumps, 4. catalysis Agent regenerates boiling pot, 5. regenerated catalyst delivery pumps, 6. fresh catalyst buckets, 7. barrel pumps, 8. hermetically sealed cans.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings.
A kind of benzene hydrogenating catalyst regenerative system, as shown in Fig. 2, including sequentially connected catalyst regeneration stripper 1, urging Agent regenerated aeration tank 2, aeration and catalyzing agent delivery pump 3, catalyst regeneration boiling pot 4 and regenerated catalyst delivery pump 5, are being aerated Vapor tight tank 8, sealed storage raw catelyst in vapor tight tank 8, aeration and catalyzing agent conveying are equipped at the suction line of catalyst transport pump 3 Pump 3 by the regenerated catalyst transport of needs in the raw catelyst and catalyst regeneration aeration tank 4 in vapor tight tank 8 to catalyst again Raw boiling pot 4, then by regenerated catalyst delivery pump 5 by the raw catelyst in catalyst regeneration boiling pot 4 and the catalysis after regeneration The transport reactor of agent.
Pipeline between vapor tight tank 8 and aeration and catalyzing agent delivery pump 3 is equipped with valve.It can be realized newly by the switch of valve The timing of catalyst is added;It can be realized the quantitative addition of raw catelyst by the aperture of valve simultaneously.
The entrance of vapor tight tank 8 is equipped with the pipeline that raw catelyst is added.For adding raw catelyst into vapor tight tank 8.
The instrument air entrance of catalyst regeneration aeration tank 2 is provided with catalyst regeneration aeration tank sidewall bottom.
The nitrogen inlet of catalyst regeneration aeration tank 2 is provided with catalyst regeneration aeration tank sidewall bottom.
It is passed through instrument air and nitrogen into catalyst regeneration aeration tank 2 simultaneously, to realize to catalyst regeneration aeration tank 2 In be passed through oxygen denuded air.
Its process flow is as follows:
Need regenerated catalyst after catalyst regeneration stripper deoils, into catalyst regeneration aeration tank, oxygen deprivation Air is passed through the bottom of catalyst regeneration aeration tank, is aerated in catalyst regeneration aeration tank, and oxidation removes catalyst particle The hydrogen of upper depth absorption, aeration and catalyzing agent delivery pump go catalyst regeneration aeration tank in catalyst and vapor tight tank after dehydrogenation Raw catelyst is delivered to catalyst regeneration boiling pot and carries out heating purification, and catalyst passes through middle pressure steam boiling in boiling pot Afterwards, the sulphur and metal ion in catalyst are removed, restores the activity of catalyst, is then delivered to by regenerated catalyst delivery pump Reactor.
The catalyst used is ruthenium catalyst, the cotton-shaped nano metal precipitating of the black being immersed in desalted water, and catalyst is It is interrupted under desalted water water seal state and is added, to prevent vapor tight tank from generating negative pressure,
Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not to invention protection scope Limitation, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not required to It is still within the scope of the present invention to make the creative labor the various modifications or changes that can be made.

Claims (10)

1. a kind of benzene hydrogenating catalyst regenerative system, characterized in that including sequentially connected catalyst regeneration stripper, catalyst Regenerated aeration tank, aeration and catalyzing agent delivery pump, catalyst regeneration boiling pot and regenerated catalyst delivery pump, in the aeration and catalyzing Vapor tight tank is equipped at the suction line of agent delivery pump, sealed storage raw catelyst in the vapor tight tank, the aeration and catalyzing agent is defeated Send pump by the regenerated catalyst transport of needs in the raw catelyst and catalyst regeneration aeration tank in the vapor tight tank to catalysis Agent regenerates boiling pot, then by regenerated catalyst delivery pump by the raw catelyst in catalyst regeneration boiling pot and the catalysis after regeneration Agent is delivered to reactor.
2. the system as claimed in claim 1, characterized in that the catalyst regeneration boiling pot is equipped with blender.
3. the system as claimed in claim 1, characterized in that the pipe between the vapor tight tank and the aeration and catalyzing agent delivery pump Line is equipped with valve.
4. system as claimed in claim 2, characterized in that the entrance of the vapor tight tank is equipped with the pipeline that raw catelyst is added.
5. the system as claimed in claim 1, characterized in that the oxygen denuded air entrance of the catalyst regeneration aeration tank is provided with Catalyst regeneration aeration tank sidewall bottom.
6. a kind of any system of claim 1-5 is preparing the application in cyclohexanone system.
7. a kind of benzene hydrogenating catalyst regeneration technology, characterized in that provide catalyst regeneration stripper, catalyst regeneration aeration Tank, aeration and catalyzing agent delivery pump, catalyst regeneration boiling pot, regenerated catalyst delivery pump and vapor tight tank, it is close in the vapor tight tank Envelope storage raw catelyst, needs regenerated catalyst after catalyst regeneration stripper deoils, is aerated into catalyst regeneration Tank carries out the hydrogen that aeration removal needs to adhere in regenerated catalyst, and regenerated catalyst delivery pump is by catalyst regeneration aeration tank The raw catelyst in catalyst and vapor tight tank after removal hydrogen is delivered to catalyst regeneration boiling pot and carries out heating purification, finally By regenerated catalyst delivery pump by the catalyst transport in catalyst regeneration boiling pot to reactor.
8. technique as claimed in claim 7, characterized in that the pipeline of raw catelyst can be provided for vapor tight tank by providing one.
9. technique as claimed in claim 7, characterized in that instrument air is passed through the bottom of catalyst regeneration aeration tank, makes instrument Table air is needs regenerated catalyst to provide oxygen, with the hydrogen adhered in the catalyst of oxidation regeneration.
10. a kind of any technique of claim 7-9 is preparing the application in cyclohexanone technique.
CN201611208943.9A 2016-12-23 2016-12-23 A kind of benzene hydrogenating catalyst regenerative system and technique Active CN106824301B (en)

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CN107233931A (en) * 2017-07-03 2017-10-10 中国平煤神马集团尼龙科技有限公司 A kind of continuous catalyst regenerating device and method
US10799858B2 (en) * 2018-03-09 2020-10-13 Uop Llc Process for managing sulfur compounds on catalyst
CN109647544B (en) * 2019-01-03 2021-06-11 飞潮(无锡)过滤技术有限公司 Process for recovering waste copper bismuth catalyst by dry-wet composite regeneration
CN115178304A (en) * 2022-06-30 2022-10-14 福建永荣科技有限公司 Catalyst regeneration process for cyclohexanone production based on cyclohexene hydration method
CN115318344A (en) * 2022-09-23 2022-11-11 聊城鲁西聚酰胺新材料科技有限公司 Anti-blocking method for benzene hydrogenation catalyst slurry

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CN1281718C (en) * 2003-10-16 2006-10-25 中国石油化工股份有限公司 Cracking process for hydrocarbon oil
CN102875348A (en) * 2012-09-29 2013-01-16 中国天辰工程有限公司 High-yield production method of cyclohexanone

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Address after: 252211 location of Luxi group in Liaocheng chemical industry park, Liaocheng City, Shandong Province

Patentee after: Liaocheng Luxi polyamide New Material Technology Co., Ltd

Address before: 252000 Shandong Province, Liaocheng City Development Zone, Gu Guan Tun Town resident

Patentee before: LIAOCHENG MEISI NEW MATERIAL TECHNOLOGY CO., LTD.

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Inventor after: Zhang Qingxi

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