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CN103551086A - Hydrogenation reaction device for refining caprolactam - Google Patents

Hydrogenation reaction device for refining caprolactam Download PDF

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Publication number
CN103551086A
CN103551086A CN201310556756.XA CN201310556756A CN103551086A CN 103551086 A CN103551086 A CN 103551086A CN 201310556756 A CN201310556756 A CN 201310556756A CN 103551086 A CN103551086 A CN 103551086A
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China
Prior art keywords
reactor
sedimentation
catalyst
hydrogenation reaction
reaction device
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CN201310556756.XA
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CN103551086B (en
Inventor
张电子
李磊
李识寒
王大勇
景国耀
禹保卫
杜卫民
余保银
任文杰
孙超伟
庞向川
张恒超
刘国学
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Nylon Science and Technology Ltd. of China Ping Meishen horse group
Shenma Industrial Co., Ltd.
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SHENMA INDUSTRIAL 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

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  • Other In-Based Heterocyclic Compounds (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

The invention discloses a hydrogenation reaction device for refining caprolactam. The hydrogenation reaction device comprises a reaction system and a catalyst sedimentation recycling system. The reaction system comprises a reactor and a reactor stirrer which is arranged in the reactor, and the inner bottom of the reactor is provided with a liquid-phase distributor and a gas-phase distributor; the catalyst sedimentation recycling system comprises a sedimentation kettle and a sedimentation kettle stirrer and a baffle plate, which are arranged inside the sedimentation kettle, the top of the sedimentation kettle is provided with a gas-phase outlet, the side part of the sedimentation kettle is provided with a liquid-phase product outlet, the bottom of the sedimentation kettle is provided with a sedimentation kettle catalyst outlet, the sedimentation kettle catalyst outlet is connected with a reactor feeding port through a pipeline, so that the catalyst can be reused. The hydrogenation reaction device is reasonable and simple in design and good in hydrogenation reaction effect; moreover, the catalyst can be well reused, the energy consumption is reduced, the corporate benefit is increased, and the practicability is strong.

Description

A kind of hydrogenation reaction device for refined caprolactam
Technical field
The present invention relates to a kind of reaction unit for refined caprolactam, relate in particular to a kind of hydrogenation reaction device that comprises the refined caprolactam of reaction system and catalyst sedimentation recovery system, belong to chemical technology field.
Background technology
Caprolactam is a kind of important chemical products, closely bound up with the development of national economy and the people's life.Caprolactam, mainly as the monomer of nylon-6, generates polyamide by polymerization caprolactam and cuts into slices, and further polyamide slice processing is become to nylon-6 fiber, nylon-6 engineering plastics, nylon-6 film.Nylon-6 fiber can be processed into civilian silk and industrial yarn, industrial yarn is mainly used in making tyre cord, cable, safety belt, parachute, canvas, insulating materials and conveyer belt etc., and civilian silk can be used for making textile as carpet, clothes, woollen blanket, nonwoven, case and bag and rope etc.Nylon-6 engineering plastics are widely used in the fields such as automobile, boats and ships, industrial machinery, electrical and electronic component.Nylon-6 film is mainly used in the preservative film of processed food etc.In a word, caprolactam purposes is very extensive.
In caprolactam production, be divided into rough and refining two steps.In crude caprolactam, contain the unsaturated materials that some physical propertys and caprolactam are close (for example, 2-hydroxy-cyclohexanone, cyclonene etc.).The existence of these unsaturated compounds has had a strong impact on the quality of caprolactam product, and is difficult to be removed with conventional separation method.Caprolactam refining process is by carrying out hydrotreatment under catalyst existence condition, becoming boiling point higher or lower than the material of caprolactam these unsaturated impurity conversion, so that separated in subsequent handling.
At present the hydrofinishing work of caprolactam acid amides is focused mostly on catalyst and novel reactor, for example, the amorphous nickel catalyst that China PetroChemical Corporation proposes and magnetic stablizing bed under under magnetic noble metal catalyst exists, the hydrogenation reaction to caprolactam under anhydrous condition.China Tianchen Engineering Co., Ltd has proposed Hydrogen distribution device of horizontally set below the agitator of hydrogenation reaction kettle, is convenient to control hydrogenation reaction, reduces the consumption of hydrogen.These prior aries all can not realize optimizes the object that hydrogenation reaction equipment reaches sedimentation recycling catalyst.
Summary of the invention
For the existing deficiency of prior art, technical problem to be solved by this invention be to provide a kind of structural design more rationally, technique is simple, reaction effect is better, the hydrogenation reaction device of the refined caprolactam of Energy Intensity Reduction.
For realizing above-mentioned object, the present invention adopts following technical scheme:
A hydrogenation reaction device, comprise reaction system and catalyst sedimentation recovery system;
Described reaction system is connected with described catalyst sedimentation recovery system by pipeline;
Described reaction system comprises reactor and the reactor agitator that is built in described reactor, and described reactor is also provided with reactor charging aperture and the outlet of reactor product;
Described catalyst sedimentation recovery system comprises sedimentation still and the sedimentation still agitator that is built in described sedimentation still, and described sedimentation still is also provided with sedimentation still charging aperture, the outlet of sedimentation still product and sedimentation still catalyst outlet;
Described reactor product outlet is connected with described sedimentation still charging aperture by pipeline, and described sedimentation still catalyst outlet is connected with described reactor charging aperture by pipeline.
Wherein more preferably, described reactor charging aperture comprises: hydrogen feed mouth and caprolactam water solution charging aperture; Described hydrogen feed mouth is arranged on described reactor bottom.
Wherein more preferably, described hydrogen feed mouth is in described reactor and is also provided with gaseous distributer, and described gaseous distributer is positioned at described reactor bottom.
Wherein more preferably, described gaseous distributer is positioned at described reactor bottom, and the distance bottom described reactor is 1/5~1/4 place that described reactor is high.
Wherein more preferably, described caprolactam water solution charging aperture is in described reactor and is also provided with liquid phase distributor, and described liquid phase distributor is positioned at described reactor bottom.
Wherein more preferably, described liquid phase distributor is positioned at described reactor bottom, and the distance bottom described reactor is 1/5~1/4 place that described reactor is high.
Wherein more preferably, described liquid phase distributor is positioned at described gaseous distributer top, leaves the space of passing through for reactant between the two.
Wherein more preferably, the distance between described gaseous distributer and described liquid phase distributor is 10~50cm, preferably 10~30cm.
Wherein more preferably, described sedimentation still inner surface is provided with baffle plate.
Wherein more preferably, described sedimentation still is also provided with gaseous phase outlet, and described gaseous phase outlet is provided with automatic pressure instrument.
Wherein more preferably, the pipeline between described sedimentation still catalyst outlet and described reactor charging aperture is provided with slush pump.
Wherein more preferably, the stirring vane of described reactor agitator is single-stage or multistage blade; The stirring vane of described sedimentation still agitator is single-stage or multistage blade.
Wherein more preferably, described reactor is one or more, and described a plurality of reactors adopt serial or parallel connection mode to connect.
Wherein more preferably, described sedimentation still is one or more, and described a plurality of sedimentation stills adopt serial or parallel connection mode to connect.
Hydrogenation reaction device for refined caprolactam provided by the present invention, the gaseous distributer and the liquid phase distributor that by reactor bottom, arrange, effectively improve hydrogenation efficiency; The Multi-stage stirring blade that reactor agitator is provided with, under agitation mixes catalyst, caprolactam water solution and hydrogen, realizes the even mixing of solid, liquid, gas; Under the effect of catalyst baffle plate in sedimentation still, be easy to sedimentation, the catalyst of sedimentation is delivered to reactor through slush pump, re-uses, cost-saving.
Accompanying drawing explanation
Fig. 1 is the hydrogenation reaction apparatus structure schematic diagram of refined caprolactam.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
As shown in Figure 1, the invention provides a kind of hydrogenation reaction device of refined caprolactam, comprise reaction system and catalyst sedimentation recovery system; Reaction system comprises reactor 4 and the reactor agitator 1 that is built in reactor 4, and reactor 4 is also provided with reactor charging aperture, reactor product outlet 8; Catalyst sedimentation recovery system comprises sedimentation still 15 and is built in the sedimentation still agitator 13 of sedimentation still 15, sedimentation still 15 is provided with sedimentation still charging aperture, sedimentation still product outlet 11, sedimentation still catalyst outlet and gaseous phase outlet 10, and gaseous phase outlet 10 is controlled whole reaction system pressure and maintained 0.7MPa.Reactor product outlet 8 is connected with sedimentation still charging aperture by pipeline, and sedimentation still catalyst outlet is connected with reactor charging aperture by pipeline.Below the hydrogenation reaction device of this refined caprolactam is launched to describe in detail.
As shown in Figure 1, the reactor charging aperture of reactor 4 is divided into hydrogen feed mouth 7 and caprolactam water solution charging aperture 2.Hydrogen feed mouth 7 is arranged at the bottom of reactor 4.In order effectively to improve hydrogenation efficiency, augmenting response thing contact area, make reaction mass in the interior abundant reaction of reactor 4, in hydrogen feed mouth 7 place's reactors 4, be also provided with gaseous distributer 6, gaseous distributer 6 is positioned at reactor 4 bottoms, apart from the distance of reactor 4 bottoms, is 1/5~1/4 place that reactor 4 is high; In caprolactam water solution charging aperture 2 place's reactors 4, be provided with liquid phase distributor 5, liquid phase distributor 5 is positioned at reactor 4 bottoms, apart from the distance of reactor 4 bottoms, is 1/5~1/4 place that reactor 4 is high.Liquid phase distributor 5 is positioned at gaseous distributer 6 tops, leaves the space of passing through for reactant between the two.Distance between gaseous distributer 6 and liquid phase distributor 5 is 10~50cm, preferably 10~30cm.The stirring vane 3 of reactor agitator 1 is single-stage or multistage blade, makes reactant fully reaction fast.
For making to react reaction clear liquid and the catalyst separation in afterproduct, the stirring vane of sedimentation still agitator 13 is made as single-stage or multistage blade, and multistage blade makes to react afterproduct and better moves upward, and reaction clear liquid flows out by sedimentation still product outlet 11; Sedimentation still 15 inner surfaces are provided with baffle plate 12, and reaction afterproduct turns and moves upward at sedimentation still agitator 13 effect backspins, and catalyst moves downward under the baffling effect of baffle plate 12, falls to faster sedimentation still 15 bottoms.The catalyst of lower floor enters sedimentation still catalyst outlet, gets back to reactor 4, and so forth circulation.Preferably, the slush pump 9 being provided with on the pipeline between sedimentation still catalyst outlet and the reactor charging aperture of reactor 4, can accelerate the flow velocity that catalyst filters.Sedimentation still charging aperture is in baffle plate 12 bottoms.At this, it should be noted that, when the reactor charging aperture of reactor 4 is hydrogen feed mouth 7 and caprolactam water solution charging aperture 2, the catalyst flowing out from sedimentation still catalyst outlet can flow into reactor 4 from caprolactam water solution charging aperture 2.Can certainly on reactor 4, separately offer separately the catalyst flowing out from sedimentation still catalyst outlet into confession and flow into reactor 4.
Gaseous phase outlet 10 is installed automatic pressure instrument, and the pressure of controlling whole reaction system maintains a setting value (preferably 0.7MPa).When pressure surpasses after 0.7MPa, automatic pressure meter valve is opened pressure release to 0.7MPa.
Reactor 4 can be a plurality of, a plurality of reactors 4 adopt serial or parallel connection mode to connect, a plurality of reactors 4 can increase the reaction time of raw material caprolactam water solution, catalyst and hydrogen while being connected in series, improve reaction yield, when a plurality of reactors 4 are connected in parallel, can effectively improve the output capacity of reactant.Sedimentation still 15 can be a plurality of, and a plurality of sedimentation stills 15 adopt serial or parallel connection mode to connect.A plurality of sedimentation still 15 tandem energies are sedimentation catalyst step by step, makes catalyst further separated, and a plurality of sedimentation still 15 parallel connections can be shared the load of sedimentation still 15 when reactant output capacity is large.
Apply the process that hydrogenation reaction device provided by the invention carries out hexanolactam hydrofining as follows:
By after raw material caprolactam water solution and the catalyst mix that configures, from reactor 4 caprolactam water solution charging apertures 2, enter into liquid phase distributor 5, after liquid phase distributor 5, enter reactor 4.Meanwhile, hydrogen enters Hydrogen distribution device 6 from hydrogen feed mouth 7, through Hydrogen distribution device 6, enters into reactor 4.Hydrogen fully reacts under the uniform stirring of reactor agitator 1 fast with caprolactam water solution.Reaction temperature is controlled at 90 ℃.Reaction afterproduct exports 8 overflows from reactor product, by pipeline, flow to sedimentation still charging aperture, enters sedimentation still 15.Under the effect of sedimentation still agitator 13 and baffle plate 12, catalyst sedimentation is at the bottom of still, by sedimentation still catalyst outlet through slush pump 9 by catalyst transport to reactor 4, reaction clear liquid flows out through sedimentation still product outlet 11.The pressure of controlling whole reaction system by controlling gaseous phase outlet 10 maintains 0.7MPa.Above one embodiment of the present of invention are had been described in detail, but described content is only the preferred embodiment of present technique, can not be considered to for limiting practical range of the present invention.All equalization variations of doing according to the present patent application scope and improvement etc., within all should still belonging to patent covering scope of the present invention.

Claims (10)

1. for a hydrogenation reaction device for refined caprolactam, it is characterized in that, comprise reaction system and catalyst sedimentation recovery system;
Described reaction system is connected with described catalyst sedimentation recovery system by pipeline;
Described reaction system comprises reactor (4) and is built in the reactor agitator (1) of described reactor, and described reactor (4) is also provided with reactor charging aperture, reactor product outlet (8);
Described catalyst sedimentation recovery system comprises sedimentation still (15) and is built in the sedimentation still agitator (13) of described sedimentation still, and described sedimentation still (15) is provided with sedimentation still charging aperture, the outlet of sedimentation still product (11) and sedimentation still catalyst outlet;
Described reactor product outlet (8) is connected with described sedimentation still charging aperture by pipeline, and described sedimentation still catalyst outlet is connected with described reactor charging aperture by pipeline.
2. hydrogenation reaction device as claimed in claim 1, is characterized in that, described reactor charging aperture comprises: hydrogen feed mouth (7) and caprolactam water solution charging aperture (2);
Described hydrogen feed mouth (7) is arranged on described reactor (4) bottom.
3. hydrogenation reaction device as claimed in claim 2, is characterized in that, described hydrogen feed mouth (7) is in described reactor (4) and is also provided with gaseous distributer (6), and described gaseous distributer (6) is positioned at described reactor (4) bottom.
4. hydrogenation reaction device as claimed in claim 2, is characterized in that, described caprolactam water solution charging aperture (2) is in described reactor (4) and is also provided with liquid phase distributor (5), and described liquid phase distributor (5) is positioned at described reactor (4) bottom.
5. hydrogenation reaction device as claimed in claim 1, is characterized in that, described sedimentation still (15) inner surface is provided with baffle plate (12).
6. hydrogenation reaction device as claimed in claim 1, is characterized in that, the pipeline between described sedimentation still catalyst outlet and described reactor charging aperture is provided with slush pump (9).
7. hydrogenation reaction device as claimed in claim 1, is characterized in that, the stirring vane (3) of described reactor agitator (1) is single-stage or multistage blade; The stirring vane (14) of described sedimentation still agitator (13) is single-stage or multistage blade.
8. hydrogenation reaction device as claimed in claim 1, is characterized in that, described sedimentation still (15) is also provided with gaseous phase outlet (10), and described gaseous phase outlet (10) is installed automatic pressure instrument.
9. hydrogenation reaction device as claimed in claim 1, is characterized in that, described reactor (4) is one or more; Described a plurality of reactor (4) adopts serial or parallel connection mode to connect.
10. hydrogenation reaction device as claimed in claim 1, is characterized in that, described sedimentation still (15) is one or more; Described a plurality of sedimentation stills (15) adopt serial or parallel connection mode to connect.
CN201310556756.XA 2013-11-08 2013-11-08 A kind of hydrogenation reaction device for refined caprolactam Active CN103551086B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106166471A (en) * 2016-08-11 2016-11-30 爱森(中国)絮凝剂有限公司 The chemical reaction device that a kind of band catalyst reclaims
CN110961067A (en) * 2019-10-28 2020-04-07 武汉有机实业有限公司 Continuous reaction device and method for benzoic acid hydrogenation
CN115253931A (en) * 2022-07-06 2022-11-01 安徽昊源化工集团有限公司 Coupling reactor for synthesizing ethylene glycol by dimethyl oxalate hydrogenation

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6379693B1 (en) * 2000-05-19 2002-04-30 Ling-Jui Cheng Chiang Trivalent chromium complex compound and milk product containing the same
CN1696087A (en) * 2005-05-17 2005-11-16 中国神马集团有限责任公司 Benzene hydrogenation to produce cyclohexene plant
CN101712621A (en) * 2009-09-02 2010-05-26 甘肃银达化工有限公司 Method for continuously preparing toluenediamine
CN202070196U (en) * 2011-04-28 2011-12-14 天津大学 Continuous settling tank
CN203663808U (en) * 2013-11-08 2014-06-25 神马实业股份有限公司 Hydrogenation reaction device for refining caprolactam

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6379693B1 (en) * 2000-05-19 2002-04-30 Ling-Jui Cheng Chiang Trivalent chromium complex compound and milk product containing the same
CN1696087A (en) * 2005-05-17 2005-11-16 中国神马集团有限责任公司 Benzene hydrogenation to produce cyclohexene plant
CN101712621A (en) * 2009-09-02 2010-05-26 甘肃银达化工有限公司 Method for continuously preparing toluenediamine
CN202070196U (en) * 2011-04-28 2011-12-14 天津大学 Continuous settling tank
CN203663808U (en) * 2013-11-08 2014-06-25 神马实业股份有限公司 Hydrogenation reaction device for refining caprolactam

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106166471A (en) * 2016-08-11 2016-11-30 爱森(中国)絮凝剂有限公司 The chemical reaction device that a kind of band catalyst reclaims
CN110961067A (en) * 2019-10-28 2020-04-07 武汉有机实业有限公司 Continuous reaction device and method for benzoic acid hydrogenation
CN110961067B (en) * 2019-10-28 2021-12-24 武汉有机实业有限公司 Continuous reaction device and method for benzoic acid hydrogenation
CN115253931A (en) * 2022-07-06 2022-11-01 安徽昊源化工集团有限公司 Coupling reactor for synthesizing ethylene glycol by dimethyl oxalate hydrogenation

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