CN103551086B - A kind of hydrogenation reaction device for refined caprolactam - Google Patents
A kind of hydrogenation reaction device for refined caprolactam Download PDFInfo
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- CN103551086B CN103551086B CN201310556756.XA CN201310556756A CN103551086B CN 103551086 B CN103551086 B CN 103551086B CN 201310556756 A CN201310556756 A CN 201310556756A CN 103551086 B CN103551086 B CN 103551086B
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- Y—GENERAL 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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- Y02P20/584—Recycling of catalysts
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Abstract
The invention discloses a kind of hydrogenation reaction device for refined caprolactam, comprise reaction system, catalyst sedimentation recovery system. Reaction system comprises reactor and the reactor agitator that is built in reactor, and reactor inner bottom part is provided with liquid phase distributor and gaseous distributer; Catalyst sedimentation recovery system comprises sedimentation still and is built in sedimentation still agitator, the baffle plate of sedimentation still, gaseous phase outlet is arranged at top, sidepiece has liquid product outlet, bottom to have sedimentation still catalyst outlet, sedimentation still catalyst outlet is connected with reactor charging aperture by pipeline, reaches catalyst recycling. The present invention is reasonable in design, and simple, hydrogenation reaction is effective, and well catalyst is recycled, and has reduced energy consumption, has increased the performance of enterprises, practical.
Description
Technical field
The present invention relates to a kind of reaction unit for refined caprolactam, relate in particular to one and comprise reaction system and urgeThe hydrogenation reaction device of the refined caprolactam of agent sedimentation recovery system, belongs 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. OneselfLactams, mainly as the monomer of nylon-6, generates polyamide section by polymerization caprolactam, and further polyamide is cutSheet is processed into nylon-6 fiber, nylon-6 engineering plastics, nylon-6 film. Nylon-6 fiber can be processed into civilian silk and industrySilk, industrial yarn is mainly used in making tyre cord, cable, safety belt, parachute, canvas, insulating materials and conveyer belt etc., the peopleCan be used for making textile as carpet, clothes, woollen blanket, nonwoven, case and bag and rope etc. with silk. Nylon-6 engineering plastics are extensively usedIn fields such as automobile, boats and ships, industrial machinery, electrical and electronic components. Nylon-6 film is mainly used in the preservative film of processed foodDeng. In a word, caprolactam purposes is very extensive.
In caprolactam production, be divided into rough and refining two steps. In crude caprolactam, contain some physicalThe unsaturated materials (for example, 2-hydroxy-cyclohexanone, cyclonene etc.) that matter and caprolactam are close. These unsaturated compoundsExistence has had a strong impact on the quality of caprolactam product, and is difficult to be removed with conventional separation method. Caprolactam essenceProcess processed is by carry out hydrotreatment under catalyst existence condition, by these unsaturated impurity conversion become boiling point higher than or lowIn the material of caprolactam, so that separate in subsequent handling.
At present the hydrofinishing work of caprolactam acid amides is focused mostly on catalyst and novel reactor, for example, inPetrochemical industry group company of state propose amorphous nickel catalyst and magnetic stablizing bed under magnetic noble metal catalyst exist under, rightThe hydrogenation reaction of caprolactam under anhydrous condition. China Tianchen Engineering Co., Ltd has proposed the agitator at hydrogenation reaction kettleHydrogen distribution device of below horizontally set, is convenient to control hydrogenation reaction, reduces the consumption of hydrogen. These prior aries all can notRealize the object that optimization 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 is to provide a kind of structural designMore 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 for refined caprolactam, comprises 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 establishedStill charging aperture and the outlet of reactor product respond;
Described catalyst sedimentation recovery system comprises sedimentation still and the sedimentation still agitator that is built in described sedimentation still, described inSedimentation 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, described sedimentation still catalyst outletBe 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; DescribedHydrogen feed mouth is arranged on described reactor bottom.
Wherein more preferably, described hydrogen feed mouth is in and in described reactor, is also provided with gaseous distributer, described gas phaseDistributor is positioned at described reactor bottom.
Wherein more preferably, described gaseous distributer is positioned at described reactor bottom, apart from the distance of described reactor bottom is1/5～1/4 place that described reactor is high.
Wherein more preferably, described caprolactam water solution charging aperture is in and in described reactor, is also provided with liquid distributionDevice, described liquid phase distributor is positioned at described reactor bottom.
Wherein more preferably, described liquid phase distributor is positioned at described reactor bottom, apart from the distance of described reactor bottom is1/5～1/4 place that described reactor is high.
Wherein more preferably, described liquid phase distributor is positioned at described gaseous distributer top, leaves between the two for reactantThe space of passing through.
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 slurriesPump.
Wherein more preferably, the stirring vane of described reactor agitator is single-stage or multistage blade; Described sedimentation still stirsThe stirring vane of device is single-stage or multistage blade.
Wherein more preferably, described reactor is one or more, and described multiple reactors adopt serial or parallel connection mode to connectConnect.
Wherein more preferably, described sedimentation still is one or more, and described multiple sedimentation stills adopt serial or parallel connection mode to connectConnect.
Hydrogenation reaction device for refined caprolactam provided by the present invention, the gas phase arranging by reactor bottomDistributor and liquid phase distributor, effectively improve hydrogenation efficiency; The Multi-stage stirring blade that reactor agitator is provided with, makes catalysisAgent, caprolactam water solution and hydrogen under agitation mix, and realize the even mixing of solid, liquid, gas; Catalyst is at sedimentation stillUnder the effect of middle baffle plate, be easy to sedimentation, the catalyst of sedimentation is delivered to reactor through slush pump, re-uses, cost-saving.
Brief description of the drawings
Fig. 1 is the hydrogenation reaction apparatus structure schematic diagram of refined caprolactam.
Detailed description of the invention
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 catalysisAgent sedimentation recovery system; Reaction system comprises reactor 4 and the reactor agitator 1 that is built in reactor 4, and reactor 4 is also establishedStill charging aperture, reactor product outlet 8 respond; Catalyst sedimentation recovery system comprises sedimentation still 15 and is built in sedimentation still 15Sedimentation still agitator 13, sedimentation still 15 be provided with sedimentation still charging aperture, sedimentation still product outlet 11, sedimentation still catalyst outlet andGaseous phase outlet 10, gaseous phase outlet 10 is controlled whole reaction system pressure and is maintained 0.7MPa. Pipeline is passed through in reactor product outlet 8Be connected with sedimentation still charging aperture, sedimentation still catalyst outlet is connected with reactor charging aperture by pipeline. Refining own to this belowThe hydrogenation reaction device of lactams launches 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 aperture2. Hydrogen feed mouth 7 is arranged at the bottom of reactor 4. In order effectively to improve hydrogenation efficiency, augmenting response thing contact area, makesReaction mass, in the interior abundant reaction of reactor 4, is also provided with gaseous distributer 6, gas phase in hydrogen feed mouth 7 place's reactors 4Distributor 6 is positioned at reactor 4 bottoms, is 1/5～1/4 place that reactor 4 is high apart from the distance of reactor 4 bottoms; At caprolactamIn aqueous 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 reactorThe distance of 4 bottoms is 1/5～1/4 place that reactor 4 is high. Liquid phase distributor 5 is positioned at gaseous distributer 6 tops, stays between the twoThere is the space of passing through for reactant. 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 listLevel or multistage blade, multistage blade makes to react afterproduct and better moves upward, and reaction clear liquid is by sedimentation still product outlet 11Flow out; Sedimentation still 15 inner surfaces are provided with baffle plate 12, and reaction afterproduct acts on backspin at sedimentation still agitator 13 and turns and move upward, and urgesAgent moves downward under the baffling effect of baffle plate 12, falls to faster sedimentation still 15 bottoms. It is heavy that the catalyst of lower floor entersFall still catalyst outlet, get back to reactor 4, and so forth circulation. Preferably, at sedimentation still catalyst outlet and reactor 4The slush pump 9 that pipeline between reactor charging aperture is provided with, can accelerate the flow velocity that catalyst filters. Sedimentation still charging aperture existsBaffle plate 12 bottoms. It should be noted that at this, when the reactor charging aperture of reactor 4 is hydrogen feed mouth 7 and caprolactam waterWhen solution feed mouth 2, the catalyst flowing out from sedimentation still catalyst outlet can flow into anti-from caprolactam water solution charging aperture 2Answer still 4. Can certainly on reactor 4, separately offer separately the catalyst flowing out from sedimentation still catalyst outlet into confession flows intoReactor 4.
Gaseous phase outlet 10 is installed automatic pressure instrument, and the pressure of controlling whole reaction system maintains a setting value (preferably0.7MPa). When pressure exceedes after 0.7MPa, automatic pressure meter valve is opened pressure release to 0.7MPa.
Reactor 4 can be multiple, and multiple reactors 4 adopt serial or parallel connection mode to connect, and multiple reactor 4 series connection connectWhile connecing, can increase the reaction time of raw material caprolactam water solution, catalyst and hydrogen, improve reaction yield, multiple reactors4 can effectively improve the output capacity of reactant while being connected in parallel. Sedimentation still 15 can be multiple, and multiple sedimentation stills 15 adopt stringConnection or parallel way connect. Multiple sedimentation still 15 tandem energies sedimentation catalyst step by step, further separates catalyst, multiple sedimentationsStill 15 parallel connections can be shared the load of sedimentation still 15 in the time that 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, enter from reactor 4 caprolactam water solutionsMaterial mouth 2 enters into liquid phase distributor 5, enters reactor 4 after liquid phase distributor 5. Meanwhile, hydrogen enters from hydrogen feed mouth 7Hydrogen distribution device 6, enters into reactor 4 through Hydrogen distribution device 6. Hydrogen and caprolactam water solution are at reactor agitator 1Fully reaction fast under uniform stirring. Reaction temperature is controlled at 90 DEG C. Reaction afterproduct exports 8 overflows from reactor product, logicalCross pipeline and flow to sedimentation still charging aperture, enter sedimentation still 15. Under the effect of sedimentation still agitator 13 and baffle plate 12, catalyst is heavyAt the bottom of dropping to still, by sedimentation still catalyst outlet through slush pump 9 by catalyst transport to reactor 4, reaction clear liquid through sedimentation stillProduct outlet 11 is flowed out. The pressure of controlling whole reaction system by controlling gaseous phase outlet 10 maintains 0.7MPa. Right aboveOne embodiment of the present of invention have been described in detail, but described content is only the preferred embodiment of this technology, can not be considered toBe used for limiting practical range of the present invention. All equalization variation and improvement etc. of doing according to the present patent application scope, all should still belong toWithin patent covering scope of the present invention.
Claims (3)
1. for a hydrogenation reaction device for refined caprolactam, it is characterized in that, comprise reaction system and catalyst sedimentationRecovery 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, described reactor(4) be also provided with reactor charging aperture, reactor product outlet (8); Described reactor charging aperture comprises hydrogen feed mouth (7) and ownLactam aqueous solution charging aperture (2); Described hydrogen feed mouth (7) is arranged on described reactor (4) bottom, described hydrogen feed mouth(7) be also provided with gaseous distributer (6), described gaseous distributer (6) is positioned at described reactor (4) bottom, described caprolactamAqueous 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 atDescribed reactor (4) bottom;
The stirring vane (3) of described reactor agitator (1) is single-stage or multistage blade; Stirring of described sedimentation still agitator (13)Mixing blade (14) is single-stage or multistage blade;
Described catalyst sedimentation recovery system comprises sedimentation still (15) and is built in the sedimentation still agitator (13) of described sedimentation still,Described sedimentation still (15) is provided with sedimentation still charging aperture, the outlet of sedimentation still product (11), sedimentation still catalyst outlet, gaseous phase outlet(10) and baffle plate (12), described gaseous phase outlet (10) is installed automatic pressure instrument;
Described reactor product outlet (8) is connected with described sedimentation still charging aperture by pipeline, described sedimentation still catalyst outletBe connected with described reactor charging aperture by pipeline, on the pipeline between sedimentation still catalyst outlet and described reactor charging apertureBe provided with slush pump (9);
Sedimentation still (15) inner surface is provided with baffle plate (12), and reaction afterproduct turns to upper fortune at sedimentation still agitator (13) effect backspinMoving, catalyst moves downward under the baffling effect of baffle plate (12), falls to faster sedimentation still (15) bottom.
2. hydrogenation reaction device as claimed in claim 1, is characterized in that, described reactor (4) is one or more; Described manyIndividual reactor (4) adopts serial or parallel connection mode to connect.
3. hydrogenation reaction device as claimed in claim 1, is characterized in that, described sedimentation still (15) is one or more; Described manyIndividual sedimentation still (15) adopts serial or parallel connection mode to connect.
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| 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 |
| 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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| CN1696087A (en) * | 2005-05-17 | 2005-11-16 | 中国神马集团有限责任公司 | Equipment for producing cyclohexenol through benzene plus hydrogen |
| CN101712621B (en) * | 2009-09-02 | 2012-10-31 | 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 |
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Owner name: CHINA PINGMEI SHENMA GROUP NYLON TECHNOLOGY CO., L Effective date: 20140806 |
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Effective date of registration: 20140806 Address after: 467000 No. 63, middle Jianshe Road, Pingdingshan, Henan Applicant after: Shenma Industrial Co., Ltd. Applicant after: Nylon Science and Technology Ltd. of China Ping Meishen horse group Address before: 467000 No. 63, middle Jianshe Road, Pingdingshan, Henan Applicant before: Shenma Industrial Co., Ltd. |
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