CN206089509U - Catalytic hydrogenation serialization apparatus for producing - Google Patents

Abstract

The utility model discloses a catalytic hydrogenation serialization apparatus for producing, include and connect gradually just inclosed melt zone, reation kettle hydrogenation section, catalyst autosegregation and the section of returning, fixed bed reactor hydrogenation section through the pipeline, the catalyst autosegregation and the section of returning are including two sets of parallelly connected catalyst autosegregation equipment. The utility model discloses can realize automated control continuous production, the production procedure is short, reduces the energy consumption, improves production efficiency, does not need subsequent processing, reduces the energy consumption, can produce the hydrogenation product of high quality, high yield. Simultaneously, the totally -enclosed of serialization production process, operation environment is good, can reduce to the harm of the person with to the pollution of environment.

Description

Catalytic hydrogenation continuous production device

Technical field

This utility model is related to a kind of chemical process, and in particular to a kind of catalytic hydrogenation continuous production device.

Background technology

At present, catalytic hydrogenation production is substantially using batch tank reactor or continuous tank reactor, Huo Zhegu Fixed bed reactor, or fluidized-bed reactor.Batch tank reactor, advantage is flexible operation, it is easy to different operating condition and Product variety, it is adaptable to small lot, multi items, response time longer production；Have the disadvantage the discontinuous production being interrupted, often The properties of product of batch reaction are affected the presence of fluctuation by operating.Although continuous tank reactor flow reactor can the company of realization Continuous production, however it is necessary that more reactors in series or parallel connection, but is only suitable for special reaction, for prolonging with the trans time Long side reaction increases or in the not high hydrogenation reaction of complete mixing flow state response selectivity.There is reaction in itself in fixed bed reactors Efficiency is low, the big shortcoming of disposable loaded catalyst, can not solve very well to move heat problem simultaneously for hydrogenation reaction.

Hexahydrobenzoic acid is a kind of important chemical and medicine industry intermediate, is obtained from benzoic acid or sodium benzoate catalytic hydrogenation. It can be used for the synthesis of light curing agent 184, while being also efficient ultraviolet light polymerization initiator and non-flavescence initiator, sulfuration rubber The solubilizing agent of glue, the clarifier of oil and medicine intermediate, as resisted pregnant 392 and treatment schistosomicide new drug praziquantel for medicine Synthesis.Additionally, benzoic acid hydrogenation synthesizing cyclohexane 1 alkane formic acid is also SNIA companies toluene method prepares caprolactam technology route (SNIA Technique) important step.Industrially, benzoic acid hydrogenation technique is mainly with Pd/C as catalyst, at 165 DEG C or so, 1.2- Under the conditions of 14MPa, carry out in tank reactor, mainly have hydrogenation of carboxylic acids to generate alcohol, carboxylic acid decarboxylic reaction in course of reaction and generate The side reactions such as CO2 and CO.Wherein, by-product CO and CO2 easily adsorb by force on Pd surfaces, make catalyst poisoning, therefore course of reaction In generally must use suitable method, add appropriate auxiliary agent, protection major catalyst, reaction condition is also harsher.

Chinese patent literature CN101092349 discloses a kind of hydrogenation process for benzoic acid of addition Ru/C.Auxiliary agent uses 5% The Ru/C of left and right, consumption accounts for the 2～10% of Pd/C weight, 150～170 DEG C of reaction temperature, under 1.0～6MPa, the series connection of the kettles of Jing tetra- After reaction, conversion ratio is up to 99%.After the method, device without outer row's catalyst and auxiliary agent, without Jing often in system Fresh catalyst and auxiliary agent is added, catalyst recovered frequency is reduced, while improve the benzoic acid hydrogenation of Pd/C catalyst Activity, increases the working ability of device.

Chinese patent literature CN103599795A disclose a kind of catalyst of benzoic acid hydrogenation preparing cyclohexane formic acid and its Preparation method and application, using fixed bed reactors, catalyst includes carrier, auxiliary agent and activated carbon composition Pd.Carrier is from bubble Foam nickel or activated carbon.

Chinese patent literature CN100522919C discloses a kind of method of benzoic acid hydrogenation, in Pd/C catalyst and Ru/C Under conditions of auxiliary agent, benzoic acid and the hydrogen of melting carry out in the reactor hydrogenation reaction, and mixture is through spinning liquid point after reaction From and centrifugation, the turbid liquid containing high concentration catalyst and auxiliary agent loops back reactor, and the clear liquid isolated enters vaporizer Further separate, the catalyst and auxiliary agent isolated completely returns to reactor assembly.

Chinese patent literature CN1224605C discloses hydrogenation process for benzoic acid, will melting benzoic acid in Pd/C catalyst and In the presence of nickel auxiliary agent, after hydrogen haptoreaction, using spinning liquid, centrifugation and Magneto separate three-level separation process, by catalyst from mixed Reactor is separated and looped back in compound, and the turbid liquid wherein after rotary filter press loops back reactor, and clear liquid enters whizzer, The catalyst of separated rear lower loops back reactor, and upper clear supernate carries out Magneto separate, isolates Ni-based promoter and loops back Reactor.

Chinese patent literature CN1195725C discloses a kind of method of benzoic acid selective hydrogenation hexahydrobenzoic acid, will The hydrogenation catalyst that hydrogen is placed in fixed bed reactors with liquid benzoic acid is contacted, and is 0.5 in 160～220 DEG C, Hydrogen Vapor Pressure ～4.0MPa, 0.1～15.0h of air speed^-1, carry out trickle bed reaction under conditions of hydrogen and benzoic acid mol ratio 3～15.Catalyst For the faintly acid aluminium oxide of Supported Pt Nanoparticles.

Chinese patent literature CN100352797C discloses a kind of method of synthesizing cyclohexyl formic acid by benzoic acid hydrogenation, benzene first Acid in the presence of carrier-borne transition metal rhodium catalyst, solvent-free, in supercritical carbon dioxide and hexahydrobenzoid acid, in temperature Initial ring catalytic reaction is contacted with hydrogen under (20～80 DEG C of temperature, 1～10MPa of pressure) under the reaction condition of sum.Profit after reaction Dissolubility with hexahydrobenzoid acid in supercritical carbon dioxide is extracted, and catalyst is separated with product.

In sum, nowadays SNIA methods production hexahydrobenzoic acid commercial plant has stopped production in China, benzoic acid catalysis hydrogen Metaplasia is produced the production of hexahydrobenzoic acid and there is many defects, and the need multi-floating bodies, the complicated catalyst of some needs having are separated Equipment, purification apparatus after some needs hydrogenation, what is had needs super critical condition, and using single-reactor continuous metaplasia cannot be met Product demand, although multi-floating bodies can realize continuous production, but because reactor is complete mixed reaction, and cause through multi-floating bodies Response time is long, reduces product yield, quality variation.Simultaneously because benzoic acid easily distils, hexahydrobenzoic acid abnormal smells from the patient is disliked Smelly, opening wide system or intermediate steps closed all can not can cause the injury to body and the pollution to air, simultaneously because benzene There is easy decarboxylation in formic acid hydrogenation, in addition to catalyst poisoning is caused, can also cause hexahydrobenzoic acid yield to reduce, production cost Increase.Separation and purification and the loss problem of solvent can be caused if adding organic solvent to be reacted, increases production cost And operational hazards.Therefore in the urgent need to designing a kind of new continuous catalytic hydrogenation production technology and equipments, to overcome existing life The deficiency of production. art and equipment.

Utility model content

Technical problem to be solved in the utility model is to provide a kind of catalytic hydrogenation continuous production device, and it can be real Existing Automated condtrol is continuously produced, and improves efficiency, it is not necessary to subsequent treatment, reducing energy consumption, produce high-quality, the six of high yield pulp1 Hydrogen benzoic acid product.

To solve above-mentioned technical problem, the technical solution of this utility model catalytic hydrogenation continuous production device is：

Including being sequentially connected by pipeline and closed melt zone 1, reactor hydrogenation section 2, catalyst is automatically separated and returns Return section 3, fixed bed reactors hydrogenation section 4；Catalyst is automatically separated and return phase 3 includes that two sets of catalyst in parallel are automatically separated Equipment；Raw material is melted in melt zone 1；Fused raw material enters reactor and is hydrogenated with section 2, sends out with hydrogen in the presence of hydrogenation catalyst Raw hydrogenation reaction, material after being hydrogenated with；After hydrogenation material be automatically separated into catalyst and return phase 3 wherein a set of catalysis Agent automatic separation equipment, filtrate and catalyst residue Jing after filtering and obtain reactor hydrogenation, catalyst residue returns reactor, instead Answer filtrate after kettle hydrogenation to enter fixed bed reactors and be hydrogenated with section 4, carry out under the catalytic action of fixed bde catalyst 44 with hydrogen Reaction, obtains hydrogenation product.

The melt zone 1 includes the first hermetic container 11 and the second hermetic container 12, and the first hermetic container 11 is close with second Close and pipeline 14 is provided between container 12；First hermetic container 11 offers material inlet；Second hermetic container 12 passes through raw material Conveyance conduit coupled reaction kettle is hydrogenated with the high-pressure hydrogenation reactor 21 of section 2；Feedstock transportation pump 13 is provided with feedstock transportation pipeline.

The reactor hydrogenation section 2 includes high-pressure hydrogenation reactor 21, and high-pressure hydrogenation reactor 21 offers feed(raw material)inlet 24th, hydrogen inlet 23, catalyst inlet 22, the first catalyst return entrance 27, the second catalyst and return thing after entrance 25, hydrogenation Material outlet 26, gas drain；The feed(raw material)inlet 24 connects feedstock transportation pipeline.

The high-pressure hydrogenation reactor 21 is equipped with temperature monitoring, pressure detector, automatic control heating device, cooling One or more in device, agitating device.

The high-pressure hydrogenation reactor 21 adopts magnetic agitation；The alr mode of high-pressure hydrogenation reactor 21 is stirred for self-priming Mix.

The catalyst is automatically separated and return phase 3 includes the first catalyst automatic separation equipment 31, the second catalyst certainly Dynamic separation equipment 32, pans 33, the first catalyst automatic separation equipment 31 and the second catalyst automatic separation equipment 32 are constituted Described two sets catalyst automatic separation equipments in parallel；

Filter element is provided with first catalyst automatic separation equipment 31；Filter element is by 31 points of the first catalyst automatic separation equipment It is divided into filter ante-chamber and filter back cavity；The filter ante-chamber of the first catalyst automatic separation equipment 31 connects high-pressure hydrogenation reactor by pipeline Material outlet 26 after 21 hydrogenation；The filter ante-chamber of the first catalyst automatic separation equipment 31 is connected by the first solution export pipeline The delivery outlet of pans 33, is provided with the first solution transfer pump 37 on the first solution export pipeline；First catalyst is automatically separated The filter ante-chamber of equipment 31 connects the first catalyst and receives tank 35；First catalyst receives tank 35 and passes through the first catalyst export pipeline Connection high-pressure hydrogenation reactor 21；The first catalyst transport pump 39 is provided with first catalyst export pipeline；First catalyst The filter back cavity of automatic separation equipment 31 connects the input port of pans 33 by pipeline；First catalyst automatic separation equipment 31 Filter back cavity is also connected with nitrogen purge line；

Filter element is provided with second catalyst automatic separation equipment 32；Filter element is by 32 points of the second catalyst automatic separation equipment It is divided into filter ante-chamber and filter back cavity；The filter ante-chamber of the second catalyst automatic separation equipment 32 connects high-pressure hydrogenation reactor by pipeline Material outlet 26 after 21 hydrogenation；The filter ante-chamber of the second catalyst automatic separation equipment 32 is connected by the second solution export pipeline The delivery outlet of pans 33, is provided with the second solution transfer pump 36 on the second solution export pipeline；Second catalyst is automatically separated The filter ante-chamber of equipment 32 connects the second catalyst and receives tank 34；Second catalyst receives tank 34 and passes through the second catalyst export pipeline Connection high-pressure hydrogenation reactor 21；The second catalyst transport pump 38 is provided with second catalyst export pipeline；Second catalyst The filter back cavity of automatic separation equipment 32 connects the input port of pans 33 by pipeline；Second catalyst automatic separation equipment 32 Filter back cavity is also connected with nitrogen purge line.

The filter element is high technology ceramics filter element or precision metallic sintered filter core.

The pans 33 are equipped with automatic decompression device.

First solution transfer pump 37, the first catalyst transport pump 39, the second solution transfer pump 36, the second catalyst are defeated Pump 38 is sent to be dosing pump.

The fixed bed reactors hydrogenation section 4 includes fixed bed reactors 42, condenser 45, gas-liquid separator 46, fixed Gas-liquid distributor 43 is provided with bed reactor 42；The input port of fixed bed reactors 42 connects catalyst by Location Detection of Medium Transportation Pipeline Be automatically separated and return phase 3 pans 33, material-handling pump 41 is provided with Location Detection of Medium Transportation Pipeline；Fixed bed reactors 42 Delivery outlet connects the input port of condenser 45, the delivery outlet connection gas-liquid separator 46 of condenser 45；Gas-liquid separator 46 is connected Hydrogen pipeloop, is provided with hydrogen gas circulating pump 47 on hydrogen pipeloop；Fixed bed reactors 42 connect hydrogen inlet manifold line, Hydrogen inlet manifold line and hydrogen pipeloop connect outside constant pressure hydrogen gas lines 48 jointly.

What this utility model can reach has the technical effect that：

This utility model can realize that Automated condtrol is continuously produced, and production procedure is short, reducing energy consumption, improve production effect Rate, it is not necessary to subsequent treatment, reducing energy consumption can produce high-quality, hydrogenation product in high yield.Meanwhile, continuous prodution mistake Journey total enclosing, operating environment is excellent, can reduce harm and the pollution to environment to the person.

Description of the drawings

This utility model is described in further detail with reference to the accompanying drawings and detailed description：

Fig. 1 is the schematic diagram of this utility model catalytic hydrogenation continuous production device；

Fig. 2 is the flow chart that catalytic hydrogenation continuous production method is carried out using this utility model.

Description of reference numerals in figure：

1 is melt zone, and 2 is that reactor is hydrogenated with section,

3 are automatically separated and return phase for catalyst, and 4 is that fixed bed reactors are hydrogenated with section,

11 is the first hermetic container, and 12 is the second hermetic container,

13 is feedstock transportation pump, and 14 is pipeline,

21 is high-pressure hydrogenation reactor, and 22 is catalyst inlet,

23 is hydrogen inlet, and 24 is feed(raw material)inlet,

25 is that the second catalyst returns entrance, and 26 are material outlet after hydrogenation,

27 is that the first catalyst returns entrance,

31 is the first catalyst automatic separation equipment, and 32 is the second catalyst automatic separation equipment,

33 is pans, and 34 is that the second catalyst receives tank,

35 is that the first catalyst receives tank, and 36 is the second solution transfer pump,

37 is the first solution transfer pump, and 38 is the second catalyst transport pump,

39 is the first catalyst transport pump,

41 is material-handling pump, and 42 is fixed bed reactors,

43 is gas-liquid distributor, and 44 is fixed bde catalyst,

45 is condenser, and 46 is gas-liquid separator,

47 is hydrogen gas circulating pump, and 48 are outside constant pressure hydrogen gas lines.

Specific embodiment

As shown in figure 1, this utility model catalytic hydrogenation continuous production device, for realizing prepared by benzoic acid catalytic hydrogenation The continuous production of hexahydrobenzoic acid；Including being sequentially connected by pipeline and closed melt zone 1, reactor hydrogenation section 2, catalyst It is automatically separated and return phase 3, fixed bed reactors hydrogenation section 4；Starting benzoic acid sequentially passes through melt zone 1, reactor hydrogenation section 2nd, catalyst is automatically separated and return phase 3, fixed bed reactors hydrogenation section 4, obtains hydrogenation product hexahydrobenzoic acid；Whole material In air-tight state, material realizes automatic transport.

Melt zone 1 includes the first hermetic container 11 and the second hermetic container 12, and pipeline 14 is provided between the two；First is close Closing the hermetic container 12 of container 11 and second can adopt automatic temperature control heating；By controlling whether the connection of pipeline 14 is realized continuously Charging；Realize that the first hermetic container 11 is isobaric with the second hermetic container 12 when pipeline 14 is connected；

Second hermetic container 12 connects the feed(raw material)inlet 24 of high-pressure hydrogenation reactor 21 by feedstock transportation pipeline；Raw material is defeated Send and be provided with pipeline feedstock transportation pump 13；Feedstock transportation pump 13 is preferably dosing pump；

Reactor hydrogenation section 2 includes high-pressure hydrogenation reactor 21, and high-pressure hydrogenation reactor 21 offers feed(raw material)inlet 24, hydrogen Gas entrance 23, catalyst inlet 22, the second catalyst return material after entrance 25, the first catalyst return entrance 27, hydrogenation and go out Mouth 26 and gas drain；All gateways are equipped with valve；Feed(raw material)inlet 24, the second catalyst return entrance 25, first Catalyst returns entrance 27 and is provided with dosing pump realization control；Hydrogen inlet 23 is provided with self-measuring device, and using outside constant pressure Into；

Hydrogen inlet 23 and feed(raw material)inlet 24 are passed through the bottom of reactor 21, and material outlet 26 is located at reactor 21 after hydrogenation Top, catalyst inlet 22 is located at the top of reactor 21, and the second catalyst returns the catalyst of entrance 25 and first and returns entrance 27 It is located at the top of reactor 21；

High-pressure hydrogenation reactor 21 may be equipped with temperature monitoring, pressure detector, automatic control heating device and cold But device and agitating device；

High-pressure hydrogenation reactor 21 adopts magnetic agitation, and alr mode is self-priming stirring；

Catalyst is automatically separated and return phase 3 includes that the first catalyst automatic separation equipment 31, the second catalyst divide automatically From equipment 32, pans 33, high technology ceramics filter element is provided with the first catalyst automatic separation equipment 31 or precision metallic burns Knot filter element；First catalyst automatic separation equipment 31 is divided into filter ante-chamber and filter back cavity by filter element；First catalyst is automatically separated The filter ante-chamber of equipment 31 connects material outlet 26 after the hydrogenation of high-pressure hydrogenation reactor 21 by pipeline；First catalyst divides automatically Filter ante-chamber from equipment 31 connects the delivery outlet of pans 33 by the first solution export pipeline, sets on the first solution export pipeline It is equipped with the first solution transfer pump 37；The filter ante-chamber of the first catalyst automatic separation equipment 31 connects the first catalyst and receives tank 35； First catalyst is received tank 35 and is returned by the first catalyst that the first catalyst export pipeline connects high-pressure hydrogenation reactor 21 Entrance 27；The first catalyst transport pump 39 is provided with first catalyst export pipeline；First catalyst automatic separation equipment 31 Filter back cavity by pipeline connection pans 33 input port；The filter back cavity of the first catalyst automatic separation equipment 31 is also connected with nitrogen Air-blowing sweeping；

High technology ceramics filter element or precision metallic sintered filter core are provided with second catalyst automatic separation equipment 32；Filter element Second catalyst automatic separation equipment 32 is divided into into filter ante-chamber and filter back cavity；Before the filter of the second catalyst automatic separation equipment 32 Chamber material outlet 26 after the hydrogenation of pipeline connection high-pressure hydrogenation reactor 21；The filter of the second catalyst automatic separation equipment 32 Ante-chamber connects the delivery outlet of pans 33 by the second solution export pipeline, and on the second solution export pipeline the second solution is provided with Delivery pump 36；The filter ante-chamber of the second catalyst automatic separation equipment 32 connects the second catalyst and receives tank 34；Second catalyst connects Closed cans 34 returns entrance 25 by the second catalyst that the second catalyst export pipeline connects high-pressure hydrogenation reactor 21；Second urges The second catalyst transport pump 38 is provided with agent export pipeline；The filter back cavity of the second catalyst automatic separation equipment 32 is by pipe Line connects the input port of pans 33；The filter back cavity of the second catalyst automatic separation equipment 32 is also connected with nitrogen purge line；

Pans 33 are equipped with automatic decompression device；

First solution transfer pump 37, the first catalyst transport pump 39, the second solution transfer pump 36, the second catalyst transport pump 38 are preferably dosing pump；

Fixed bed reactors hydrogenation section 4 includes fixed bed reactors 42, condenser 45, gas-liquid separator 46, and fixed bed is anti- The top for answering device 42 is provided with gas-liquid distributor 43；The input port of fixed bed reactors 42 connects pans by Location Detection of Medium Transportation Pipeline 33, material-handling pump 41 is provided with Location Detection of Medium Transportation Pipeline；The delivery outlet of fixed bed reactors 42 connects the input of condenser 45 Mouthful, the delivery outlet connection gas-liquid separator 46 of condenser 45；

Gas-liquid separator 46 connects hydrogen pipeloop, and hydrogen gas circulating pump 47 is provided with hydrogen pipeloop；Fixed bed Reactor 42 connects hydrogen inlet manifold line, and hydrogen inlet manifold line and hydrogen pipeloop connect outside constant pressure hydrogen gas lines jointly 48。

As shown in Fig. 2 the catalytic hydrogenation continuous production method realized using this utility model, is continuously set in closed Standby middle production hexahydrobenzoic acid (can certainly need hydrogenation material for other), comprises the following steps：

Step S1, melting step：Pipeline 14 between first hermetic container 11 and the second hermetic container 12 is cut off, Solid material benzoic acid is added in one hermetic container 11, is heated in solid-state benzoic acid by automatic control heating system (not shown) Melting；Pipeline 14 is connected, pipeline 14 makes the first hermetic container 11 isobaric with the second hermetic container 12；The benzoic acid of melting is entered The temperature control of the second hermetic container 12, the first hermetic container 11 and the second hermetic container 12 at 100～150 DEG C, the benzene of melting Formic acid is delivered to high-pressure hydrogenation reactor 21 by feedstock transportation pump 13；

Step S2, reactor hydrogenation step：It is anti-that fresh hydrogenation catalyst is added to high-pressure hydrogenation by catalyst inlet 22 Answer in kettle 21；In the presence of catalyst, the benzoic acid of melting reacts with the hydrogen for coming from hydrogen inlet 23 in high-pressure hydrogenation There is hydrogenation reaction, material after being hydrogenated with kettle 21；80～180 DEG C of controlling reaction temperature, 1～6MPa of pressure, mixing speed 600～1300r/min, stirs as self-priming stirring；

Hydrogenation catalyst is loaded catalyst, and the composition of hydrogenation catalyst includes active component, auxiliary agent and carrier；Activity Component can be one or more in Pt, Pd, Rh, Ru, Ir, Ni, Cu, Co, Fe；Auxiliary agent can for Na, K, Mg, Ca, Ba, One or more in Cr, Mn, Mo, Zn, rare earth element；Carrier can be activated carbon, modified activated carbon, aluminium oxide, modified oxygen Change one or more in aluminum, silicon oxide, molecular sieve；

Hydrogenation catalyst is powder catalyst, one or more such as in powder palladium charcoal, ruthenium charcoal, platinum charcoal, rhodium charcoal (when Other similar hydrogenation catalysts can also so be included, the acquisition scope of hydrogenation catalyst should can be pre- for those skilled in the art Expect, similarly hereinafter)；

Preferably, hydrogenation catalyst is the mixed catalyst of palladium charcoal and ruthenium charcoal, and wherein the ratio of palladium charcoal and ruthenium charcoal is 100: 0.5～5, the content of metal of palladium charcoal and ruthenium charcoal is 1～5%；

Material is catalyzed by the hydrogenated rear material outlet 26 of pressure in high-pressure hydrogenation reactor 21 into first after hydrogenation The catalyst automatic separation equipment 32 of agent automatic separation equipment 31 or second；

Step S3, catalyst are automatically separated and return to step：Material is by anti-after the hydrogenation of high-pressure hydrogenation reactor 21 Pressure in kettle is answered staggeredly to enter the first catalyst automatic separation equipment 31 and the second catalyst automatic separation equipment 32；

Material is entered after the filter ante-chamber of the first catalyst automatic separation equipment 31 after hydrogenation, is using the pressure in reactor Power, being separated by filtration through filter element obtains filtrate and catalyst residue after reactor hydrogenation；Filtrate Jing the after reactor hydrogenation The filter back cavity of one catalyst automatic separation equipment 31 enters pans 33, and catalyst residue is stayed in filter ante-chamber；In pans 33 Fraction after reactor hydrogenation in filtrate the first solution of Jing export pipeline in the presence of the first solution transfer pump 37 is back to The filter ante-chamber of the first catalyst automatic separation equipment 31, so that catalyst residue is diluted；By nitrogen purge line to The filter back cavity of one catalyst automatic separation equipment 31 is purged, and the residue that will attach to filter element outer wall is blown down, and realizes catalyst Automatically strip, to keep the filter effect of filter element；Catalyst residue enters the first catalyst and receives tank 35, and comes from centre Filtrate is uniform by the beating of magnetic agitation (not shown) after the reactor hydrogenation of tank 33, then in the first catalyst transport pump The first catalyst of Jing export pipeline returns high-pressure hydrogenation reactor 21 in the presence of 39；

Or, material is entered after the filter ante-chamber of the second catalyst automatic separation equipment 32, through the filtration of filter element after hydrogenation Separate, obtain filtrate and catalyst residue after reactor hydrogenation；The catalyst of filtrate Jing second is automatically separated and sets after reactor hydrogenation Standby 32 filter back cavity enters pans 33, and catalyst residue is stayed in filter ante-chamber；In pans 33 after reactor hydrogenation in filtrate Fraction in the presence of the second solution transfer pump 36 the second solution of Jing export pipeline be back to the second catalyst and be automatically separated The filter ante-chamber of equipment 32, so that catalyst residue is diluted；The second catalyst is automatically separated by nitrogen purge line is set Standby 32 filter back cavity is purged, and the residue that will attach to filter element outer wall is blown down, to keep the filter effect of filter element；Catalyst is residual Slag enters the second catalyst and receives tank 34, and filtrate beating is uniform after being hydrogenated with the reactor for coming from pans 33, then the The second catalyst of Jing export pipeline returns high-pressure hydrogenation reactor 21 in the presence of two catalyst transport pumps 38；

Above-mentioned two groups of filtration systems automatically switch, when the first catalyst automatic separation equipment 31 works, the second catalyst Catalyst in automatic separation equipment 32 returns high-pressure hydrogenation reactor 21, staggeredly carries out, with the seriality for ensureing to react；

Step S4, fixed bed reaction step：Material-handling pump 41 will be big in filtrate after reactor hydrogenation in pans 33 The top of fixed bed reactors 42 is partially driven into, fixed bed reactors 42 are built with fixed bde catalyst 44；Outside constant pressure hydrogen Pipeline 48 is input into hydrogen in fixed bed reactors 42, the catalysis of filtrate and hydrogen in fixed bde catalyst 44 after reactor hydrogenation Reacted under effect；Reaction temperature control in fixed bed reactors 42 at 80～170 DEG C, 1～6MPa of pressure；

Fixed bde catalyst 44 is loaded catalyst, and the composition of fixed bde catalyst includes active component, auxiliary agent and load Body；Active component can be one or more in Pt, Pd, Rh, Ru, Ir, Ni, Cu, Co, Fe；Auxiliary agent can for Na, K, Mg, One or more in Ca, Ba, Cr, Mn, Mo, Zn, rare earth element；Carrier can for activated carbon, modified activated carbon, aluminium oxide, One or more in modified aluminas, silicon oxide, molecular sieve；

Fixed bde catalyst 44 be beaded catalyst, such as one or more in graininess palladium charcoal, ruthenium charcoal, platinum charcoal, rhodium charcoal；

Preferably, fixed bde catalyst 44 is particulate supported type palladium catalyst charcoal and ruthenium charcoal mixed catalyst, wherein palladium The ratio of charcoal and ruthenium charcoal is 100:0.5～10, the content of metal of palladium charcoal and ruthenium charcoal is 1～5%；

Hydrogenation reaction product passes sequentially through condenser 45 and gas-liquid separator 46, through condensation and gas-liquid separation, obtains hydrogen Change product hexahydrobenzoic acid；

Hydrogen is circulated by hydrogen gas circulating pump 47, and supplements consumed hydrogen by outside constant pressure hydrogen gas lines 48.

Here description of the present utility model and application are illustrative, are not wishing to be limited in scope of the present utility model In stating embodiment.The deformation and change of embodiments disclosed herein is possible, such as melt zone can be material and solvent Mixing, catalyst is automatically separated section and is changed to magnetic force or cyclone separator according to using the difference of catalyst, and catalytic hydrogenation connects Continuousization process units equally can be real for those skilled in the art with other hydrogenation materials of continuous prodution The replacement applied and equivalent various parts are known.It should be appreciated by the person skilled in the art that new without departing from this practicality In the case of the spirit or essential characteristics of type, this utility model can in other forms, structure, arrangement, ratio, and use other Component, material and part are realizing.In the case of without departing from this utility model scope and spirit, can be to described herein Embodiment carries out other deformations and changes.

Claims (10)

1. a kind of catalytic hydrogenation continuous production device, it is characterised in that：Including being sequentially connected by pipeline and closed melting Section (1), reactor are hydrogenated with section (2), catalyst is automatically separated and return phase (3), fixed bed reactors hydrogenation section (4)；Catalyst It is automatically separated and return phase (3) is including two sets of catalyst automatic separation equipments in parallel；

Raw material is melted in melt zone (1)；Fused raw material enters reactor hydrogenation section (2), with hydrogen in the presence of hydrogenation catalyst There is hydrogenation reaction, material after being hydrogenated with gas；After hydrogenation material alternately enter catalyst be automatically separated and return phase (3) two Set catalyst automatic separation equipment, obtains filtrate and catalyst residue after reactor hydrogenation, and catalyst residue returns reactor, instead Filtrate after kettle hydrogenation is answered to enter fixed bed reactors hydrogenation section (4), with hydrogen under the catalytic action of fixed bde catalyst (44) Reacted, obtained hydrogenation product.

2. catalytic hydrogenation continuous production device according to claim 1, it is characterised in that：The melt zone (1) includes First hermetic container (11) and the second hermetic container (12), are arranged between the first hermetic container (11) and the second hermetic container (12) There is pipeline (14)；First hermetic container (11) offers material inlet；Second hermetic container (12) is connected by feedstock transportation pipeline Connect the high-pressure hydrogenation reactor (21) of reactor hydrogenation section (2)；Feedstock transportation pump (13) is provided with feedstock transportation pipeline.

3. catalytic hydrogenation continuous production device according to claim 1, it is characterised in that：The reactor is hydrogenated with section (2) including high-pressure hydrogenation reactor (21), high-pressure hydrogenation reactor (21) offer feed(raw material)inlet (24), hydrogen inlet (23), Catalyst inlet (22), the first catalyst return entrance (27), the second catalyst and return material outlet after entrance (25), hydrogenation (26)；The feed(raw material)inlet (24) connects feedstock transportation pipeline.

4. catalytic hydrogenation continuous production device according to claim 3, it is characterised in that：The high-pressure hydrogenation reactor (21) equipped with the one kind in temperature monitoring, pressure detector, automatic control heating device, chiller, agitating device or It is several.

5. catalytic hydrogenation continuous production device according to claim 3, it is characterised in that：The high-pressure hydrogenation reactor (21) magnetic agitation is adopted；The alr mode of high-pressure hydrogenation reactor (21) is self-priming stirring.

6. catalytic hydrogenation continuous production device according to claim 1, it is characterised in that：The catalyst is automatically separated And return phase (3) is including the first catalyst automatic separation equipment (31), the second catalyst automatic separation equipment (32), pans (33), the first catalyst automatic separation equipment (31) and the second catalyst automatic separation equipment (32) constitute two sets of parallel connections Catalyst automatic separation equipment；

Filter element is provided with first catalyst automatic separation equipment (31)；Filter element divides the first catalyst automatic separation equipment (31) It is divided into filter ante-chamber and filter back cavity；The filter ante-chamber of the first catalyst automatic separation equipment (31) connects high-pressure hydrogenation reaction by pipeline Material outlet (26) after the hydrogenation of kettle (21)；The filter ante-chamber of the first catalyst automatic separation equipment (31) is exported by the first solution The delivery outlet of pipeline connection pans (33), is provided with the first solution transfer pump (37) on the first solution export pipeline；First urges The filter ante-chamber of agent automatic separation equipment (31) connects the first catalyst and receives tank (35)；First catalyst receives tank (35) and passes through First catalyst export pipeline connection high-pressure hydrogenation reactor (21)；The first catalyst is provided with first catalyst export pipeline Delivery pump (39)；The filter back cavity of the first catalyst automatic separation equipment (31) connects the input port of pans (33) by pipeline；

Filter element is provided with second catalyst automatic separation equipment (32)；Filter element divides the second catalyst automatic separation equipment (32) It is divided into filter ante-chamber and filter back cavity；The filter ante-chamber of the second catalyst automatic separation equipment (32) connects high-pressure hydrogenation reaction by pipeline Material outlet (26) after the hydrogenation of kettle (21)；The filter ante-chamber of the second catalyst automatic separation equipment (32) is exported by the second solution The delivery outlet of pipeline connection pans (33), is provided with the second solution transfer pump (36) on the second solution export pipeline；Second urges The filter ante-chamber of agent automatic separation equipment (32) connects the second catalyst and receives tank (34)；Second catalyst receives tank (34) and passes through Second catalyst export pipeline connection high-pressure hydrogenation reactor (21)；The second catalyst is provided with second catalyst export pipeline Delivery pump (38)；The filter back cavity of the second catalyst automatic separation equipment (32) connects the input port of pans (33) by pipeline.

7. catalytic hydrogenation continuous production device according to claim 6, it is characterised in that：The filter element is high technology ceramics Filter element or precision metallic sintered filter core.

8. catalytic hydrogenation continuous production device according to claim 6, it is characterised in that：The pans (33) are equipped with Automatic decompression device.

9. catalytic hydrogenation continuous production device according to claim 6, it is characterised in that：First solution transfer pump (37), the first catalyst transport pump (39), the second solution transfer pump (36), the second catalyst transport pump (38) are dosing pump.

10. catalytic hydrogenation continuous production device according to claim 1, it is characterised in that：The fixed bed reactors Hydrogenation section (4) includes being set in fixed bed reactors (42), condenser (45), gas-liquid separator (46), fixed bed reactors (42) There is gas-liquid distributor (43)；The input port of fixed bed reactors (42) by Location Detection of Medium Transportation Pipeline connect catalyst be automatically separated and The pans (33) of return phase (3), are provided with material-handling pump (41) on Location Detection of Medium Transportation Pipeline；Fixed bed reactors (42) it is defeated The input port of outlet connection condenser (45), delivery outlet connection gas-liquid separator (46) of condenser (45)；Fixed bed reactors (42) hydrogen inlet manifold line is connected.