CN207981116U - A kind of slurry bed circulatory flow reactor - Google Patents
A kind of slurry bed circulatory flow reactor Download PDFInfo
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- CN207981116U CN207981116U CN201721586345.5U CN201721586345U CN207981116U CN 207981116 U CN207981116 U CN 207981116U CN 201721586345 U CN201721586345 U CN 201721586345U CN 207981116 U CN207981116 U CN 207981116U
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Abstract
A kind of slurry bed circulatory flow reactor, including tedge (1), the widened expanding reach of tedge top caliber (2), solid-liquid separator (10) and the down-comer (3) being sequentially communicated, the solid-liquid separator (10) bottom is connected to through down-comer (3) with tedge (1) bottom；Setting guide shell (5) and baffle plate (6) in the expanding reach (2), the guide shell is the cylinder that from top to bottom diameter reduces, the baffle plate is made of at least one circular tablet, between expanding reach and guide shell, setting filter assemblies (11) in the solid-liquid separator (10), and through filter assemblies setting purified liquor outlet (16), described tedge (1) bottom is equipped with feed(raw material)inlet (4), and gas vent (15) is equipped at the top of the expanding reach (2).Slurry bed circulatory flow reactor provided by the utility model is suitable for the reaction of gas-liquid-solid three-phase, and gas-liquid-solid three-phase separative efficiency is high, can avoid overreaction, be particularly suitable in anthraquinone legal system hydrogen peroxide process.
Description
Technical field
The utility model is related to a kind of paste state bed reactors, more specifically to a kind of slurry suitable for hydrogenation reaction
State bed external loop reactor.
Background technology
Hydrogen peroxide is a kind of important Inorganic Chemicals, it is widely used in papermaking, weaving, chemicals synthesis, army
The numerous areas such as work, electronics, food processing, medicine, cosmetics, environmental protection, metallurgy.Hydrogen peroxide generates water and oxygen after decomposing
Gas is a kind of green chemical to environment non-secondary pollution.At present both at home and abroad generally using the anthraquinone life for carrying out hydrogen peroxide
Production.Process for prepairng hydrogen peroxide by anthraquinone under the effect of the catalyst, will be dissolved with hydrogen using anthraquinone derivative as working material
Anthraquinone derivative hydrogenation in organic solvent, generates corresponding hydrogen anthraquinone.Then, hydrogen anthraquinone oxidation generates hydrogen peroxide and anthracene
Quinone derivative.Finally, it uses water to extract the hydrogen peroxide in organic solvent and obtains certain density aqueous hydrogen peroxide solution as production
Product, the working solution containing anthraquinone derivative and organic solvent are then recycled.Wherein, the efficiency of anthraquinone hydrogenation process is directly determined
The yield and concentration for determining hydrogen peroxide, it is marginal to the production tool of entire hydrogen peroxide.The country is in anthraquinone hydrogenation mistake at present
The most commonly used is down-type fixed-bed reactors, i.e. trickle bed reactor in journey, but there are catalyst profits for fixed bed reactors
With efficiency is low, reaction selectivity is low, temperature distribution is non-uniform in bed, catalyst part liquid holdup is big and working solution degradation is serious
The problem of.Hydrogenation process is carried out using fixed bed reactors, hydrogen effect is typically only 6~7g/LHydride.And use gas and liquid flowing upward
The reactor of movement is the optimal selection for carrying out anthraquinone derivative hydrogenation process.Such reactor includes the reaction of tubular type suspension bed
Device, bubbling bed reactor and paste state bed reactor.During gas-liquid two-phase cocurrent flows up, working solution and hydrogen anthraquinone are mixed
Solution is closed as continuous phase, and hydrogen (or hydrogen and inert gas gaseous mixture) is used as dispersed phase, can both improve working solution
The utilization rate for the treatment of capacity and catalyst increases anthraquinone conversion ratio, and it is big to overcome fixed bed catalyst bed part liquid holdup, temperature
The problem of working solution is degraded caused by degree is unevenly distributed.The newly-built large-scale hydrogen peroxide manufacture device of foreign countries generally uses up flow type
Fluid bed carries out hydrogenation, and hydrogen effect is generally up to 12g/LHydrideMore than.
US4428923 discloses a kind of tubular type suspension bed hydrogenation reactor system of process for prepairng hydrogen peroxide by anthraquinone, reaction
Device is connected between horizontal tube and vertical tube by elbow at pass-over offset system, each section of pipe nominal diameter having the same.Pipe is outer set
Pipe is for heating and cooling down, and hydrogenation process with regard to carrying out in the reactor.Working solution enters with hydrogen before hydrogenator, first through one
Venturi mixer premixes, and catalyst continuously flows together with working solution, and working solution is reacted with hydrogen, is passed through after the reaction
A separator is crossed, catalyst and hydride are subjected to preliminary separation；A dedicated hydrogenation liquid filter must be used after separation
Hydride is detached again with catalyst, hydrogenation efficiency 12g/LHydride。
CN1298369A provides a kind of bubbling bed reactor.Reactor is preferably vertical type bubbling tower, in reactor at least
It is partial comprising hydraulic diameter between 1 to 10mm through-hole or flow path member, usually bed, knitted fabric, open-celled foams or
Filler, usually with structure as Sulzer BX earthfill rockfill concrete riprap RCCs, so that working solution or hydrogen pass through.Ensure the side wall of flow path member
Roughness is that 0.5 to 5 times of catalyst average grain diameter, working solution and gas phase enter reactor together by reactor lower part, is being urged
Agent effect is lower to carry out hydrogenation reaction, and the separation that equipment for separating liquid from solid carries out hydride and catalyst is entered after reaction.The reaction
System can carry out the operation of interval and continuous two ways, and hydrogenation efficiency is up to 15g/LHydrideMore than.
The above technology is analyzed, current process for prepairng hydrogen peroxide by anthraquinone hydrogenates on-fixed bed reactor, and there are Railway Projects：
The gas-liquid-solid separating effect of reactor is bad, and larger pressure is caused to operations such as subsequent filterings；Fluid flows in reactor
State is disorderly, be easy to cause that have a hydrogenation reaction excessive, leads to catalyst inactivation, reduces hydrogen effect；It is separated by solid-liquid separation and needs additionally
Power-equipment not only increases energy consumption, and increases the abrasion probability to catalyst.Compare above-mentioned reactor, slurry reactor
Device eliminates the influence spread in catalyst, tool due to catalyst particle diameter very little (generally tens microns or smaller)
There are very high reaction specific surface and activity, the dosage of catalyst can be greatly reduced, had evenly inside simultaneous reactions device
Flow regime has good technology development prospect.
Utility model content
The technical problem to be solved by the present invention is to provide a kind of slurry bed circulatory flow reactors.
The utility model provides a kind of slurry bed circulatory flow reactor, including tedge 1, the tedge upper tube being sequentially communicated
The widened expanding reach 2 of diameter, solid-liquid separator 10 and down-comer 3,10 bottom of solid-liquid separator is through down-comer 3 and tedge
1 bottom is connected to；Setting guide shell 5 and baffle plate 6 in the expanding reach 2, the guide shell reduce for diameter from top to bottom
Cylinder, the baffle plate is made of at least one circular tablet, between expanding reach and guide shell, the solid-liquid
Filter assemblies 11 are set in separator 10, and purified liquor outlet 16 is set through filter assemblies, 1 bottom of tedge is equipped with raw material
Entrance 4,2 top of expanding reach are equipped with gas vent 15.
Slurry bed circulatory flow reactor provided by the utility model has the beneficial effect that：
Setting guide shell and baffle plate, guide shell make stream in slurry bed circulatory flow reactor expanding reach provided by the utility model
Body is formed in expanding reach to stream, and strengthens the three phase separation of reaction liquid, catalyst and gas；Baffle plate make enter expanding reach and
The bubble carried secretly in fluid in guide shell gap further removes, and reduces the gas holdup for entering fluid in solid-liquid separator, drop
The blocking risk of low solid-liquid separator.Gas can be removed fully in slurries, and most of catalyst granules in expanding reach stays in expansion
In big section and tedge, the operating burden of subsequent technique is alleviated, the probability of catalyst abrasion is reduced.Through solid-liquid separator mistake
Solid content is relatively low in the fluid product of filter.Partial catalyst circulates between tedge and solid-liquid separator, carries
The high concentration for rising bottom of the tube catalyst, make slurries concentration and Temperature Distribution evenly, improve the utilization rate of catalyst
And reaction efficiency.Slurry bed system hydrogenation reactor provided by the utility model can avoid in reactor there are flow dead zone and hot spot,
Catalyst abrasion probability is reduced, the risk that solid-liquid separator blocks is reduced, effectively extends the operation cycle.It was prepared as anthraquinone
The hydrogenation reactor of hydrogen oxide can effectively reduce the probability of working solution over-hydrogenation, improve hydrogen effect.
Description of the drawings
Fig. 1 is the flow diagram of slurry bed circulatory flow reactor provided by the utility model.
Wherein：1- tedges；2- expanding reach；3- down-comers；The feed(raw material)inlets 4-；5- guide shells；6- baffle plates；7- fluids point
Cloth device；8- bubbles；9- solid catalyst particles；10- solid-liquid separators；11- filter assemblies；12- secondary filters；15- gases
Outlet；16- purified liquor outlets；Mouth is added in 17- catalyst；18- catalyst unloads outlet；19,20- pipelines.
Fig. 2 is the structural schematic diagram of baffle plate in paste state bed reactor expanding reach provided by the utility model.
Wherein：The upper layers 13- baffle；14- lower layers baffle.
Fig. 3 is the vertical view of baffle plate in paste state bed reactor expanding reach provided by the utility model.
Specific implementation mode
Specific embodiment of the present utility model described further below, wherein " top " for the container mentioned in specification
Refer to the position of the 0-50% of container from top to bottom, " lower part " of container refers to the position of the 50%-100% of container from top to bottom
It sets, " bottom " of container refers to the position of the 90%-100% of container from top to bottom, and " top " of container refers to from top to bottom holding
The position of the 0-10% of device.
The utility model provides a kind of slurry bed circulatory flow reactor, including tedge 1, the tedge upper tube being sequentially communicated
The widened expanding reach 2 of diameter, solid-liquid separator 10 and down-comer 3,10 bottom of solid-liquid separator is through down-comer 3 and tedge
1 bottom is connected to；Setting guide shell 5 and baffle plate 6 in the expanding reach 2, the guide shell reduce for diameter from top to bottom
Cylinder, the baffle plate is made of at least one circular tablet, between expanding reach and guide shell, the solid-liquid
Filter assemblies 11 are set in separator 10, and purified liquor outlet 16 is set through filter assemblies, 1 bottom of tedge is equipped with raw material
Entrance 4,2 top of expanding reach are equipped with gas vent 15.
In slurry bed system provided by the utility model in circulation reaction unit, the slurry bed system hydrogenation reactor height can be
3-100m, preferably 5-30m, most preferably 8-20m, diameter is in 0.5-10m, preferably 3-8m.The main body packet of slurry bed system hydrogenation reactor
Include tedge and the widened expanding reach of tedge top caliber.Preferably, the diameter of the expanding reach and tedge ratio is 1.2
~6：1, preferably 2~3：1；The height ratio of the expanding reach and tedge is：0.1~0.5：1, preferably 0.2~0.3：1.
In slurry bed system hydrogenation reactor provided by the utility model, guide shell is set, guide shell is in the expanding reach
The uniform cylinder of diameter, or a cylindrical section that from top to bottom diameter reduces, or by the different multistage cylinder group of diameter
At.There are gap, the guide shell lower edge and expanding reach bottom walls with wall at the top of expanding reach for the guide shell upper edge
There are gap, guide shell will be enlarged by the annular space two that the space in section is divided between interior guide shell, guide shell and expanding reach wall
Part, two parts space communicate respectively in guide shell upper and lower part.
Preferably, the diameter ratio of the guide shell maximum gauge and expanding reach is 0.5~0.9：1.
Preferably, the guide shell is one or more snippets cylinder composition that from top to bottom diameter reduces, when using multistage
When cylinder composite structure, connected by inverted cone-shaped structure between two cylindrical sections.It is further preferred that the guide shell is straight from top to bottom
Diameter ratio is 1.2~3：1 two cylindrical sections form, and are connected by inverted cone-shaped structure between two cylindrical sections.
In slurry bed system hydrogenation reactor provided by the utility model, baffling is set between guide shell in the expanding reach
Plate, the baffle plate are made of a series of circular tablets, and between expanding reach and guide shell, the baffle plate is general
It tilts down, is 0 °~60 ° with horizontal sextant angle α.Diametrically d1 is equal with expanding reach diameter on described one layer of baffle plate the top,
Under diametrically the ratio between d2 and guide shell maximum gauge be 1.1~4：1.If baffle plate is multilayer, second layer baffle plate upper edge
Diameter d3 is equal with adjacent guide cylinder diameter, under diametrically d4 and expanding reach diameter ratio are 0.1~0.3：1.Third layer baffling
Harden structure is identical as first layer, and the 4th layer of baffle arrangement is identical as the second layer, and so on.
Preferably, baffle plate is set as two layers, and the baffle plate can be non-porous tablet, can also exist as needed
Aperture or item seam is arranged in surface, and the diameter ratio of the minimum widith and catalyst granules of small aperture or item seam is 0.1~10:1.
Preferably, the diameter ratio of the projector distance between the baffle plate and expanding reach or guide shell and catalyst granules
It is 3~1000:1.
In slurry bed circulatory flow reactor provided by the utility model, the bottom of the tedge is equipped with feed(raw material)inlet, described
Feed(raw material)inlet can be one, and gas-phase feed mouth and liquid phase feeding mouth can also be respectively set.
Preferably, fluid distributor is set at the rising bottom of the tube feed(raw material)inlet.The fluid distributor can be with
It it is one, gas-phase feed and liquid phase feeding can share a fluid distributor after mixing.Gas phase stream can also be respectively set
Body distributor and liquid phase fluid distributor.When the feed(raw material)inlet is respectively gas-phase feed mouth and liquid phase feeding mouth, in gas
Gaseous fluid distributor and liquid fluid distributor is respectively set at phase feed inlet and liquid phase feeding mouth.Gas-phase feed and liquid phase into
Material respectively enters reactor by independent gaseous distributer and liquid phase distributor.
Preferably, the fluid distributor position is less than tedge lower part and solid-liquid separator lower part junction.More preferably
The opening direction of the fluid distributor is towards bottom of the tube is risen, to prevent solids particles precipitate by the souring of fluid
In reactor bottom.
In reactor provided by the utility model, the solid-liquid separator height can be within the scope of 0.5-10m, solid-liquid point
It is 1-20 from the diameter ratio of device and paste state bed reactor tedge:1, preferably 1-10:1, most preferably 1-5:1.The solid-liquid
Separator is one or more.Solid-liquid separator is used to detach by preliminary gas-liquid-solid three-phase to coming from paste state bed reactor top
Slurries be further separated by solid-liquid separation, the solid catalyst particle being separated by filtration in slurries.Setting inside the solid-liquid separator
Filter assemblies, filter assemblies can be one or more groups of.Filter assemblies can be ceramic membranes, metal film, forming metal sieve, burn
Tie one or more of combination such as orifice plate, non-woven bag.Filter assemblies by solid-liquid separator inner space be divided into slurries area and
Clear liquid area, slurries area are connected to by pipeline with paste state bed reactor bottom；In the clear liquid area of solid-liquid separator, purified liquor outlet is set,
Product clear liquid is discharged by purified liquor outlet.
Preferably, the solid-liquid separator lower part or solid-liquid separator are urged with being arranged in the connecting pipeline for rising bottom of the tube
Agent unloads outlet.Solid-liquid separator lower part, solid-liquid separator and in the connecting pipeline of the rising bottom of the tube or tedge bottom
Portion is arranged catalyst and mouth is added.The catalyst is added mouth setting and unloads outlet downstream in catalyst.Since reaction process can not
The meeting avoided causes abrasion and the inactivation of a part of catalyst, in order to ensure the activity of catalyst in reactor, needs periodically to examine
Abrasion and the inactivation of catalyst are surveyed, according to circumstances outlet is unloaded in catalyst and takes out part fine powder and decaying catalyst；And lead to
It crosses catalyst and mouth, regular replenishment fresh catalyst is added.Catalyst replacement process need not stop work, and extend the behaviour of whole device
Make the period.
In order to meet the requirement of ultralow catalyst granules content in product clear liquid, the especially slurry creates reaction unit
As anthraquinone hydrogenation reactor, to ensure the safety of anthraquinone hydrogenation liquid subsequent oxidation operation, it is preferable that the slurry bed system is anti-
It further includes secondary filter to answer device, for further detaching the micro-solid catalyst granules in product clear liquid.The solid-liquid
Separator purified liquor outlet is connected to secondary filter.Three-stage filtration equipment can also be again set after secondary filtration equipment, it is ensured that
Catalyst is blocked fully before oxidation operation.
Slurry bed circulatory flow reactor provided by the utility model is suitable for gas-liquid-solid phase reaction process, is particularly suitable for anthracene
The anthraquinone hydrogenation process of quinone legal system hydrogen peroxide process.Normally, the anthraquinone hydrogen peroxide process for preparing includes hydrogenation unit, oxygen
Change unit and extraction cells, hydrogenation unit using above-mentioned slurry bed circulatory flow reactor, anthraquinone working solution and hydrogen-containing gas into
Enter to rise bottom of the tube, mixes and move upwards with the slurries in tedge, in the presence of a hydrogenation catalyst, the anthraquinone in working solution
Derivative hydrogenation reaction obtains hydrogen anthraquinone, the expanding reach on reactor top, strengthens gas-liquid-solid three-phase separation, gas through guide shell
It is discharged by gas vent, after slurries further remove gas in the gap of expanding reach and guide shell under baffle plate effect, is entered
Hydrogenation catalyst granule therein is further separated by filtration in solid-liquid separator, clear liquid of the liquid phase isolated through solid-liquid separator
Outlet discharge is used as hydride；The oxidation solution containing hydrogen peroxide is obtained by the reaction in hydride in oxidation reactor with oxygen；Oxygen
Change liquid and obtains hydrogenperoxide steam generator and working solution through extraction and separation.
When slurry bed circulatory flow reactor provided by the utility model is used for anthraquinone hydrogenation process, the working solution is alkyl
Anthraquinone is dissolved in organic solvent and is formulated.Working solution disclosed in the prior art may be used, generally by anthraquinone derivative, weight virtue
The components such as hydrocarbon, trioctyl phosphate are mixed in a certain ratio composition.The catalyst used is load regulation on heat-resistant inorganic oxide
The supported catalyst of group VIII metal.The catalyst with hydrogenation/dehydrogenation performance in the prior art may be used, preferably load
The catalyst of group VIII noble metals, such as palladium, catalyst average grain diameter are 10~500 μm, preferably 30~100 μm.Described
Reaction temperature in tedge is 35~80 DEG C, preferably 55~75 DEG C；Reaction pressure be 0.1~0.5MPa, preferably 0.2~
0.3MPa.Empty tower gas velocity in the paste state bed reactor tedge is 0.01~0.2m/s, preferably 0.03~0.1m/s.
When slurry bed circulatory flow reactor provided by the utility model is used for anthraquinone hydrogenation process, it is preferably provided with secondary filtration
Device enters in secondary filter from the clear liquid for being separated by solid-liquid separation phase purified liquor outlet and filters, in the secondary filter, catalyst
Particle is stopped by filter element, forms filter cake, secondary filter is periodically discharged；The clear liquid being obtained by filtration through secondary filtration equipment is
Hydride.The fine separation of solid liquid phase may be implemented in secondary filter, it is ensured that the safety of subsequent oxidation operation.The hydrogenation
Liquid can also be filtered through three-level or level Four again before entering oxidation reactor.Ensure before entering oxidation operation, hydrogen is added in hydride
Catalyst quality solid content is less than 5ppm.The air speed of hydride is 0.01hr in secondary filter-1~10hr-1, preferably 0.1hr-1
~1hr-1, the control of secondary filter filtration pressure difference is in 0.1MPa~20MPa, preferably 0.5MPa~10MPa.Filtered hydride
Clear liquid enters the mixture that oxidizing tower oxidation generates hydrogen peroxide and anthraquinone derivative, and hydrogen peroxide production is obtained after water extracts
Product, anthraquinone derivative are recycled by being used as working solution return slurry bed system hydrogenation reactor after drying and purification.
In hydrogenation unit, without stopping work, it is fixed that outlet is unloaded by the catalyst on slurry bed system hydrogenation reaction device
Phase takes out catalyst fines and decaying catalyst, and the mouth periodically fresh makeup catalyst into reactor is added by catalyst,
Extend the operation cycle of reactor.The slurry bed system hydrogenation plant knot that hydrogen peroxide preparation method provided by the utility model uses
Structure is simple, and reaction mass improves the flow uniformity of each phase of gas-liquid-solid in reactor in paste state bed reactor interior orientation circulation,
Be concentration and Temperature Distribution evenly, avoid the probability of excessive hydrogenation, improve hydrogen effect, and then improve extraction after peroxidating
The concentration of hydrogen production.
Slurry bed circulatory flow reactor provided by the utility model is used for the anthraquinone hydrogenation unit for preparing hydrogen peroxide process,
Catalyst concn, working solution concentration and uniformity of temperature profile in paste state bed reactor inhibit working solution local excessive to add hydrogen, effectively
Improve hydrogen effect, and then improve again oxidized, hydrogen peroxide product after extracting operation concentration.It is provided by the utility model
Method extends the hydrogenation unit reactor operation cycle, reduces hydrogenation unit catalyst abrasion probability, mitigates subsequent process equipment
Pressure improves and is separated by solid-liquid separation flux and precision, the final hydrogenation efficiency for improving working solution.
The structure of slurry bed circulatory flow reactor provided by the utility model, but this practicality are further illustrated below in conjunction with attached drawing
It is novel therefore not any way limited.
Attached drawing 1 is the flow diagram of slurry bed system hydrogenation reactor provided by the utility model, if attached drawing 1 is as it can be seen that slurry
Bed hydroprocessing reactor includes tedge 1, expanding reach 2 and solid-liquid separator 10.2 top of expanding reach is connected to solid-liquid separator 10, excellent
Choosing is connected to 10 middle part of solid-liquid separator, and 10 bottom of solid-liquid separator is connected to 1 bottom of tedge through down-comer 3.1 bottom of tedge
Equipped with gas raw material entrance 6 and gas distributor 7；Liquid feed approach 4 and liquid fluid distributor 8.2 top of expanding reach is equipped with
Gas vent 15.
Wherein, guide shell 5 is set in expanding reach 2, and 5 upper edge of guide shell has certain gap, gap high with 2 top of expanding reach
Degree is within the scope of 10~500mm.5 lower edge of guide shell and 2 bottom of expanding reach there are gap, for fluid in guide shell 5 outer space
Between form circulation.5 position of guide shell can be adjusted according to actual conditions.
Baffle plate 6 is set between expanding reach 2 and guide shell 5, and the baffle plate 6 is usually by a series of and horizontal sextant angle α
It is formed for 0 °~60 ° of annular plates, at least one group.The baffle plate 6 can be non-porous tablet, can also be as needed
Surface be arranged aperture or item seam, institute's small aperture or item seam minimum widith and catalyst granules diameter ratio be 0.1~
10:1.The diameter ratio of projector distance and catalyst granules between baffle plate 6 and expanding reach 2 and guide shell is 3~1000:1.
Filter assemblies 11 are set in solid-liquid separator 10, and 10 inner space of solid-liquid separator is divided into slurry by filter assemblies 11
Liquid zone and filtrate area, 10 slurries area bottom of solid-liquid separator are connected to 1 bottom of tedge, the clear liquid of the solid-liquid separator 10
Purified liquor outlet 16 is arranged in area.It is preferred that purified liquor outlet 16 is located at the top of solid-liquid separator.The bottom of solid-liquid separator 10 is through declining
Pipe 3 is connected to the bottom of tedge 1, and the down-comer 3 is equipped with catalyst outlet 18, the catalyst for abrasion to be discharged
The catalyst of fine powder and inactivation；It is additionally provided with catalyst on the solid-liquid separator bottom down-comer 3, mouth 17 is added, in order to ensure
The activity of catalyst in reactor periodically carries out the supplement of fresh catalyst.Catalyst is added the setting of mouth 17 and is drawn off in catalyst
18 downstreams of mouth.The purified liquor outlet 16 of solid-liquid separator clear liquid area is connected to secondary filter 12.Filtering group is set in secondary filter
Part further filters the clear liquid from paste state bed reactor.
Attached drawing 2 is the structural schematic diagram of baffle plate in paste state bed reactor expanding reach provided by the utility model.It is rolled in figure
Flowing plate 6 is set as two layers, and topmost diametrically d1 is equal with 2 diameter of expanding reach on one layer of baffle plate 13 for baffle plate 6, under diametrically
The ratio between d2 and 5 maximum gauge of guide shell are 1.1~4：1.Diametrically d3 and 5 diameter phase of adjacent guide cylinder on second layer baffle plate 14
Deng, under diametrically d4 and 2 diameter ratio of expanding reach are 0.1~0.3：1.If baffle plate 6 is multilayer, third layer baffle arrangement
Identical as first layer, the 4th layer of baffle arrangement is identical as the second layer, and so on.
When slurry bed circulatory flow reactor provided by the utility model is used to prepare in anthraquinone hydrogenation reaction：Hydrogen and nitrogen
Gaseous mixture through feed(raw material)inlet 4, fluid distributor 7 enters tedge 1 bottom after being mixed with anthraquinone working solution, and reaction stream is first downward
The bottom of tedge 1 is washed away in flowing, is then changed flow direction and is flowed up along tedge 1, and from solid-liquid separator 10
Cycle hydride rich in Hydrogenation catalyst granule 9 mixes, and the slurries containing bubble 8 are flowed up along tedge 1, in working solution
Anthraquinone derivative reacted with hydrogen, be continuously generated hydrogen anthraquinone, consume a large amount of hydrogen, flow velocity continuously decreases, until flow into expand
In guide shell 5 in section 2.
Guide shell 5 is made of two different cylindrical sections of diameter, since the upper diameter of guide shell 5 is more than tedge 1, slurries
Flow velocity further decreases, and the flow direction of fluid is downward by changing into parabola straight up.Due to the difference of density, great Liang Qi
Bubble 8 continues to flow to reactor head, and reactor is finally discharged.The epimere and expanding reach 2 of fluid after degassing along guide shell 5
Between gap flow downward, after encountering baffle plate 6, remaining bubble 8 is further removed from fluid in fluid, to reactor
Top is flowed, and reactor is finally discharged.Fluid after degassing along guide shell 5 flows from hypomere to expanding reach 2, due to
The hypomere diameter of guide shell 5 is smaller than epimere, and fluid increases in this region flow velocity, and the larger solid catalyst particle 9 of density adds
Speed is to expanding reach flows, with anthraquinone hydrogenation liquid initial gross separation, 9 Returning reactor tedge 1 of a large amount of catalyst granules.Contain
Annular space of the anthraquinone hydrogenation liquid of a small amount of catalyst 9 between guide shell 5 and reactor expanding reach 2 is flowed to overflow.Due to this
When slurry phase flowing velocity it is relatively low, settlement action is notable, catalyst 9 and anthraquinone hydrogenation liquid is obtained by the reaction further detaches, and is catalyzed
Agent 9 returns to 2 bottom of expanding reach.A small amount of catalyst granules 9 for being entrained to expanding reach top, it is further when flowing through baffle plate 6
Deposition return expand pars infrasegmentalis, because of the flow channel very little between baffle plate and expanding reach and guide shell, form it is larger to
Upper flow resistance, catalyst granules 9 are difficult to pass through this flow channel.Further remove the anthraquinone hydrogenation liquid of solid catalyst 9
Into solid-liquid separator 10.
In solid-liquid separator 10, the clear liquid of the particle containing trace catalyst passes through purified liquor outlet 16 of the filter medium through top
Ejector, the slurries of enriched catalytic agent particle flow downward returns to 1 bottom of tedge by 10 bottom of solid-liquid separator, continues to join
With hydrogenation reaction.Slurries circulate to form orientation circulation between tedge 1 and solid-liquid separator 10.Under preferable case, come
Enter in secondary filter 12 from the anthraquinone hydrogenation liquid clear liquid containing trace catalyst 9 of purified liquor outlet 16 and further filters.
The clear liquid being obtained by filtration through secondary filtration equipment 14 is hydride；Hydride reacts in oxidation reactor with oxygen
Obtain the oxidation solution containing hydrogen peroxide；Oxidation solution extraction and separation in extraction tower obtain hydrogenperoxide steam generator and working solution.
Preferred embodiments of the present invention, still, the utility model and unlimited are described in detail above in association with attached drawing
Detail in the above embodiment can be to the skill of the utility model in the range of the technology design of the utility model
Art scheme carries out a variety of simple variants, these simple variants belong to the scope of protection of the utility model.
The application effect of slurry bed circulatory flow reactor provided by the utility model is further illustrated by the following examples, but
Therefore the utility model is not limited.
Hydrogen in embodiment imitates assay method：Take 5mL hydrides in separatory funnel, add 10mL heavy aromatics and
The H of 20mL2SO4Solution (H2SO4Volume ratio with water is 1:4)；Lead to O into above-mentioned mixed solution2, bubbling be oxidizing to glassy yellow or
Until crocus (about 10~15min)；Reaction solution is extracted with pure water 4~5 times, every time about 20mL water；It is used into extract liquor
The KMnO of concentration 0.1mol/L4Standard solution is titrated to blush, and 30s colour-fast is terminal.Then hydrogen imitates (gH2O2/ L)=standard
Solution concentration (0.1mol/L) × standard solution volume (mL) × 17.01/5.
Used catalyst is：The palladium-carbon catalyst Pd110 of Yu Rui Chemical Co., Ltd.s production, design parameter are as follows：
Bullion content 10% ± 0.2%, specific surface area >=950m2/ g, 85~105m of metal surface area2/ g, 100 μ of carrier average grain diameter
m。
Working solution is：2- ethyl hydrazine and solvent by volume 1:1 ratio mixes, and solvent is pungent by C10 aromatic hydrocarbons and tricresyl phosphate
Ester forms, the two by volume 3:1 ratio mixes.
Embodiment 1
Embodiment 1 illustrates that paste state bed reactor provided by the utility model is applied to the anthraquinone effect for preparing hydrogen peroxide
Fruit.
Using attached paste state bed reactor shown in FIG. 1, wherein it is 150 × 5000mm of Φ, expanding reach that reaction, which rises pipe size,
Size is 450 × 1500mm of Φ, and guide shell forms by two sections, and epimere size is 400 × 500mm of Φ, hypomere size be Φ 300 ×
500mm.Baffle plate is two layers, a diameter of 450mm of first layer upper edge, a diameter of 410mm of lower edge, and the oblique angle that dips down is 30 °；Second
The layer a diameter of 400mm of upper edge, a diameter of 440mm of lower edge, the oblique angle that dips down are 30 °.Solid-liquid separator size be Φ 150 ×
1500mm, inside set each filter differential pressure and reach 0.06MPa equipped with the ceramic membrane filter component that two groups of height are 500mm
Shi Jinhang automatic backflushings, backwash liquid are to react clear liquid after filtering.Filtered clear liquid enters secondary filter, in secondary filter
The filter medium of installation is non-woven bag.
Hydrogen-containing gas after premix, is entered by the fluid distributor of rising bottom of the tube in tedge with working solution, with
Working solution containing catalyst granules flows up after mixing, while the anthraquinone derivative in hydride is reacted with hydrogen, is being expanded
Gas-liquid-solid three-phase initial gross separation in section, hydrogen-containing gas are discharged by the gas vent of reactor head.Slurries enter solid-liquid separator
In, the clear liquid obtained after filter medium is discharged by purified liquor outlet, is re-introduced into secondary filter, does not pass through being rich in for filter medium
The hydride of solid particle returns to rising bottom of the tube through solid-liquid separator bottom and continues to participate in reaction.Hydrogenation in secondary filter
The air speed of liquid is 0.3hr-1, filtration pressure difference is 0.8MPa or so, after secondary filter filters, the solid content in clear liquid be less than
5ppm.The hydride that secondary filter obtains enters oxidation reactor, and hydrogen peroxide and working solution is obtained by the reaction with oxygen-containing gas,
And obtain hydrogenperoxide steam generator after extraction tower extracts.The operating condition of oxidation reactor is：Temperature is 50 DEG C, and pressure is
0.2MPa.The operating condition of extraction tower is：Temperature is 55 DEG C, and pure water flow is 12m3/h。
Embodiment 2
Embodiment 2 uses structure of reactor same as Example 1, and one layer of baffle plate, baffle plate is only arranged in expanding reach
Structure is identical as the first layer baffle arrangement in embodiment 1.Guide shell be single diameter cylinder, size be Φ 300 ×
1000mm.Reaction condition is same as Example 1.
Comparative example 1
Using the bubbling bed reactor of size identical as reactor in embodiment 1, guide shell is not set in reactor expanding reach
And baffle plate.Reactor does not have down-comer, and all raw materials and catalyst enter reactor from reactor bottom, after reaction, anti-
Device expanding reach is answered to deaerate, gas phase is discharged from expanding reach top vent, and pipeline outflow of other fluids in the middle part of expanding reach enters
Gas phase knockout drum carries out gas-liquid separation, and slurries enter filter filtering, and clear liquid enters oxidizing tower oxidation, extracted using extraction tower
Hydrogen peroxide is obtained, the working solution and turbid after reduction reenter reactor after being mixed with raw material under the conveying of pump.
Reaction condition is same as Example 1, and experimental result is as shown in table 1.
Table 1 synthesizes hydroperoxidation condition and result
| Project | Embodiment 1 | Embodiment 2 | Comparative example 1 |
| Reaction temperature, DEG C | 50 | 50 | 50 |
| Reaction pressure, Mpa | 0.2 | 0.2 | 0.2 |
| Working solution inlet amount, m3/h | 1 | 1 | 1 |
| H2Inlet amount, Nm3/h | 4 | 4 | 4 |
| Gas superficial gas velocity, m/s | 0.064 | 0.064 | 0.064 |
| Liquid speed in solid-liquid separator, m/s | 0.04 | 0.04 | 0.04 |
| Into the gas holdup of the fluid of solid-liquid separator | 0.006 | 0.026 | 0.15 |
| Into the solid holdup of the fluid of solid-liquid separator | 0.001 | 0.095 | 0.18 |
| Hydrogen is imitated, gH2O2/l | 15 | 14 | 12 |
Claims (11)
1. a kind of slurry bed circulatory flow reactor, which is characterized in that including tedge (1), the tedge top caliber being sequentially communicated
Widened expanding reach (2), solid-liquid separator (10) and down-comer (3), the solid-liquid separator (10) bottom is through down-comer (3)
It is connected to tedge (1) bottom；Setting guide shell (5) and baffle plate (6), the guide shell are in the expanding reach (2)
The cylinder that from top to bottom diameter reduces, the baffle plate are at least one circular tablet composition, be located at expanding reach wall with
Between guide shell (5), setting filter assemblies (11) in the solid-liquid separator (10), and purified liquor outlet is set through filter assemblies
(16), the tedge (1) bottom is equipped with feed(raw material)inlet (4), and gas vent (15) is equipped at the top of the expanding reach (2).
2. slurry bed circulatory flow reactor described in accordance with the claim 1, which is characterized in that the height of the expanding reach and tedge
Degree is than being 0.1~0.5：1, the diameter ratio of the expanding reach and tedge is 1.2~6：1.
3. slurry bed circulatory flow reactor described in accordance with the claim 1, which is characterized in that the guide shell maximum gauge and expansion
The diameter ratio of big section is 0.5~0.9：1.
4. according to any slurry bed circulatory flow reactor in claim 1-3, which is characterized in that the guide shell is
Two cylindrical sections that from top to bottom diameter reduces form, and are connected by inverted cone-shaped structure between two cylindrical sections.
5. according to any slurry bed circulatory flow reactor in claim 1-3, which is characterized in that the baffle plate inclines
The angle of tiltedly setting, baffle plate and horizontal direction is 0 °~60 °.
6. slurry bed circulatory flow reactor according to claim 5, which is characterized in that aperture is arranged in the baffling plate surface
Or item seam, the diameter ratio of the minimum widith and catalyst granules of small aperture or item seam is 0.1~10：1.
7. according to any slurry bed circulatory flow reactors of claim 1-3, which is characterized in that the solid-liquid separator
Diameter ratio with tedge is 1~20：1.
8. according to any slurry bed circulatory flow reactors of claim 1-3, which is characterized in that the rising bottom of the tube
Feed(raw material)inlet also set up fluid distributor, the position of the fluid distributor is less than the connection of the down-comer and tedge
Place.
9. slurry bed circulatory flow reactor according to claim 8, which is characterized in that the trepanning side of the fluid distributor
Rise bottom of the tube to direction.
10. according to any slurry bed circulatory flow reactors of claim 1-3, which is characterized in that further include secondary filtration
The purified liquor outlet of device, the solid-liquid separator is connected to secondary filter.
11. according to any slurry bed circulatory flow reactors of claim 1-3, which is characterized in that on the down-comer
Setting catalyst unloads outlet, and mouth is added in the decline bottom of the tube or rising bottom of the tube setting catalyst.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036149A (en) * | 2019-12-02 | 2020-04-21 | 河南金鹏化工有限公司 | Water-washing continuous production process and device for thiodicarb |
| CN114984621A (en) * | 2022-07-19 | 2022-09-02 | 福建永荣科技有限公司 | Equipment for settling and separating catalyst in ammoximation reaction |
| US11738318B2 (en) | 2019-09-19 | 2023-08-29 | Qingdao Institute Of Bioenergy And Bioprocess Technology, Chinese Academy Of Sciences | External loop slurry reactor |
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2017
- 2017-11-23 CN CN201721586345.5U patent/CN207981116U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11738318B2 (en) | 2019-09-19 | 2023-08-29 | Qingdao Institute Of Bioenergy And Bioprocess Technology, Chinese Academy Of Sciences | External loop slurry reactor |
| CN111036149A (en) * | 2019-12-02 | 2020-04-21 | 河南金鹏化工有限公司 | Water-washing continuous production process and device for thiodicarb |
| CN111036149B (en) * | 2019-12-02 | 2023-06-23 | 河南金鹏化工有限公司 | Thiodicarb water washing continuous production process and device |
| CN114984621A (en) * | 2022-07-19 | 2022-09-02 | 福建永荣科技有限公司 | Equipment for settling and separating catalyst in ammoximation reaction |
| CN114984621B (en) * | 2022-07-19 | 2023-06-16 | 福建永荣科技有限公司 | Catalyst sedimentation separation equipment for ammoximation reaction |
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