CN105056845B - Paste state bed reactor and its application in hydrogen peroxide is produced - Google Patents
Paste state bed reactor and its application in hydrogen peroxide is produced Download PDFInfo
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Abstract
The invention discloses a kind of paste state bed reactor, including tedge, expanding reach, cooler, catalyst settler, filter;Expanding reach is connected on tedge top, rises tube portion and extend into expanding reach, slurries return port is provided with the tedge in expanding reach, is communicated with reative cell;Rise bottom of the tube with cooler to be connected, cooler and tedge are integral types;Catalyst settler is fed by tangential way from middle part, catalyst settler top barrier of the equipment with certain altitude stands area to be formed, it is connected at the top of catalyst settler by balance pipe with gas-liquid separation chamber, bottom is connected with cooler, filter top is connected by balance pipe with gas-liquid separation chamber, filter bottom is connected with cooler, and filter is provided with backwash facility;Tedge bottom is provided with liquid phase feed entrance and gas phase feed(raw material)inlet;It is reative cell inside tedge, reative cell bottom is provided with liquid feed distributor and gas feed distributor.Hydrogenation efficiency of the present invention reaches 14 16g/l hydrides.
Description
Technical field
The invention belongs to technical field of chemical engineering, and in particular to a kind of paste state bed reactor and its production hydrogen peroxide
In application, paste state bed reactor more particularly to hydrogenation process in process for prepairng hydrogen peroxide by anthraquinone technique and its producing
Application in hydrogen oxide.
Background technology
Hydrogen peroxide is a kind of important Inorganic Chemicals, and 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 produces water and oxygen after decomposing
Gas, it is a kind of green chemical to environment non-secondary pollution.At present both at home and abroad generally using the life of anthraquinone progress hydrogen peroxide
Production.Process for prepairng hydrogen peroxide by anthraquinone is using anthraquinone derivative as working material, in the presence of catalyst, will be dissolved with hydrogen
Anthraquinone derivative hydrogenation in organic solvent, generates corresponding hydrogen anthraquinone.Then, hydrogen anthraquinone oxidation generation hydrogen peroxide and anthracene
Quinone derivative.Finally, the hydrogen peroxide extracted by the use of water in organic solvent 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
Determine the yield and concentration of hydrogen peroxide, the production tool to whole hydrogen peroxide is marginal.The country is in anthraquinone hydrogenation mistake at present
Down-type fixed-bed reactor, i.e. trickle bed reactor are most commonly used that in journey, but fixed bed reactors have catalyst profit
With efficiency is low, reaction selectivity is low, temperature distributing disproportionation is even, the local liquid holdup of catalyst is big and working solution degraded is serious in bed
The problem of.Hydrogenation process is carried out using fixed bed reactors, hydrogen effect is typically only 6~7g/L hydrides.And use gas and liquid flowing
The reactor moved upwards is the preferable selection for carrying out anthraquinone derivative hydrogenation process.It is anti-that such reactor includes tubular type suspension bed
Answer device, bubbling bed reactor and paste state bed reactor.During gas-liquid two-phase cocurrent flows up, working solution and anthraquinone mix
Solution is closed as continuous phase, and hydrogen(Or hydrogen and inert gas gaseous mixture)As dispersed phase, working solution can be both improved
The utilization rate for the treatment of capacity and catalyst, increase anthraquinone conversion ratio, it is big to overcome fixed bed catalyst bed part liquid holdup again, temperature
The problem of working solution is degraded caused by spending skewness.External newly-built large-scale hydrogen peroxide manufacture device typically uses up flow type
Fluid bed carries out hydrogenation, and hydrogen is imitated more than typically up to 12g/L hydrides.
US4428923 discloses a kind of tubular type suspension bed hydrogenation reactor system of process for prepairng hydrogen peroxide by anthraquinone, reaction
Device is connected, each section of pipe has identical nominal diameter into pass-over offset system between horizontal tube and vertical tube by elbow.Pipe is outer set
Pipe is for heating and cooling down, and hydrogenation process with regard to carrying out in the reactor.Before working solution enters hydrogenator with hydrogen, first through one
Venturi mixer is premixed, and catalyst is continuously flowed 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 special hydrogenation liquid filter must be used after separation
Hydride is separated again with catalyst, hydrogenation efficiency is 12g/L hydrides.
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 0.5 to 5 times of catalyst average grain diameter, and working solution and gas phase enter reactor together by reactor lower part, are urging
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 interval and continuous two ways operation, hydrogenation efficiency up to 15g/L hydrides more than.
CN1817838A discloses a kind of fluidized-bed reactor suitable for anthraquinone working solution hydrogenation.The reactor body point
For upper and lower two parts, bottom is hydrogenation body region, and there is expansion segment structure to be beneficial to gas-liquid separation, inside reactor on top
For void tower, hydrogenation efficiency is up to 9.9g/L hydrides.
CN104549065 provides a kind of slurry bed circulatory flow reactor and application and a kind of method for producing hydrogen peroxide,
The expanding reach and solid-liquid separator that described slurry bed circulatory flow reactor includes tedge, tedge top caliber expands, it is described
Expanding reach connection solid-liquid separator top, described solid-liquid separator bottom connects with rising bottom of the tube;Described expanding reach
The interior three phase separator for setting double-sleeve structure, described rising bottom of the tube are provided with feed(raw material)inlet, set at the top of described expanding reach
There is gas vent, filter assemblies are set in described solid-liquid separator, the filtered component in described solid-liquid separator top is set
Purified liquor outlet.Using the slurry bed circulatory flow reactor as gas-liquid-solid three-phase point in the method for hydrogenation reactor production hydrogen peroxide
From efficiency high, catalyst local excessive hydrogenation is avoided, reduces the possibility of excessive hydrogenation, hydrogen effect is high, can obtain higher
The hydrogen peroxide product of concentration.
The content of the invention
Present invention aims at a kind of paste state bed reactor is provided, the reactor is applied to gas-liquid-solid three-phase slurry reactor
With separating, especially suitable for hydriding process in process for prepairng hydrogen peroxide by anthraquinone technique.
To reach this purpose, technical scheme proposed by the invention is:
A kind of paste state bed reactor, it is characterised in that:Including tedge, expanding reach, cooler, catalyst settler, mistake
Filter;It is reative cell inside tedge;Expanding reach is connected on tedge top, rises tube portion and extend into expanding reach, expanding
Tedge in section is provided with slurries return port, is communicated with reative cell;Rise bottom of the tube with cooler to be connected, cooler is with rising
Pipe is integral type;Expanding reach top is gas-liquid separation chamber, and top is provided with reaction gas outlet, and expanding reach middle and lower part is catalyst
Pre- decanting zone, baffle plate, expanding reach baffle plate isolated area lower open are provided with catalyst sedimentation area, upper guard-plate is provided with perforate, expands
Big section baffle plate isolated area is connected with catalyst settler by tangential feed pipe;Catalyst settler is by tangential way from middle part
Charging, catalyst sedimentation area top is provided with passes through balance pipe and gas-liquid with the barrier for standing function, catalyst settler top
Separation chamber is connected, and bottom is connected by catalyst slurry expects pipe with cooler, and barrier top passes through reaction solution overflow pipe and filter
It is connected;Filter assemblies are installed, filter top is connected by balance pipe with gas-liquid separation chamber, and clear liquid leads to after filtering in filter
The discharge of filter purified liquor outlet is crossed, filter bottom is connected with cooler by catalyst slurry expects pipe, filters and set provided with backwash
Apply;Tedge bottom is provided with liquid phase feed entrance and gas phase feed(raw material)inlet;It is gentle that reative cell bottom is provided with liquid feed distributor
Body feed distributor.
The present invention is provided with the fluid redistributor with refrigerating function in reative cell.
Tedge ratio of height to diameter is 4/1~20/1 in the present invention.
The cylinder shell footpath of expanding reach is 1.2/1~2/1 with rising shell footpath ratio in the present invention.
The ratio of height to diameter 0.5/1~4/1 of expanding reach cylinder in the present invention.
It is 0.3~0.6 that tedge, which stretches into the height of expanding reach with the height ratio of expanding reach cylinder, in the present invention.
The filter assemblies of the present invention are two or more sets.
The cooler of the present invention is ripple tube cooler.
Application of the above-mentioned paste state bed reactor in hydrogen peroxide is produced, using above-mentioned paste state bed reactor, working solution
Liquid feed distributor is entered by liquid phase feed feed entrance, hydrogen-containing gas is entered by phase feed feed entrance into gas
Expect distributor, mix with the slurries in tedge and move upwards, under hydrogenation catalyst effect, the anthraquinone-derivative in working solution
Thing carries out hydrogenation reaction in tedge and obtains hydrogen anthraquinone;Material is after rising tube reaction after hydrogenation reaction, into expanding reach,
Gas-liquid separation chamber on expanding reach top carries out gas-liquid separation, and reacting gas discharges reactor from reaction gas outlet;Expanding
Middle and lower part carries out solid-liquid initial gross separation, and the high slurries of partially catalyzed agent concentration return to reative cell, removing unit from slurries return port
The reaction solution of divided catalyst particle enters catalyst settler from the top overflow of expanding reach baffle plate isolated area with tangential way;Urging
Agent settler, hydrogenation reaction solution carries out waterpower and gravitational settling, and is acted on through catalyst settler grid standing, and catalyst sinks
The slurries for dropping device bottom return to cooler by connecting tube, the gas-liquid separation chamber top of the gas phase Returning reactor on top, pass through
Reaction solution after sedimentation separation catalyst enters filter from the overflow of grid top;In the filter, the filtered component of reaction solution
It is separated by filtration, clear liquid discharges to obtain hydride from purified liquor outlet, and hydride obtains in oxidation reactor with oxygen reaction
Oxidation solution containing hydrogen peroxide;Oxidation solution obtains hydrogenperoxide steam generator and working solution through extract and separate, and gaseous substance returns to
Reactor gas-liquid separation chamber top, slurries are back to cooler from filter bottom by connecting tube;From catalyst sedimentation room and
After the slurries that filter comes are exchanged heat in cooler, it is again introduced into tedge and carries out hydrogenation reaction.
The outlet of unloading of hydrogenation catalyst is located at filter and cooler connecting tube top, adds mouth and is located at filter and cooling
Connecting tube bottom.
In method provided by the invention, reaction temperature in described paste state bed reactor is 35~80 DEG C, preferably 55~
75℃;Reaction pressure is 0.1~0.5MPa, preferably 0.2~0.3MPa.
The method provided by the invention for preparing hydrogen peroxide has the beneficial effect that:
Cooler of the present invention and tedge are integral type, have so both realized the cooling of circulation fluid, and have served circulation fluid again
Distributor acts on, and makes circulation liquid energy even into reative cell;The redistributor with refrigerating function is provided with reaction zone, is realized
Reaction solution gas-solid Three-phase Flow is uniform, improves the mass-transfer performance of fluid, while controls the temperature change of reaction solution.These technologies
The implementation of scheme, improves hydrogenation efficiency, and hydrogenation efficiency reaches 14-16 g/L hydrides.
The hydrogenation unit of the method provided by the invention for preparing hydrogen peroxide uses paste state bed reactor, the top of tedge
Expanding reach is extend into, the expanding reach on reactor top is gas-liquid separation chamber and catalyst sedimentation Disengagement zone, and catalyst is in catalyst
Sedimentation separation area is settled in advance, and catalyst sedimentation Disengagement zone bottom is connected provided with slurries return port with reative cell, containing high concentration
The slurries of catalyst return to reative cell from the slurries return port, and baffle plate, catalyst are provided with catalyst sedimentation Disengagement zone middle and upper part
Light liquid after pre- sedimentation enters baffle plate isolated area, and perforate arranged at baffle plate top, and gas is discharged into gas-liquid separation chamber from perforate, in isolated area
The slurries for removing partial catalyst enter catalyst settler by the tangential feed pipe of catalyst settler;Catalyst settler
Top is provided with the barrier for possessing and standing function, and the reaction solution on barrier top enters filter by tube overflow;These technical sides
The implementation of case, the expanding reach gas-liquid separation chamber of reactor realize gas-liquid separation, and catalyst sedimentation Disengagement zone realizes that solid-liquid divides in advance
From, while the high slurries of catalyst concn are returned into reative cell, reative cell middle and upper part catalyst concn had so both been improved, had been reacted
In the case that thing concentration gradient reduces, high hydrogenation efficiency is obtained, reduces the catalyst concn 20%-30% in reaction solution again,
Mitigate downstream catalyst segregational load;Catalyst settler is set before filter, and catalyst settler further separates
60%-70% catalyst, is so greatly reduced filter loading, it is possible to reduce the 70% of filter area, filter assemblies operation week
Phase has obtained significant extension, and compared with the direct filtering for being not added with catalyst settler, filter assemblies run time can extend 2-3
Times, the backwash frequency reduces 60%-80%.
Cooler and tedge are arranged to integral type by the present invention, and are ripple tube coolers.So it can both rise
Acted on to cooling heat transferring, while play the effect of slurry feed distributor, catalyst slurry is can be uniformly distributed in reative cell;
The application of glass stria tube formula cooler prevents deposition of the catalyst in cooler, can make cooler long-term operation.
By the implementation of the above technical scheme, hydrogenation efficiency reaches 15-16 g/L hydrides, the filtering of filter assemblies
Area reduces more than 60%, and filter assemblies run time can extend 2-3 times, and the backwash frequency reduces 60%-80%.
Accompanying drawing says figure
Fig. 1 paste state bed reactor schematic diagrames.
In figure:1- tedges;2- expanding reach;3- catalyst settlers;4- filters;5- coolers;6- liquid feedstocks point
Cloth device;7- gas feed distributors;8- reative cells;9- gas-liquid separation chamber;10- reaction gas outlets;11- bubbles;12- solids are urged
Catalyst particles;13- liquid phase feed entrances;14- phase feed entrances;15- cooling water inlets;16 coolant outlets;17- clear liquids go out
Mouthful;18- filter assemblies;19- slurries return ports;20- baffle plates;21- settler tangential feed pipes;22- settler barriers;23- is arranged
Gas port;The overflow pipe of 24- catalyst settlers and filter;25- fluid redistributors;26- cooling water inlets;27 cooling waters go out
Mouthful.
Embodiment
Below by specific example, the present invention will be described, but does not form the further limitation to invention.
Embodiment of the invention described further below:
Embodiment 1
Paste state bed reactor as shown in Figure 1, including tedge 1, expanding reach 2, cooler 5, catalyst settler 3, mistake
Filter 4;Expanding reach is connected on tedge top, rises tube portion and extend into expanding reach, be provided with the tedge in expanding reach
Slurries return port 19, communicated with reative cell 8;Rise bottom of the tube with cooler 5 to be connected, cooler and tedge are integral types;
Expanding reach top is gas-liquid separation chamber 9, and top is provided with reaction gas outlet 10, and expanding reach middle and lower part is the pre- decanting zone of catalyst,
Baffle plate 20 is provided with the pre- decanting zone of catalyst and forms baffle plate isolated area, lower open, upper guard-plate is provided with perforate 23, baffle plate isolation
Area is connected with catalyst settler 3 by tangential feed pipe 21;Catalyst settler is fed by tangential way from middle part, catalysis
Agent settler top is provided with barrier 22, is connected at the top of catalyst settler by balance pipe with gas-liquid separation chamber 9, bottom and cooling
Device 5 is connected, and barrier top is connected with filter 4;Filter assemblies 18 are installed in filter, filter top by balance pipe with
Gas-liquid separation chamber is connected, and clear liquid is discharged by filter purified liquor outlet after filtering, and filter bottom is connected with cooler 5, filtering
Device is provided with backwash facility;Tedge bottom is provided with liquid phase feed entrance 13 and gas phase feed(raw material)inlet 14;It is anti-inside tedge
Room 8 is answered, reative cell bottom is provided with liquid feed distributor 6 and gas feed distributor 7.
The outlet of unloading of hydrogenation catalyst is located at filter and cooler connecting tube top, adds mouth and is located at filter and cooling
Connecting tube bottom.
Three groups of fluid redistributors 25 are provided with reative cell.
Tedge ratio of height to diameter is 10/1.
The diameter of expanding reach cylinder is 1.5/1 with rising pipe diameter ratio.
The ratio of height to diameter 2/1 of expanding reach cylinder.
It is 0.6 that tedge, which stretches out the height of expanding reach with the height ratio of expanding reach cylinder,.
The filter assemblies used are two groups.
Working solution is entered into liquid feed distributor by liquid phase feed feed entrance, hydrogen-containing gas is entered by phase feed
Material entrance enters gas feed distributor, mixes with the slurries in tedge and moves upwards, under hydrogenation catalyst effect, work
Make the anthraquinone derivative in liquid and carry out hydrogenation reaction in tedge to obtain hydrogen anthraquinone;Material is anti-by tedge after hydrogenation reaction
After should rising, into expanding reach, the gas-liquid separation chamber on expanding reach top carries out gas-liquid separation, and reacting gas goes out from reacting gas
Mouth discharge reactor;Solid-liquid initial gross separation is carried out in expanding reach middle and lower part, expanding reach bottom is the high slurries of catalyst concn, from
Slurries return port returns to reative cell, and the baffle plate isolated area of expanding reach middle and upper part is containing the relatively low hydrogenation reaction of catalyst concn
Liquid, from expanding reach middle part inflow catalyst settler;In catalyst settler, hydrogenation reaction solution carries out sedimentation separation, and bottom is
Slurries containing catalyst, cooler, the gas-liquid separation chamber top of the gas phase Returning reactor at top, grid are entered by connecting tube
Top is the hydrogenation reaction solution for separating rear catalyst, enters filter through overflow pipe;In the filter, reaction solution passes through filtering group
Part, which enters, to be separated by filtration, and clear liquid discharges to obtain hydride from purified liquor outlet, and hydride obtains in oxidation reactor with oxygen reaction
To the oxidation solution containing hydrogen peroxide;Oxidation solution obtains hydrogenperoxide steam generator and working solution through extract and separate, and gaseous substance returns
To reactor gas-liquid separation chamber top, the slurries containing catalyst enter cooler from filter bottom by connecting tube;From catalysis
After the slurries that agent expansion chamber and filter come are exchanged heat in cooler, it is again introduced into tedge and carries out hydrogenation reaction.
Reaction temperature in paste state bed reactor is 35~80 DEG C;Reaction pressure be 0.1~0.5MPa, preferably 0.2~
0.3MPa。
Embodiment 2
Hydrogen imitates assay method:5mL hydrides are taken to add 10mL heavy aromatics and 20mL H in separatory funnel2SO4It is molten
Liquid(H2SO4Volume ratio with water is 1:4);Lead to O into above-mentioned mixed solution2, untill bubbling is oxidizing to glassy yellow or crocus
(About 10~15min);With pure water extractive reaction liquid 4~5 times, about 20mL water every time;Concentration 0.1mol/ is used into extract
L KMnO4Standard liquid is titrated to blush, and 30s colour-fast is terminal.Then hydrogen is imitated(gH2O2/L)=concentration of standard solution
(0.1mol/L) × standard liquid 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, the μ of carrier average grain diameter 100
m。
Working solution is:2- EAQs content is 120-180g/L, and solvent is made up of C10 aromatic hydrocarbons and trioctyl phosphate, two
Person by volume 3:1 ratio mixes.
Embodiment 3
Using the paste state bed reactor shown in accompanying drawing 1, wherein, it is 100 × 1000mm of Φ that reaction, which rises pipe size, expanding reach
Size is 150 × 300mm of Φ, and the height that tedge grows expanding reach is 150 mm;Filter has two groups of height for 400mm's
Sintering metal filter element filtering component, set when each filter assemblies pressure difference reaches 0.05MPa and carry out automatic backflushing, backwash liquid was
Clear liquid is reacted after filter.
Working solution inlet amount is 0.3 m3/ h, hydrogen inlet amount are 5.0 Nm3/h, 50-55 DEG C of reaction temperature, reaction pressure
0.25-0.5 MPa。
Filter assemblies service life is 60 hours, each backwashing time 40 seconds.
Hydrogenation efficiency reaches 12-14 g/L hydrides.
Embodiment 4
Using the paste state bed reactor shown in accompanying drawing 1, wherein, it is 100 × 1000mm of Φ that reaction, which rises pipe size, expanding reach
Size is 150 × 300mm of Φ, and the height that tedge grows expanding reach is 150 mm;Filter has two groups of height for 400mm's
Sintering metal filter element filtering component, set when each filter assemblies pressure difference reaches 0.05MPa and carry out automatic backflushing, backwash liquid was
Clear liquid is reacted after filter.A fluid redistributor of the group with refrigerating function is set in reative cell, redistributor is even to be arranged on reaction
In the middle part of room.
Working solution inlet amount is 0.3 m3/ h, hydrogen inlet amount are 5.0 Nm3/h, 50-55 DEG C of reaction temperature, reaction pressure
0.25-0.5 MPa。
Filter assemblies service life is 60 hours, each backwashing time 40 seconds.
Hydrogenation efficiency reaches 15-16 g/L hydrides.
Claims (9)
1. a kind of paste state bed reactor, including tedge(1), expanding reach(2), cooler(5), catalyst settler(3), filtering
Device(4);Tedge top is connected to expanding reach, rises tube portion and extend into expanding reach, and the tedge section bottom in expanding reach is set
There is slurries return port(19), with reative cell(8)Communicate;Rise bottom of the tube and cooler(5)It is connected, cooler(5)With tedge
(1)It is integral type;Expanding reach top is gas-liquid separation chamber(9), top is provided with reaction gas outlet(10), expanding reach middle and lower part
For the pre- decanting zone of catalyst, baffle plate is provided with the pre- decanting zone of catalyst(20), isolated area is formed between baffle plate and expanding reach cylinder, every
It is what is opened wide from area bottom, upper guard-plate is provided with perforate(23), expanding reach baffle plate isolated area and catalyst settler(3)By cutting
Line feed pipe(21)It is connected;Catalyst settler top is provided with barrier(22), catalyst settler top passes through balance pipe and gas
Liquid separation chamber(9)It is connected, bottom and cooler(5)It is connected, barrier top is overflow area, and overflow area passes through overflow line(24)With
Filter(4)It is connected;Filter assemblies are installed in filter(18), filter top passes through balance pipe and gas-liquid separation chamber's phase
Even;Filter bottom and cooler(5)It is connected, filter is provided with backwash facility;Tedge bottom is provided with liquid phase feed entrance
(13)With gas phase feed(raw material)inlet(14);It is reative cell inside tedge(8), reative cell bottom is provided with liquid feed distributor(6)
And gas feed distributor(7), reative cell is interior to be provided with the fluid redistributor with refrigerating function(25).
2. paste state bed reactor according to claim 1, it is characterised in that:Tedge ratio of height to diameter is 4/1~20/1.
3. paste state bed reactor according to claim 1, it is characterised in that:The cylinder shell footpath of expanding reach is with rising shell footpath
Than for 1.2/1~2/1.
4. paste state bed reactor according to claim 1, it is characterised in that:The cylinder ratio of height to diameter 0.5/1~4/ of expanding reach
1。
5. paste state bed reactor according to claim 1, it is characterised in that:Tedge stretches out height and the expansion of expanding reach
The height ratio of section cylinder is 0.3~0.6.
6. paste state bed reactor according to claim 1, it is characterised in that:Filter assemblies are two or more sets.
7. paste state bed reactor according to claim 1, it is characterised in that:Cooler is ripple tube cooler.
8. the paste state bed reactor described in claim any one of 1-7, it is characterised in that:In the application of production hydrogen peroxide,
Working solution enters liquid feed distributor by liquid phase feed feed entrance, and hydrogen-containing gas is entered by phase feed feed entrance
Gas feed distributor, mix with the slurries in tedge and move upwards, under hydrogenation catalyst effect, the anthracene in working solution
Quinone derivative carries out hydrogenation reaction in tedge and obtains hydrogen anthraquinone;Material enters after rising tube reaction after hydrogenation reaction
Expanding reach, the gas-liquid separation chamber on expanding reach top carry out gas-liquid separation, and reacting gas discharges reactor from reaction gas outlet;
Hydrogenation reaction solution containing catalyst granules expanding reach middle and lower part carry out solid-liquid initial gross separation, the high slurries of partially catalyzed agent concentration from
Slurries return port is returned directly to reative cell, and the hydrogenation reaction solution for removing partial catalyst particle flows into from tangent line in the middle part of expanding reach
Catalyst settler;In catalyst settler, hydrogenation reaction solution is settled, and the slurries of bottom are entered by connecting tube to be cooled down
Device, the gas-liquid separation chamber top of the gas phase Returning reactor at top, reaction solution are stood by waterpower sedimentation, gravitational settling and grid
After further removing catalyst granules, enter filter from the overflow of catalyst settler top;In the filter, reaction solution passes through
Filter assemblies, which enter, to be separated by filtration, and clear liquid discharges to obtain hydride from purified liquor outlet, hydride in oxidation reactor with oxygen
Reaction obtains the oxidation solution containing hydrogen peroxide;Oxidation solution obtains hydrogenperoxide steam generator and working solution, gas gas-phase objects through extract and separate
Matter returns to reactor gas-liquid separation chamber top, and slurries enter cooler from filter bottom by connecting tube;Sunk from catalyst
After the slurries that drop device and filter come are cooled in cooler, it is again introduced into tedge and carries out hydrogenation reaction.
9. paste state bed reactor according to claim 1, it is characterised in that:Set in filter and cooler connecting tube top
There is the outlet of unloading of hydrogenation catalyst, add mouth and be located at filter and cooling connecting tube bottom.
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CN108114666B (en) * | 2016-11-28 | 2021-02-05 | 中国石油化工股份有限公司 | Catalyst grading method for anthraquinone hydrogenation |
CN109678120B (en) * | 2017-10-19 | 2020-06-09 | 中国石油化工股份有限公司 | Hydrogenation reactor and hydrogenation method for producing hydrogen peroxide by anthraquinone process |
CN117548043B (en) * | 2024-01-09 | 2024-04-02 | 黎明化工研究设计院有限责任公司 | Fluidized bed hydrogenation device for producing hydrogen peroxide by anthraquinone process and application method thereof |
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