CN107098318A - Produce the fluid bed hydrogenation system and hydrogenation processes of hydrogen peroxide - Google Patents
Produce the fluid bed hydrogenation system and hydrogenation processes of hydrogen peroxide Download PDFInfo
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- CN107098318A CN107098318A CN201710452002.8A CN201710452002A CN107098318A CN 107098318 A CN107098318 A CN 107098318A CN 201710452002 A CN201710452002 A CN 201710452002A CN 107098318 A CN107098318 A CN 107098318A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/022—Preparation from organic compounds
- C01B15/023—Preparation from organic compounds by the alkyl-anthraquinone process
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The present invention relates to a kind of fluid bed hydrogenation system and hydrogenation processes for producing hydrogen peroxide, the hydride outlet of hydrogenation reaction cauldron bottom is connected by hydride loop pipe with each catalyst filter inlet；The outlet of each catalyst filter is separately installed with triple valve, and the outlet of triple valve is connected with hydride outlet pipe and hydriding reactor working solution recoil tube respectively；Agitating shaft and stirrer paddle are provided with along the axis of hydrogenation reaction cauldron；Each catalyst filter bottom is connected by catalyst filter flow reversal house steward with working solution supply pipe respectively, and working solution supply pipe inserts the inner chamber of hydrogenation reaction cauldron from middle part and curves downward and to axis；The top of hydrogenation reaction cauldron is provided with gaseous phase outlet and is plugged with catalyst adding tube and hydrogen feed pipe respectively, and hydrogen feed pipe extends downward into the bottom of hydrogenation reaction cauldron and turn extends upwardly to the lower central of hydrogenation reaction cauldron.The hydrogenation system manufacturing cost and unit consumption of product of the present invention is low, and production efficiency is high.
Description
Technical field
The present invention relates to a kind of fluid bed hydrogenation system for producing hydrogen peroxide, the invention further relates to a kind of fluid bed
The hydrogenation processes of hydrogen peroxide are produced, belong to hydrogen peroxide manufacturing equipment technical field.
Background technology
Hydrogen peroxide is a kind of important Inorganic Chemicals, be widely used in papermaking, weaving, medicine, chemical industry, electronics,
The fields such as environmental protection.Hydrogen peroxide produces water and oxygen after decomposing, and does not have secondary pollution to environment, meets the reason of green product production
Read.
In the prior art, hydrogen peroxide is generally produced by anthraquinone, anthraquinone is the palladium using 2- EAQs as carrier
For catalyst, hydrogen peroxide is directly combined to by hydrogen and oxygen, successively will be through processes such as over hydrogenation, oxidation, extraction and post processings.
Wherein hydrogenation is general is carried out in fixed bed, anthraquinone working solution in the presence of certain pressure, temperature and palladium catalyst, with
Hydrogenation occurs for hydrogen, produces hydrogen anthraquinone.
The anthraquinone low production efficiency of fixed bed, unit scale are less than normal, product production raw material and power unit consumption are high, set
Standby heavy, floor space is big, and manufacturing cost is high.
The content of the invention
The primary and foremost purpose of the present invention is that overcoming problems of the prior art, there is provided a kind of hydrogen peroxide of producing
Continuous production can be achieved in fluid bed hydrogenation system, facility compact, and the production consumption of unit product is low, and production efficiency is high, system
Cause low.
For solve above technical problem, a kind of fluid bed hydrogenation system for producing hydrogen peroxide of the invention, including
Hydride outlet is uniformly provided with vertical hydrogenation reaction cauldron, the lower circumference of the hydrogenation reaction cauldron, each hydride goes out
Mouth is connected with being looped around the hydride loop pipe of hydrogenation reaction cauldron periphery respectively, and the hydride loop pipe and catalyst filter are total
Inlet tube is connected, and filter inlet valve of the catalyst filter general import pipe respectively with each catalyst filter inlet is connected；Respectively
The outlet of catalyst filter is separately installed with triple valve, and the first outlet of the triple valve is connected with hydride outlet pipe, described
The second outlet of triple valve is connected with hydriding reactor working solution recoil tube；Agitating shaft is provided with along the center line of the hydrogenation reaction cauldron,
The agitating shaft is provided with stirrer paddle；The bottom of each catalyst filter is separately installed with catalyst filter flow reversal valve, each described
The outlet of catalyst filter flow reversal valve is connected with catalyst filter flow reversal house steward respectively, under the catalyst filter flow reversal house steward
End is connected with working solution supply pipe, and the middle part insertion hydrogenation of the working solution supply pipe from the hydrogenation reaction cauldron short transverse is anti-
Answer the inner chamber of kettle and be bent downwardly the axis for extending to the hydrogenation reaction cauldron；The top of the hydrogenation reaction cauldron is provided with hydriding reactor
Gaseous phase outlet and the catalyst adding tube extended straight down and hydrogen feed pipe are plugged with respectively, the upper end of the catalyst adding tube
It is connected by the outlet that catalyst adds valve with catalyst adds tank, the hydrogen feed pipe extends to hydrogen along the inwall of hydrogenation reaction cauldron
The bottom and turn of changing reactor extend upwardly to the lower central of the hydrogenation reaction cauldron.
Relative to prior art, the present invention achieves following beneficial effect：Catalyst addition valve is opened to throw appropriate catalyst
Enter hydrogenation reaction cauldron, while fresh working solution enters the center of hydrogenation reaction cauldron liquid Space and downward from working solution supply pipe
Spray, spread under the agitation of stirrer paddle to surrounding downwards；Fresh hydrogen sprays upwards from the lower port of hydrogen feed pipe,
It is separated into multiple minute bubbles under the agitation of stirrer paddle to spread upward all round, the opposite convection current of fresh working solution and hydrogen makes
Obtaining both can mix and react rapidly；Anthraquinone in working solution generates hydrogen anthracene in the presence of powdered palladium catalyst with hydrogen reaction
Quinone, nitrogen is discharged with remaining unreacted hydrogen from the hydriding reactor gaseous phase outlet at the top of hydrogenation reaction cauldron.Under hydrogenation reaction cauldron
Hydride outlet is uniformly arranged on portion's circumference and hydride loop pipe is imported, is conducive to hydride uniform flow in whole circumference
Go out.Most of catalyst filters are normal all in working condition, and now triple valve is in first outlet conducting, second outlet closing
State, after catalyst filter retains catalyst, the hydride of cleaning flows out into hydride from the first outlet of triple valve and gone out
Mouth pipe；When accumulating excessive catalyst on the filter core of catalyst filter, the filter capacity of catalyst filter is on the one hand caused to decline,
On the other hand the concentration of catalyst in hydrogenation reaction cauldron can be reduced, the progress of hydrogenation is influenceed, triple valve is now switched to the
One port closing, second outlet conducting state, while opening the hydrogen in catalyst filter flow reversal valve, hydriding reactor working solution recoil tube
Change liquid and enter the catalyst filter from recoil valve, the catalyst for being deposited in cartridge surface is rushed, through catalyst filter flow reversal valve and
Catalyst filter flow reversal house steward enters working solution supply pipe, follows fresh working solution to return in hydrogenation reaction cauldron, all catalyst
Recycled.Multiple catalyst filters are set, are easy to carry out the recoil of catalyst in turn, it is ensured that fluid bed can be continuously steady
Fixed production；For example fluid bed operationally, keeps a catalyst filter to be in recoil state, and remaining catalyst filter is in
Working condition, can both improve production efficiency, improve the yield of hydrogen anthraquinone, can ensure the filtering effect of each catalyst filter again
Rate, it is ensured that the concentration of catalyst in hydrogenation reaction cauldron, makes fluid bed all the time in stable working condition.Pass through changing for triple valve
To normal work and the switching of recoil are very convenient quick.The system hydrogenation of the present invention is rapid, touching in hydrogenation reaction cauldron
Matchmaker's concentration is stable, is capable of the hydride of steady and continuous output high-quality, and hydrogen unit consumption is low, and hydrogenation efficiency is high.
As the improvement of the present invention, the top of the agitating shaft is set with center sleeve, the upper end of the center sleeve with
The inwall closing connection of the hydrogenation reaction cauldron, the lower end of the center sleeve is inserted into the liquid Space of hydrogenation reaction cauldron.
Center sleeve and permeability cell are to the gas-phase space formation fluid-tight at the top of hydrogenation reaction cauldron, by condensate liquid passage and hydrogenation reaction cauldron top
The gas-phase space in portion is kept apart, and the condensate liquid for entering center sleeve is delivered into the central area of reactor liquid Space.
As a further improvement on the present invention, the hydriding reactor gaseous phase outlet is connected with the air inlet of condenser, described cold
The exhaust outlet of condenser is connected by Exhaust Emission Control valve with tail gas blow-down pipe, and the leakage fluid dram of the condenser is returned by condensate liquid
Flow tube is connected with the top of the center sleeve.The non-incoagulable gas such as the solvent vapo(u)r discharged from hydriding reactor gaseous phase outlet are through cold
Turn into liquid again after condenser condensation, center sleeve is flowed back to from condensate liquid return duct, continue to participate in the reaction of hydrogenation reaction cauldron, have
Beneficial to reduction material loss；Exhaust Emission Control valve can control the discharge capacity of tail gas and adjust the pressure in hydrogenation reaction cauldron,
The fluid-tight effect of center sleeve can avoid gas at the top of hydrogenation reaction cauldron from entering condensate liquid return duct, and condensate liquid is from center
Pipe lower end outflow after directly arrival reactor liquid Space central area, under the agitation of stirrer paddle rapidly with it is fresh
Working solution mixing is spread downwards to surrounding jointly, with the upward uniform hybrid reaction of hydrogen.
As a further improvement on the present invention, along the inwall of the hydrogenation reaction cauldron liquid Space at least provided with vertical together
Baffle plate, the diameter extension of the cross section of the vertical baffle plate along hydrogenation reaction cauldron.The rotation of stirrer paddle, can drive working solution to revolve
Turn, circulation is formed in hydrogenation reaction cauldron inner chamber, stable circulation causes the material of the material and circulation internal layer of circulation outer layer to be difficult to
Mixing；Vertical baffle plate is radially inserted in circulation layer, is conducive to thoroughly destroying circulation layer so that working solution can be rapid with hydrogen
Hydrogenation occurs for uniform mixing.
As a further improvement on the present invention, the lower end of the catalyst filter flow reversal house steward is connected with backflow pipe bend,
The lower end of the backflow pipe bend is inserted in the working solution supply pipe, and the outlet of the backflow pipe bend is located at the working solution
The center of supply pipe and in the same direction with the flow direction of working solution.The catalyst that each catalyst filter recoil is reclaimed is returned from catalyst filter
The backflow pipe bend of stream house steward is directly injected into the center of working solution supply pipe, is made rapidly using the jet action of fresh working solution
The catalyst of backflow is spread apart rapidly in fresh working solution, plays mixed uniformly effect, it is to avoid it is anti-that catalyst conglomeration enters hydrogenation
Answer kettle.
As a further improvement on the present invention, the lower end of the catalyst filter flow reversal house steward is connected to the big of taper
Hold circumference on, taper be sleeved on the periphery of the working solution supply pipe and with working solution supply pipe coaxial line, taper
Big end seal close, the small end of taper towards hydrogenation reaction cauldron and it is relative with working solution supply pipe connect, the working solution supply
The part that pipe is located in taper is provided with the aditus laryngis of reduced diameter, and the aditus laryngis stretches to the small end of taper.Catalyst
The catalyst that filter recoil is reclaimed enters in taper from catalyst filter flow reversal house steward, and fresh working solution is supplied in working solution
Pipe high speed flow forward, flow velocity is accelerated at aditus laryngis, pressure reduction, and suction work is played to entering the catalyst in taper
With catalyst is able to be uniformly dispersed rapidly in fresh working solution, it is to avoid catalyst conglomeration enters hydrogenation reaction cauldron.
As a further improvement on the present invention, the bottom of the hydrogenation reaction cauldron is provided with the ring with hydrogenation reaction cauldron coaxial line
Shape set, the inwall of the circumference of the annular sleeve and the hydrogenation reaction cauldron is spaced a distance, and each hydride outlet is located at
On the hydrogenation reaction cauldron circumference contour with annular sleeve axial direction middle part；The bottom of the agitating shaft is provided with lower stirring paddle
Leaf, the lower stirring paddle leaf is located in the annular sleeve, and the middle part of the agitating shaft is provided with upper stirrer paddle；The working solution is supplied
Outlet to pipe is positioned at the top of the upper stirrer paddle；The outlet of the hydrogen feed pipe is located in the annular sleeve lower port
The lower section of the heart.Annular sleeve is blocked to the formation of each hydride outlet, fresh hydrogen after the discharge of the port of hydrogen feed pipe, first to
The center of upper entrance annular sleeve, the lower stirring paddle leaf rotated smashes and is separated into multiple bubbles into the circulation in annular sleeve
In, annular sleeve prevents hydrogen gas bubbles from choking from hydride outlet；Fresh working solution flows out against upper stirrer paddle from top to bottom,
It is scattered to surrounding on one side downwards on one side under the rotational agitation of upper stirrer paddle, be conducive to the hydrogen gas bubbles with rising uniformly to mix
Close, hydrogenation occurs rapidly, annular sleeve can equally avoid the fresh working solution having just enter into from directly choking from hydride outlet；
The working solution sprayed downwards is flowed up again after being mixed with the hydrogen gas bubbles of lower section so that most fresh working solution first with hydrogen
Concentration highest region is contacted, and is conducive to improving hydrogenation efficiency.
It is another object of the present invention to overcome problems of the prior art to be produced there is provided a kind of fluid bed
The hydrogenation processes of hydrogen oxide, can be achieved continuous production, and the production consumption of unit product is low, and production efficiency is high, manufacturing cost
It is low.
To solve above technical problem, the present invention produces the hydrogenation of hydrogen peroxide using fluid bed hydrogenation system
Method, in turn includes the following steps, and (1) configures hydrogenation solvent；(2) 2- EAQs and 2- amyl groups are added into above solvent
The working solution of hydrogenation is constituted after anthraquinone, wherein adding 2- EAQs in every liter of solvent（80~110）G/L, every liter of solvent
In add 2- amyl anthraquinones（60~140）g/L；(3) powdered palladium catalyst is prepared, and the particle diameter volume distributed median of the palladium catalyst is：Particle diameter
Percent by volume more than 120 microns is no more than 4%；The percent by volume that particle diameter is less than 80 microns is no more than 4%, and remaining particle diameter is equal
For 80~120 microns；(4) open catalyst addition valve and appropriate catalyst is put into hydrogenation reaction cauldron, while fresh working solution is from work
Make liquid supply pipe into the center of hydrogenation reaction cauldron liquid Space and spray downwards, downwards to surrounding under the agitation of stirrer paddle
Diffusion；Fresh hydrogen is sprayed upwards from the lower port of hydrogen feed pipe, and multiple minute bubbles are separated under the agitation of stirrer paddle
Spread upward all round, be sufficiently mixed and stir with fresh working solution；(5) work of the anthraquinone in working solution in powdered palladium catalyst
Hydrogen anthraquinone is generated with lower reacted with hydrogen；(6) the gaseous substance on hydrogenation reaction cauldron top is escaped and enter from hydriding reactor gaseous phase outlet
Condenser is condensed, and incoagulable gas includes unreacted hydrogen and discharged from tail gas blow-down pipe, and condensate liquid is returned in center sleeve；⑺
Hydride enters hydride loop pipe together with powder catalyst from each hydride outlet in hydrogenation reaction cauldron lower circumference, then through touching
Matchmaker's filter general import pipe is filtered into each catalyst filter；Triple valve is switched into first outlet conducting, second outlet to close
State, after catalyst filter retains catalyst, the hydride of cleaning flows out into hydride from the first outlet of triple valve and gone out
Mouth pipe；(8) each catalyst filter is recoiled in turn, triple valve is switched into first outlet closing, second outlet during recoil leads
Logical state, while the hydride opened in catalyst filter flow reversal valve, hydriding reactor working solution recoil tube is touched from recoil valve into this
Matchmaker's filter, the catalyst for being deposited in cartridge surface is rushed, entered through catalyst filter flow reversal valve and catalyst filter flow reversal house steward
Enter working solution supply pipe, follow fresh working solution to return in hydrogenation reaction cauldron.
Relative to prior art, the present invention achieves following beneficial effect：Fresh working solution is evenly distributed on hydrogenation
On the lower circumference of reactor, and spray downwards；Hydrogen is divided into numerous tiny bubble hydrogens by densely covered hydrogen dispensing orifice, increases
The big contact area of hydrogen and working solution, and most fresh working solution contacts with density of hydrogen highest region first, favorably
In hydrogenation occurs rapidly, hydrogenation efficiency is improved.After catalyst flows out with hydride, retained by catalyst filter, by turn
Recoil returns to hydrogenation reaction cauldron, by the lasting Rational flow of catalyst, both ensure that the filter efficiency of catalyst filter, and had kept again
Catalyst concentration in hydrogenation reaction cauldron.The catalyst and hydrogen that the present invention is used are able to whole recyclings, advantageously reduce list
The production consumption of position product, improves hydrogenation efficiency, reduces production cost.
As the present invention preferred scheme, step (1) in hydrogenation solvent by following percent by volume configuration, two is different
Butyl carbinol：（45~50）V%, C10 aromatic hydrocarbons：（50~55）V%, both volume summations are 100%.C10 aromatic hydrocarbons is used to dissolve 2-
EAQ and 2- amyl anthraquinones, diisobutyl carbinol (DIBC) increase the solubility of 2- EAQs and 2- amyl anthraquinones.
As the present invention preferred scheme, step (1) in hydrogenation solvent by following percent by volume configuration, four fourths
Base urea：（12~30）V%, trioctyl phosphate：（8~12）V%, C10 aromatic hydrocarbons：（60~76）V%, the volume summation of three is 100%.
C10 aromatic hydrocarbons mainly dissolves the tetrahydrochysene 2- EAQs that 2- EAQs, 2- amyl anthraquinones and reaction are produced, and can not dissolve hydrogenation
The 2- ethyl hydrogen anthraquinones and tetrahydrochysene 2- ethyl hydrogen anthraquinones generated afterwards；Therefore also need to that 2- ethyl hydrogen anthraquinones and tetrahydrochysene 2- second can be dissolved
The trioctyl phosphate and tetrabutyl urea of base anthraquinone are used as polar solvent.The present invention has higher C10 arene contents, can avoid
Working solution proportion increases, and causes extraction tower operating difficulties；Trioctyl phosphate has high boiling point, non-stimulated taste, dissolved hydrogen anthraquinone
The strong advantage of ability, but if too high levels, work fluid viscosity can be caused to increase, cause mass transfer difficult；Tetrabutyl urea is
Bright or slightly yellowish liquid, viscosity is slightly bigger than water, has the advantages that and water density difference is big, surface tension is big, relative to
Trioctyl phosphate is big to the solubility of 2- ethyl hydrogen anthraquinones and tetrahydrochysene 2- EAQs, distribution coefficient of the hydrogen peroxide in two-phase
Greatly.Solvent composition combination and ratio using the present invention so that working solution have volatilization loss it is small, using safety, favourable operation
Environment, reduction raffinate hydrogen peroxide content, the advantage for improving extract concentration, due to being reduced with the stock solubility of water so that
The TOC of dioxygen aquatic products（Total organic carbon）Content is greatly reduced, and is conducive to the lifting of product quality.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description, accompanying drawing only provide with reference to
Illustrate to use, be not used to the limitation present invention.
Fig. 1 produces the structural representation of the fluid bed hydrogenation system of hydrogen peroxide for the present invention.
Fig. 2 is the top view of hydride outlet and hydride loop pipe in Fig. 1.
Fig. 3 is catalyst filter flow reversal house steward and the schematic diagram of second of connection scheme of working solution supply pipe.
In figure：1. hydrogenation reaction cauldron；1a. hydriding reactor gaseous phase outlets；1b. hydride outlets；1c. center sleeves；1d. is vertical
Baffle plate；1e. annular sleeves；1f. agitating shafts；1g. stirrer paddles；1h. hydride loop pipes；2. catalyst adds tank；3. condenser；4.
Catalyst filter；G1. working solution supply pipe；G1a. taper；G2. hydrogen feed pipe；G3. catalyst adding tube；G4. tail gas is put
Blank pipe；G5. condensate liquid return duct；G6. catalyst filter general import pipe；G7. hydride outlet pipe；G8. hydriding reactor working solution is anti-
Washing pipe；G9. catalyst filter flow reversal house steward；V1. catalyst adds valve；V2. triple valve；V3. filter inlet valve；V4. catalyst mistake
Filter return valve；V5. Exhaust Emission Control valve.
Embodiment
As shown in Figure 1 and Figure 2, the fluid bed hydrogenation system of present invention production hydrogen peroxide is anti-including vertical hydrogenation
Answer and hydride outlet 1b is uniformly provided with kettle 1, the lower circumference of hydrogenation reaction cauldron 1, each hydride outlet 1b is respectively with being looped around
The hydride loop pipe 1h of hydrogenation reaction cauldron periphery is connected, and hydride loop pipe 1h is connected with catalyst filter general import pipe G6,
Filter inlet valve V3s of the catalyst filter general import pipe G6 respectively with each entrance of catalyst filter 4 is connected；Each catalyst filter 4
Outlet be separately installed with triple valve V2, triple valve V2 first outlet is connected with hydride outlet pipe G7, the of triple valve V2
Two outlets are connected with hydriding reactor working solution recoil tube G8；It is provided with along the center line of hydrogenation reaction cauldron 1 on agitating shaft 1f, agitating shaft 1f
Provided with stirrer paddle 1g；The bottom of each catalyst filter 4 is separately installed with catalyst filter flow reversal valve V4, and each catalyst filter is returned
Stream valve V4 outlet is connected with catalyst filter flow reversal house steward G9 respectively, catalyst filter flow reversal house steward G9 lower end and working solution
Supply pipe G1 is connected, and working solution supply pipe G1 inserts the inner chamber of hydrogenation reaction cauldron 1 simultaneously from the middle part of hydrogenation reaction cauldron short transverse
It is bent downwardly the axis for extending to hydrogenation reaction cauldron 1；The top of hydrogenation reaction cauldron 1 is provided with hydriding reactor gaseous phase outlet 1a and inserts respectively
The catalyst adding tube G3 and hydrogen feed pipe G2 extended straight down is connected to, valve is added in catalyst adding tube G3 upper end by catalyst
The outlet that V1 adds tank 2 with catalyst is connected, and inwalls of the hydrogen feed pipe G2 along hydrogenation reaction cauldron 1 extends to hydrogenation reaction cauldron 1
Simultaneously turn round and extend upwardly to the lower central of hydrogenation reaction cauldron 1 in bottom.
Open catalyst addition valve V1 and appropriate catalyst is put into hydrogenation reaction cauldron 1, while fresh working solution is from working solution
Supply pipe G1 enters the center of hydrogenation reaction cauldron liquid Space and sprayed downwards, downwards to surrounding under stirrer paddle 1g agitation
Diffusion；Fresh hydrogen sprays upwards from hydrogen feed pipe G2 lower port, is separated under stirrer paddle 1g agitation multiple small
Bubble spreads upward all round, and the opposite convection current of fresh working solution with hydrogen enables both to mix and react rapidly；Work
Make the anthraquinone in liquid in the presence of powdered palladium catalyst with hydrogen reaction generation hydrogen anthraquinone, nitrogen and remaining unreacted hydrogen from
Hydriding reactor gaseous phase outlet 1a discharges at the top of hydrogenation reaction cauldron.Hydride is uniformly arranged in the lower circumference of hydrogenation reaction cauldron 1 to go out
Mouth 1b simultaneously imports hydride loop pipe 1h, is conducive to hydride uniformly to be flowed out in whole circumference.
Most of catalyst filters 4 are normal all in working condition, and now triple valve V2 is in first outlet conducting, second
Port closing state, after catalyst filter 4 retains catalyst, the hydride of cleaning is gone forward side by side from triple valve V2 first outlet outflow
Enter hydride outlet pipe G7；When accumulating excessive catalyst on the filter core of catalyst filter 4, on the one hand cause catalyst filter 4
Filter capacity decline, on the other hand can reduce the concentration of catalyst in hydrogenation reaction cauldron 1, influence the progress of hydrogenation, now
Triple valve V2 is switched into first outlet closing, second outlet conducting state, while catalyst filter flow reversal valve V4 is opened, hydrogenation
Hydride in kettle working solution recoil tube G8 enters the catalyst filter from recoil valve, and the catalyst for being deposited in cartridge surface is rushed
Fall, enter working solution supply pipe G1 through catalyst filter flow reversal valve V4 and catalyst filter flow reversal house steward G9, follow fresh work
Liquid is returned in hydrogenation reaction cauldron 1, and all catalyst are recycled.
Multiple catalyst filters are set, are easy to carry out the recoil of catalyst in turn, it is ensured that fluid bed being capable of continuous and stable production；
For example fluid bed operationally, keeps a catalyst filter to be in recoil state, and remaining catalyst filter is in work shape
State, can both improve production efficiency, improve the yield of hydrogen anthraquinone, can ensure the filter efficiency of each catalyst filter again, it is ensured that
The concentration of catalyst in hydrogenation reaction cauldron 1, makes fluid bed all the time in stable working condition.
Agitating shaft 1f top is set with center sleeve 1c, and center sleeve 1c upper end is sealed with the inwall of hydrogenation reaction cauldron 1
Connection is closed, center sleeve 1c lower end is inserted into the liquid Space of hydrogenation reaction cauldron 1.
Hydriding reactor gaseous phase outlet 1a is connected with the air inlet of condenser 3, and the exhaust outlet of condenser 3 passes through Exhaust Emission Control
Valve V5 is connected with tail gas blow-down pipe G4, the top phase that the leakage fluid dram of condenser 3 passes through condensate liquid return duct G5 and center sleeve 1c
Even.Turn into liquid again after being condensed from the condensed device 3 of the non-incoagulable gas such as hydriding reactor gaseous phase outlet 1a solvent vapo(u)rs discharged,
Center sleeve 1c is flowed back to from condensate liquid return duct G5, continues to participate in the reaction of hydrogenation reaction cauldron 1, is conducive to reducing material loss；
Exhaust Emission Control valve V5 can control the discharge capacity of tail gas and adjust the pressure in hydrogenation reaction cauldron 1；Center sleeve 1c and thoroughly
Tracheae is to the gas-phase space formation fluid-tight at the top of hydrogenation reaction cauldron, by the gas-phase space at the top of condensate liquid passage and hydrogenation reaction cauldron
Keep apart, the gas at the top of hydrogenation reaction cauldron can be avoided to enter condensate liquid return duct G5, condensate liquid is from center sleeve 1c's
Lower end outflow after directly arrival reactor liquid Space central area, under stirrer paddle 1g agitation rapidly with fresh work
Make liquid mixing to spread to surrounding downwards jointly, with the upward uniform hybrid reaction of hydrogen.
Along the inwall of hydrogenation reaction cauldron liquid Space at least provided with vertical baffle plate 1d, vertical baffle plate 1d cross section edge together
The diameter extension of hydrogenation reaction cauldron 1.Stirrer paddle 1g rotation, can drive working solution to rotate, and be formed in hydrogenation reaction cauldron inner chamber
Circulation, stable circulation causes the material of circulation outer layer to be difficult to mix with the material of circulation internal layer；Vertical baffle plate 1d is radially inserted
Enter in circulation layer, be conducive to thoroughly destroying circulation layer so that working solution can uniformly mix rapidly generation hydrogenation with hydrogen.
Catalyst filter flow reversal house steward G9 lower end is connected with backflow pipe bend, the lower end insertion working solution of backflow pipe bend
In supply pipe G1, the outlet of backflow pipe bend is positioned at working solution supply pipe G1 center and in the same direction with the flow direction of working solution.
Catalyst from catalyst filter flow reversal house steward G9 that each catalyst filter recoil is reclaimed backflow pipe bend are directly injected into working solution
Supply pipe G1 center, the catalyst for making backflow rapidly using the jet action of fresh working solution spreads rapidly in fresh working solution
Open, play mixed uniformly effect, it is to avoid catalyst conglomeration enters hydrogenation reaction cauldron 1.
As shown in figure 3, another scheme is：Catalyst filter flow reversal house steward G9 lower end is connected to taper G1a's
On big end circumference, taper G1a be sleeved on working solution supply pipe G1 periphery and with working solution supply pipe G1 coaxial lines, taper
Sleeve pipe G1a big end seal is closed, taper G1a small end towards hydrogenation reaction cauldron 1 and it is relative with working solution supply pipe G1 connect, work
Make the aditus laryngis that parts of the liquid supply pipe G1 in taper G1a is provided with reduced diameter, aditus laryngis stretches to taper G1a
Small end.The catalyst that the recoil of catalyst filter is reclaimed enters in taper G1a from catalyst filter flow reversal house steward G9, fresh work
Make liquid in working solution supply pipe G1 high speed flow forwards, flow velocity is accelerated at aditus laryngis, pressure reduction, to entering taper
Catalyst in G1a plays swabbing action, and catalyst is able to be uniformly dispersed rapidly in fresh working solution, it is to avoid catalyst conglomeration enters hydrogen
Change reactor 1.
The bottom of hydrogenation reaction cauldron 1 is provided with the annular sleeve 1e with hydrogenation reaction cauldron coaxial line, annular sleeve 1e circumference and hydrogen
The inwall for changing reactor 1 is spaced a distance, and each hydride outlet 1b is located at hydrogenation reaction cauldron 1, and axially middle part is contour with annular sleeve
Circumference on；Agitating shaft 1f bottom is provided with lower stirring paddle leaf, and lower stirring paddle leaf is located in annular sleeve 1e, agitating shaft 1f middle part
Provided with upper stirrer paddle；Working solution supply pipe G1 outlet is positioned at the top of upper stirrer paddle；Hydrogen feed pipe G2 outlet position
Lower section in annular sleeve lower port center.
Annular sleeve 1e is blocked to each hydride outlet 1b formation, after fresh hydrogen is discharged from hydrogen feed pipe G2 port,
Annular sleeve 1e center is upwardly into first, and the lower stirring paddle leaf rotated smashes and is separated into multiple bubbles into annular sleeve 1e
In interior circulation, annular sleeve 1e prevents hydrogen gas bubbles from choking from hydride outlet 1b；Fresh working solution is from top to bottom against upper
Stirrer paddle flows out, under the rotational agitation of upper stirrer paddle, on one side downwards while, the hydrogen that is conducive to and rises scattered to surrounding
Gas bubble is uniformly mixed, and occurs hydrogenation rapidly, annular sleeve 1e can equally avoid the fresh working solution that has just enter into directly from
Hydride outlet 1b chokes；The working solution sprayed downwards is flowed up again after being mixed with the hydrogen gas bubbles of lower section so that most fresh
Working solution contacted first with density of hydrogen highest region, be conducive to improve hydrogenation efficiency.
The present invention produces the hydrogenation processes of hydrogen peroxide using fluid bed hydrogenation system, successively including following step
Suddenly, hydrogenation solvent is (1) configured；(2) hydrogenation is constituted after 2- EAQs and 2- amyl anthraquinones are added into above solvent
Working solution, wherein adding 2- EAQs in every liter of solvent（80~110）2- amyl anthraquinones are added in g/L, every liter of solvent（60
~140）g/L；(3) powdered palladium catalyst is prepared, and the particle diameter volume distributed median of the palladium catalyst is：Particle diameter is more than 120 microns of volume hundred
Divide than being no more than 4%；The percent by volume that particle diameter is less than 80 microns is no more than 4%, and remaining particle diameter is 80~120 microns；(4) beat
Open catalyst addition valve V1 and appropriate catalyst is put into hydrogenation reaction cauldron 1, while fresh working solution enters from working solution supply pipe G1
Enter the center of hydrogenation reaction cauldron liquid Space and spray downwards, spread under the agitation of stirrer paddle to surrounding downwards；Fresh hydrogen
Gas is sprayed upwards from hydrogen feed pipe G2 lower port, and multiple minute bubbles are separated under the agitation of stirrer paddle upward all round
Diffusion, is sufficiently mixed and stirs with fresh working solution；Anthraquinone in working solution in the presence of powdered palladium catalyst with hydrogen
Reaction generation hydrogen anthraquinone；(6) the gaseous substance on the top of hydrogenation reaction cauldron 1 escapes and enter condenser 3 from hydriding reactor gaseous phase outlet 1a
Condensation, incoagulable gas includes unreacted hydrogen and discharged from tail gas blow-down pipe G4, and condensate liquid is returned in center sleeve 1c；(7) hydrogen
Change liquid and enter hydride loop pipe 1h from each hydride outlet 1b in hydrogenation reaction cauldron lower circumference together with powder catalyst, then pass through
Catalyst filter general import pipe G6 is filtered into each catalyst filter；Triple valve V2 is switched into first outlet conducting, second gone out
Mouth closed mode, after catalyst filter retains catalyst, hydride from the triple valve V2 of cleaning first outlet are flowed out into
Hydride outlet pipe G7；(8) each catalyst filter is recoiled in turn, triple valve V2 is switched into first outlet during recoil closes
Close, second outlet conducting state, while open catalyst filter flow reversal valve V4, the hydride in hydriding reactor working solution recoil tube G8
From recoil valve enter the catalyst filter, by be deposited in cartridge surface catalyst rush fall, through catalyst filter flow reversal valve V4 and touch
Matchmaker filter flow reversal house steward G9 enters working solution supply pipe G1, follows fresh working solution to return in hydrogenation reaction cauldron 1.
Oxygen content and the continuous monitoring of carbon monoxide content, wherein oxygen must be carried out to the hydrogen that hydrogen feed pipe G2 is provided
Volumn concentration have to be lower than 1%, higher than the level, then must bypass hydrogenation reaction cauldron 1.Hydrogen feed pipe G2 supplies hydrogen
In carbon monoxide content have to be lower than 1.0ppm, it is to avoid palladium catalyst poisoning.
Reaction temperature in hydrogenation reaction cauldron 1 is 50~65 DEG C, and the working solution residence time is 0.25~0.55 hour, hydrogenation
Pressure in reactor 1 is that the pressure of fresh hydrogen in 100~150KPa, hydrogen feed pipe G2 is 0.25~0.35MPa.
Step (1) in hydrogenation solvent can be configured by following percent by volume, diisobutyl carbinol (DIBC)：（45~50）
V%, C10 aromatic hydrocarbons：（50~55）V%, both volume summations are 100%.C10 aromatic hydrocarbons is used to dissolve 2- EAQs and 2- amyl groups
Anthraquinone, diisobutyl carbinol (DIBC) increases the solubility of 2- EAQs and 2- amyl anthraquinones.
Under the solvent formula, the hydrogenation efficiency that embodiment one~tetra- reaches is as shown in table 1：
Table 1
。
Step (1) in hydrogenation solvent can also be configured by following percent by volume, tetrabutyl urea：（12~30）V%,
Trioctyl phosphate：（8~12）V%, C10 aromatic hydrocarbons：（60~76）V%, the volume summation of three is 100%.C10 aromatic hydrocarbons mainly dissolves
The tetrahydrochysene 2- EAQs that 2- EAQs, 2- amyl anthraquinones and reaction are produced, and the 2- ethyls generated after hydrogenation can not be dissolved
Hydrogen anthraquinone and tetrahydrochysene 2- ethyl hydrogen anthraquinones；Therefore also need to that the tricresyl phosphate of 2- ethyl hydrogen anthraquinones and tetrahydrochysene 2- EAQs can be dissolved
Monooctyl ester and tetrabutyl urea are used as polar solvent.The present invention has higher C10 arene contents, and working solution proportion can be avoided to increase
Greatly, extraction tower operating difficulties is caused；Trioctyl phosphate has the advantages that high boiling point, non-stimulated taste, dissolved hydrogen anthraquinone ability are strong,
But if too high levels, work fluid viscosity can be caused to increase, cause mass transfer difficult；Tetrabutyl urea is transparent or slightly slightly yellow
Liquid, viscosity is slightly bigger than water, has the advantages that and water density difference is big, surface tension is big, relative to trioctyl phosphate to 2-
The solubility of ethyl hydrogen anthraquinone and tetrahydrochysene 2- EAQs is big, and distribution coefficient of the hydrogen peroxide in two-phase is big.Using the present invention
Solvent composition combination and ratio so that working solution have volatilization loss it is small, using safety, favourable operating environment, reduction raffinate
Liquid hydrogen peroxide content, the advantage for improving extract concentration, due to being reduced with the stock solubility of water so that dioxygen aquatic products
TOC（Total organic carbon）Content is greatly reduced, and is conducive to the lifting of product quality.
Under the solvent formula, the hydrogenation efficiency that embodiment five~eight reaches is as shown in table 2：
Table 2
。
It the foregoing is only the preferable possible embodiments of the present invention, non-therefore the limitation present invention patent protection model
Enclose.In addition to the implementation, the present invention can also have other embodiment, and the direction of such as left and right can be exchanged, all uses etc.
With the technical scheme replaced or equivalent transformation is formed, all fall within the protection domain of application claims.The present invention is without description
Technical characteristic can be realized by or using prior art, will not be repeated here.
Claims (10)
1. a kind of fluid bed hydrogenation system for producing hydrogen peroxide, including vertical hydrogenation reaction cauldron, it is characterised in that：Institute
State and hydride outlet is uniformly provided with the lower circumference of hydrogenation reaction cauldron, each hydride outlet is respectively with being looped around hydrogenation instead
The hydride loop pipe of kettle periphery is answered to be connected, the hydride loop pipe is connected with catalyst filter general import pipe, the catalyst
Filter inlet valve of the filter general import pipe respectively with each catalyst filter inlet is connected；The outlet difference of each catalyst filter
Triple valve is installed, the first outlet of the triple valve is connected with hydride outlet pipe, the second outlet and hydrogen of the triple valve
Change kettle working solution recoil tube to be connected；Agitating shaft is provided with along the center line of the hydrogenation reaction cauldron, the agitating shaft is provided with stirring
Blade；The bottom of each catalyst filter is separately installed with catalyst filter flow reversal valve, and each catalyst filter flow reversal valve goes out
Mouth is connected with catalyst filter flow reversal house steward respectively, lower end and the working solution supply pipe phase of the catalyst filter flow reversal house steward
Even, the working solution supply pipe is inserted the inner chamber of hydrogenation reaction cauldron from the middle part of the hydrogenation reaction cauldron short transverse and is turned under
Song extends to the axis of the hydrogenation reaction cauldron；The top of the hydrogenation reaction cauldron is provided with hydriding reactor gaseous phase outlet and grafting respectively
There are the catalyst adding tube extended straight down and hydrogen feed pipe, valve is added with touching in the upper end of the catalyst adding tube by catalyst
The outlet connection of matchmaker's addition tank, inwall of the hydrogen feed pipe along hydrogenation reaction cauldron extends to the bottom of hydrogenation reaction cauldron and turned
The curved lower central for extending upwardly to the hydrogenation reaction cauldron.
2. the fluid bed hydrogenation system of production hydrogen peroxide according to claim 1, it is characterised in that：The stirring
The top of axle is set with center sleeve, and the upper end of the center sleeve is connected with the inwall closing of the hydrogenation reaction cauldron, described
The lower end of center sleeve is inserted into the liquid Space of hydrogenation reaction cauldron.
3. the fluid bed hydrogenation system of production hydrogen peroxide according to claim 2, it is characterised in that：The hydrogenation
Kettle gaseous phase outlet is connected with the air inlet of condenser, and the exhaust outlet of the condenser is vented by Exhaust Emission Control valve and tail gas
Pipe is connected, and the leakage fluid dram of the condenser is connected by condensate liquid return duct with the top of the center sleeve.
4. the fluid bed hydrogenation system of production hydrogen peroxide according to claim 1, it is characterised in that：Along the hydrogen
Change the inwall of reactor liquid Space at least provided with vertical baffle plate together, the cross section of the vertical baffle plate is along hydrogenation reaction cauldron
Diameter extends.
5. the fluid bed hydrogenation system of production hydrogen peroxide according to claim 1, it is characterised in that：The catalyst
The lower end of filter flow reversal house steward is connected with backflow pipe bend, and the working solution supply pipe is inserted in the lower end of the backflow pipe bend
In, the outlet of the backflow pipe bend is positioned at the center of the working solution supply pipe and in the same direction with the flow direction of working solution.
6. the fluid bed hydrogenation system of production hydrogen peroxide according to claim 1, it is characterised in that：The catalyst
The lower end of filter flow reversal house steward is connected on the big end circumference of taper, and taper is sleeved on the working solution supply pipe
Periphery and with working solution supply pipe coaxial line, the big end seal of taper closes, and the small end of taper is towards hydrogenation reaction cauldron
And it is relative with working solution supply pipe connect, the working solution supply pipe is located at part in taper provided with reduced diameter
Aditus laryngis, the aditus laryngis stretches to the small end of taper.
7. the fluid bed hydrogenation system of production hydrogen peroxide according to claim 1, it is characterised in that：The hydrogenation
The bottom of reactor is provided with the annular sleeve with hydrogenation reaction cauldron coaxial line, the circumference of the annular sleeve and the hydrogenation reaction cauldron
Inwall is spaced a distance, and each hydride outlet is located at the hydrogenation reaction cauldron, and axially middle part is contour with the annular sleeve
On circumference；The bottom of the agitating shaft is provided with lower stirring paddle leaf, and the lower stirring paddle leaf is located in the annular sleeve, the stirring
The middle part of axle is provided with upper stirrer paddle；The outlet of the working solution supply pipe is positioned at the top of the upper stirrer paddle；The hydrogen
Lower section of the outlet of gas supply pipe positioned at the annular sleeve lower port center.
8. the fluid bed hydrogenation system any one of a kind of use claim 3 to 7 produces the hydrogenation of hydrogen peroxide
Reaction method, it is characterised in that in turn include the following steps, (1) configures hydrogenation solvent；(2) 2- is added into above solvent
The working solution of hydrogenation is constituted after EAQ and 2- amyl anthraquinones, wherein adding 2- EAQs in every liter of solvent（80~
110）2- amyl anthraquinones are added in g/L, every liter of solvent（60~140）g/L；(3) powdered palladium catalyst, the grain of the palladium catalyst are prepared
Footpath volume distributed median is：The percent by volume that particle diameter is more than 120 microns is no more than 4%；Particle diameter is less than 80 microns of percent by volume not
More than 4%, remaining particle diameter is 80~120 microns；(4) open catalyst addition valve and appropriate catalyst is put into hydrogenation reaction cauldron, together
Shi Xinxian working solution enters the center of hydrogenation reaction cauldron liquid Space from working solution supply pipe and sprayed downwards, in stirrer paddle
Agitation under spread to surrounding downwards；Fresh hydrogen sprays upwards from the lower port of hydrogen feed pipe, in the agitation of stirrer paddle
Under be separated into multiple minute bubbles and spread upward all round, be sufficiently mixed and stir with fresh working solution；(5) the anthracene in working solution
Quinone generates hydrogen anthraquinone in the presence of powdered palladium catalyst with hydrogen reaction；(6) the gaseous substance on hydrogenation reaction cauldron top is from hydriding reactor
Gaseous phase outlet escapes and enter condenser condensation, and incoagulable gas includes unreacted hydrogen and discharged from tail gas blow-down pipe, condensation
Liquid is returned in center sleeve；(7) hydride enters together with powder catalyst from each hydride outlet in hydrogenation reaction cauldron lower circumference
Hydride loop pipe, then filtered through catalyst filter general import pipe into each catalyst filter；Triple valve is switched into first to go out
Mouthful conducting, second outlet closed mode, after catalyst filter retains catalyst, the first outlet of the hydride of cleaning from triple valve
Flow out into hydride outlet pipe；(8) each catalyst filter is recoiled in turn, triple valve is switched to first during recoil
Port closing, second outlet conducting state, while opening the hydrogenation in catalyst filter flow reversal valve, hydriding reactor working solution recoil tube
Liquid from recoil valve enter the catalyst filter, by be deposited in cartridge surface catalyst rush fall, through catalyst filter flow reversal valve and touch
Matchmaker's filter flow reversal house steward enters working solution supply pipe, follows fresh working solution to return in hydrogenation reaction cauldron.
9. it is according to claim 8 production hydrogen peroxide hydrogenation processes, it is characterised in that step (1) in hydrogenation
Reaction dissolvent is configured by following percent by volume, diisobutyl carbinol (DIBC)：（45~50）V%, C10 aromatic hydrocarbons：（50~55）V%, both
Volume summation be 100%.
10. it is according to claim 8 production hydrogen peroxide hydrogenation processes, it is characterised in that step (1) in hydrogen
Change reaction dissolvent to configure by following percent by volume, tetrabutyl urea：（12~30）V%, trioctyl phosphate：（8~12）V%, C10 virtue
Hydrocarbon：（60~76）V%, the volume summation of three is 100%.
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| CN109678121A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of efficient hydrogenation process and system of hydrogen dioxide solution production by anthraquinone process |
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