CN206901770U - The system of process for prepairng hydrogen peroxide by anthraquinone - Google Patents

Abstract

It the utility model is related to a kind of system of process for prepairng hydrogen peroxide by anthraquinone, the bottom of working liquid tank is by working liquid pump and working solution supply pipe is connected with the entrance of hydrogenation apparatus, the outlet of hydrogenation apparatus is connected with hydrogenation flow container, the bottom for hydrogenating flow container is connected by hydrogenating liquid pump, hydrogenation flow container efferent duct, hydrogenation liquid filter and hydride cooler with the entrance of oxidizing tower, and the outlet of oxidizing tower is connected with oxidation solution efferent duct；The outlet of hydrogenation reaction cauldron is connected with catalyst filter, and the outlet of each catalyst filter is connected with hydride outlet pipe and hydriding reactor working solution recoil tube respectively；Each catalyst filter bottom is connected with working solution supply pipe, and working solution supply pipe inserts the inner chamber of hydrogenation reaction cauldron from middle part；Catalyst adding tube is plugged with the top of hydrogenation reaction cauldron, 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 system can continuous production, unit consumption of product is low, and production efficiency is high.

Description

The system of process for prepairng hydrogen peroxide by anthraquinone

Technical field

A kind of system of process for prepairng hydrogen peroxide by anthraquinone is the utility model is related to, belongs to hydrogen peroxide manufacturing technology 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 generally is 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 carried out typically 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 be less than normal, product production Raw material and power unit consumption are high, equipment is heavy, floor space is big, and manufacturing cost is high.

Hydrogen anthraquinone liquid is commonly called as hydride, after filtering and cooling, is admitted to oxidizing tower oxidation.Traditional oxidizing tower is sky Chamber tower body, hydride and air enter in oxidizing tower from bottom simultaneously, stir while up, air bubble is bigger, hydrogen It is small to change the contact area of liquid and air, oxidation efficiency will generally set to save in oxidation and be saved in tower, oxidation under tower and oxidation than relatively low Save tower to carry out after repeatedly aoxidizing, extraction process could be entered.Equipment investment is big, and oxidation efficiency is low.

Utility model content

The purpose of this utility model is, overcomes problems of the prior art, there is provided a kind of anthraquinone production peroxide Change the system of hydrogen, facility compact, continuous production can be achieved, the production consumption of unit product is low, and production efficiency is high, manufacturing cost It is low.

To solve above technical problem, a kind of system of process for prepairng hydrogen peroxide by anthraquinone of the present utility model, including work Flow container, hydrogenation apparatus, hydrogenation flow container and oxidizing tower, the bottom of the working liquid tank are connected with the entrance for the liquid pump that works, institute The outlet for stating work liquid pump is connected by working solution supply pipe with the entrance of the hydrogenation apparatus, the hydrogenation apparatus Outlet by hydride outlet pipe with it is described hydrogenation flow container be connected, it is described hydrogenation flow container bottom with hydrogenation liquid pump entrance connect Connect, the outlet of the hydrogenation liquid pump is by hydrogenating flow container efferent duct, hydrogenation liquid filter and hydride cooler and the oxidation The entrance of tower is connected, and the outlet of the oxidizing tower is connected with oxidation solution efferent duct, and the hydrogenation apparatus includes hydrogenation Kettle, hydride outlet is uniformly provided with the lower circumference of the hydrogenation reaction cauldron, each hydride outlet is respectively with being looped around The hydride loop pipe of hydrogenation reaction cauldron periphery is connected, and the hydride loop pipe is connected with catalyst filter general import pipe, institute Filter inlet valve of the catalyst filter general import pipe respectively with each catalyst filter inlet is stated to be connected；Each catalyst filter goes out Mouth is separately installed with triple valve, and the first outlet of the triple valve is connected with hydride outlet pipe, and the second of the triple valve goes out Mouth is connected with hydriding reactor working solution recoil tube；Agitating shaft is provided with along the center line of the hydrogenation reaction cauldron, is set on the agitating shaft There is stirrer paddle；The bottom of each catalyst filter is separately installed with catalyst filter flow reversal valve, each catalyst filter flow reversal The outlet of valve is connected with catalyst filter flow reversal house steward respectively, and lower end and the working solution of the catalyst filter flow reversal house steward supply Pipe is connected, the working solution supply pipe from the middle part of the hydrogenation reaction cauldron short transverse insert hydrogenation reaction cauldron inner chamber and to It is lower to bend 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 difference The catalyst adding tube extended straight down and hydrogen feed pipe are plugged with, valve is added in the upper end of the catalyst adding tube by catalyst Outlet with catalyst addition tank is connected, and inwall of the hydrogen feed pipe along hydrogenation reaction cauldron extends to the bottom of hydrogenation reaction cauldron And turn round and extend upwardly to the lower central of the hydrogenation reaction cauldron.

Relative to prior art, the utility model achieves following beneficial effect：Working solution in working liquid tank is by working Liquid pump is conveyed by working solution supply pipe to hydrogenation apparatus, and the hydride of hydrogenation apparatus production passes through hydride outlet Pipe enters hydrogenation flow container and kept in, and is then pumped into hydrogenation flow container efferent duct by hydride, and first hydrogenated liquid filter, which filters off, removes The temperature of hydride is reduced to less than 40 DEG C by impurity, hydride cooler, is sent into oxidizing tower and is aoxidized, oxidation solution is oxidized Liquid efferent duct exports.When hydrogenation apparatus produces hydride, open catalyst addition valve and appropriate catalyst is put into hydrogenation Kettle, while fresh working solution enters the center of hydrogenation reaction cauldron liquid Space from working solution supply pipe and sprayed downwards, is stirring Mix and spread under the agitation of blade to surrounding downwards；Fresh hydrogen sprays upwards from the lower port of hydrogen feed pipe, in stirrer paddle Agitation under be separated into multiple minute bubbles and spread upward all round, the opposite convection current of fresh working solution and hydrogen enables both It is enough to mix and react rapidly；Anthraquinone in working solution reacts generation hydrogen anthraquinone, nitrogen in the presence of powdered palladium catalyst with hydrogen Discharged with remaining unreacted hydrogen from the hydriding reactor gaseous phase outlet at the top of hydrogenation reaction cauldron.In the lower circumference of hydrogenation reaction cauldron It is uniformly arranged hydride outlet and imports hydride loop pipe, is advantageous to hydride and is uniformly flowed out in whole circumference.It is most of Catalyst filter is normally all in working condition, and now triple valve is in first outlet conducting, second outlet closed mode, catalyst After filter retains catalyst, the hydride of cleaning flows out into hydride outlet pipe from the first outlet of triple valve；When tactile When accumulating excessive catalyst on the filter core of matchmaker's 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, influences the progress of hydrogenation, triple valve now is switched into first outlet closes Close, second outlet conducting state, while open catalyst filter flow reversal valve, the hydride in hydriding reactor working solution recoil tube enters The catalyst filter, the catalyst punching for being deposited in cartridge surface is fallen, it is total through catalyst filter flow reversal valve and catalyst filter flow reversal Pipe enters working solution supply pipe, follows fresh working solution to return in hydrogenation reaction cauldron, all catalyst are recycled.If Multiple catalyst filters are put, are easy to carry out the recoil of catalyst in turn, it is ensured that fluid bed being capable of continuous and stable production；Such as fluid bed At work, a catalyst filter is kept to be in recoil state, remaining catalyst filter is in working condition, can both carry High efficiency, the yield of hydrogen anthraquinone is improved, the filter efficiency of each catalyst filter can be ensured again, ensured in hydrogenation reaction cauldron The concentration of catalyst, make fluid bed all the time in stable working condition.By the commutation of triple valve, normal work is cut with recoil Change very convenient quick.System hydrogenation of the present utility model is rapid, and the catalyst concentration in hydrogenation reaction cauldron is stable, Neng Gouwen The hydride of fixed continuous output high-quality, and hydrogen unit consumption is low, hydrogenation efficiency is high.

As improvement of the present utility model, the top of the agitating shaft is set with center sleeve, the center sleeve it is upper End and the inwall closing of the hydrogenation reaction cauldron connect, and the lower end of the center sleeve is inserted into the liquid Space of hydrogenation reaction cauldron In；The hydriding reactor gaseous phase outlet is connected with the air inlet of reactor condenser, and the exhaust outlet of the reactor condenser passes through Exhaust Emission Control valve is connected with tail gas blow-down pipe, the leakage fluid dram of the reactor condenser by condensate liquid return duct with it is described The top of center sleeve is connected.Center sleeve and permeability cell form fluid-tight to the gas-phase space at the top of hydrogenation reaction cauldron, will condense Liquid passage is kept apart with the gas-phase space at the top of hydrogenation reaction cauldron, and the condensate liquid for entering center sleeve is delivered into reactor The central area of liquid Space.The reacted kettle condensers of non-incoagulable gas such as the solvent vapo(u)r from the discharge of hydriding reactor gaseous phase outlet Again turn into liquid after condensation, center sleeve is flowed back to from condensate liquid return duct, continue to participate in the reaction of hydrogenation reaction cauldron, be advantageous to Reduce material loss；Exhaust Emission Control valve can control the discharge capacity of tail gas and adjust the pressure in hydrogenation reaction cauldron, center The fluid-tight effect of sleeve pipe can avoid the gas at the top of hydrogenation reaction cauldron from entering condensate liquid return duct, and condensate liquid is from center sleeve Lower end outflow after directly arrival reactor liquid Space central area, under the agitation of stirrer paddle rapidly with fresh work Liquid mixing is common to spread downwards to surrounding, with the upward uniform hybrid reaction of hydrogen.

As further improvement of the utility model, along the inwall of the hydrogenation reaction cauldron liquid Space at least provided with together Vertical baffle plate, the diameter extension of the cross section of the vertical baffle plate along hydrogenation reaction cauldron.The rotation of stirrer paddle, work can be driven Liquid is rotated, and circulation is formed in hydrogenation reaction cauldron inner chamber, and stable circulation causes the material of circulation outer layer and the material of circulation internal layer It is difficult to mix；Vertical baffle plate is radially inserted in circulation layer, is advantageous to thoroughly destroy circulation layer so that working solution can with hydrogen Hydrogenation occurs for rapid uniformly mixing.

As further improvement of the utility model, the lower end of the catalyst filter flow reversal house steward is connected to taper Big end circumference on, taper be sleeved on the periphery of the working solution supply pipe and with working solution supply pipe coaxial line, taper The big end seal of sleeve pipe is closed, the small end of taper towards hydrogenation reaction cauldron and it is relative with working solution supply pipe connect, the working solution The part that supply 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. The catalyst of catalyst filter recoil recovery enters in taper from catalyst filter flow reversal house steward, and fresh working solution is in working solution Supply pipe high speed flow forward, flow velocity is accelerated at aditus laryngis, and pressure reduces, and suction is played to entering the catalyst in taper Effect, catalyst are able to be uniformly dispersed rapidly in fresh working solution, avoid catalyst conglomeration from entering hydrogenation reaction cauldron.

As further improvement of the utility model, the bottom of the hydrogenation reaction cauldron is provided with and hydrogenation reaction cauldron coaxial line Annular sleeve, the inwall of the circumference of the annular sleeve and the hydrogenation reaction cauldron is spaced a distance, each hydride outlet On the circumference contour positioned at the hydrogenation reaction cauldron and annular sleeve axial direction middle part；The bottom of the agitating shaft is provided with lower stirring Blade, the lower stirring paddle leaf are located in the annular sleeve, and the middle part of the agitating shaft is provided with upper stirrer paddle；The working solution The outlet of supply pipe is positioned at the top of the upper stirrer paddle；The outlet of the hydrogen feed pipe is located at the annular sleeve lower port The lower section at center.Annular sleeve is formed to each hydride outlet and blocked, and fresh hydrogen is after the discharge of the port of hydrogen feed pipe, first The center of annular sleeve is upwardly into, 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, Under the rotational agitation of upper stirrer paddle, on one side downwards on one side disperse to surrounding, be advantageous to rising hydrogen gas bubbles uniformly mix Close, hydrogenation occurs rapidly, the fresh working solution that annular sleeve can equally avoid having just enter into directly chokes from hydride outlet； The working solution sprayed downwards flows 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 contacts, and is advantageous to improve hydrogenation efficiency.

As further improvement of the utility model, the top center of the oxidizing tower is provided with oxidizing tower gaseous phase outlet, institute The upper portion side wall for stating oxidizing tower is connected with oxidizing tower hydride entrance, and the oxidizing tower hydride entrance is located at the liquid level of oxidizing tower Above line, the bottom of the oxidizing tower is provided with air distribution device, and the air distribution device and the oxidizing tower on oxidizing tower are total Air intake connects, and the bottom centre of the oxidizing tower exports provided with oxidizing tower；It is horizontal that multiple tracks is provided with along oxidizing tower short transverse The oxidation tower tray of shape, the oxidation tower tray of adjacent layer mutually stagger make the runner of working solution S-shaped in the horizontal direction.Compressed air quilt The air distribution device of bottom is distributed into numerous bubbles, flows from bottom to top；Hydrogen anthraquinone liquid enters from the oxidizing tower hydride on top Mouthful enter oxidizing tower in, fall first on the oxidation tower tray of top layer, it is then S-shaped successively to flow downward, hydrogen anthraquinone liquid while to Lower flowing, while oxidation reaction generation hydrogen peroxide occurs with the oxygen in bubble, counter-current flow, work is presented with air in working solution What is contacted when flowing to oxidation tower bottom as liquid is most ozone, to ensure that oxidation reaction is properly completed, then from bottom Oxidizing tower outlet outflow.The oxidation tower tray of adjacent layer mutually stagger in the horizontal direction working solution is flowed downward while Horizontal direction, which is formed, repeatedly turns back, and extends the flow distance of working solution, also extends the time of contact of working solution and oxygen, have Hydrogen peroxide is turned into by exhaustive oxidation beneficial to hydrogen anthraquinone liquid.Oxidizing tower hydride entrance, which is located above liquid level line, can prevent to aoxidize Liquid is choked in hydrogen anthraquinone liquid pipe road, is avoided forming upper track and is polluted.

As further improvement of the utility model, each oxidation tower tray is circular in unfilled corner, each oxidation tower tray Middle part is oxide regions, and the oxide regions are uniformly densely covered with multiple oxidation tower tray air-vents, two sides of the oxide regions Along being parallel to each other, the side of the oxide regions is the descending liquid region of hollow out, and the opposite side of the oxide regions is by closed plate The liquid receiving area domain of composition, the oxide regions are connected with the periphery in liquid receiving area domain with the inwall of oxidizing tower；Adjacent layer descending liquid The phase in region differs 180 °；The oxidation tower tray edge adjacent with descending liquid region is connected with vertical baffle plate, the vertical gear The upper limb of plate is parallel and crosses oxidation tower tray higher than oxidation tower tray, the lower edge of the vertical baffle plate and extends downwardly.The work on upper strata Liquid falls in the liquid receiving area domain being made up of closed plate first, then horizontal to be flowed to oxide regions；During air flows upwards, minute bubbles Easily mutually collide, assemble, being bonded into larger bubble, when air pocket is reached below the oxide regions of oxidation tower tray, by oxygen Change tower tray air-vent and be divided into numerous minute bubbles again, considerably increase the specific surface area of bubble, the oxidized area for the treatment of fluid flow During domain, it is in contact with countless minute bubbles, contact area is big, good mixing.Air pocket is oxidized tower for several times in uphill process Disk is divided into tiny bubble again, substantially increases oxidation efficiency, as long as an oxidizing tower can be properly completed hydrogen anthraquinone liquid Oxidation, reduce equipment investment and production cost.Working solution can just flow downward in the oxidation excessively vertical baffle plate of tower tray overflow, Residence time of the working solution in oxide regions is extended, is advantageous to be substantially oxidized；The lower edge of vertical baffle plate extends downwardly simultaneously One segment distance, the air chamber of lower ending opening is collectively forming with oxidation tower tray and oxidizing tower barrel, by air seal in the case where aoxidizing tower tray Side, avoids air from being flowed directly up from descending liquid region, forces air across each oxidation tower tray air-vent and flows up, complete by force The cutting of paired air pocket.

As further improvement of the utility model, the inner chamber of the oxidizing tower is provided with inlet bend and the oxidizing tower hydrogen To change liquid entrance to be connected, the lower end outlet of the inlet bend is located at the liquid level line lower section of oxidizing tower and the inwall of close oxidizing tower, The liquid receiving area domain of top layer oxidation tower tray is located at the underface of the inlet bend.The lower end outlet of inlet bend is located under liquid level line Side, forms fluid-tight, and hydrogen anthraquinone liquid flows downward, and fall after the lower end of inlet bend outlet outflow along the inwall of oxidizing tower Top layer aoxidizes the liquid receiving area domain of tower tray, and then advection to oxide regions is aoxidized, it is ensured that all hydrogen anthraquinone liquid is complete Oxidized region is flowed through, makes oxidation more thorough.

As further improvement of the utility model, oxidizing tower capturing device is installed at the oxidizing tower gaseous phase outlet, Each layer oxidation tower tray is respectively arranged below with spiral condenser, and the outer wall of the oxidizing tower is wound with multigroup semicanal condenser, Each semicanal condenser is respectively between adjacent two layers oxidation tower tray, and using the flow direction of low in and high out.Oxidizing tower traps Device can catch foam, avoid droplets from flying out from oxidizing tower gaseous phase outlet；Because the oxidation reaction of hydrogen anthraquinone liquid is that heat release is anti- Should, spiral condenser is respectively arranged below in each layer oxidation tower tray, working solution can be cooled down in time；Each semicanal is cold Condenser can be cooled down paragraph by paragraph to oxidizing tower, make the uniform temperature fields of whole oxidizing tower.

Brief description of the drawings

The utility model is described in further detail with reference to the accompanying drawings and detailed description, accompanying drawing only provides ginseng Examine and used with explanation, be not used to limit the utility model.

Fig. 1 is the flow chart of the system of the utility model process for prepairng hydrogen peroxide by anthraquinone.

Fig. 2 is the structural representation of hydrogenation reaction cauldron in Fig. 1.

Fig. 3 is the top view of hydride outlet and hydride loop pipe in Fig. 2.

Fig. 4 is catalyst filter flow reversal house steward and the schematic diagram of second of connection scheme of working solution supply pipe.

Fig. 5 is the front view of oxidizing tower in Fig. 1.

Fig. 6 is the top view that odd-level aoxidizes tower tray in Fig. 5.

Fig. 7 is the top view that even level aoxidizes tower tray in Fig. 5.

Fig. 8 is the structural representation of spiral condenser in Fig. 5.

Fig. 9 is the structural representation of air distribution device in Fig. 5.

Figure 10 is the schematic cross-section of air branch pipe in Fig. 9.

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. reactor is cold Condenser；4. catalyst filter；5. oxidizing tower；5a. oxidizing tower gaseous phase outlets；5b. oxidizing tower hydride entrances；5c. oxidizing towers are total Air intake；5d. oxidizing towers export；5e. oxidizing tower capturing devices；5f. inlet bends；5g. aoxidizes tower tray；5g1. zoneofoxidation Domain；5g2. liquid receiving areas domain；5g3. descending liquids region；5. aoxidize tower tray air-vent；The vertical baffle plates of 5h.；5j. spiral condensers；5k. Semicanal condenser；5m. air distribution devices；5m1. air mains；5m2. air branch pipe；5m3. air dispensing orifices；V1. catalyst adds Add valve；V2. triple valve；V3. filter inlet valve；V4. catalyst filter flow reversal valve；V5. Exhaust Emission Control valve；T1. work Flow container；T2. flow container is hydrogenated；L1. liquid filter is hydrogenated；C1. hydride cooler；B1. work liquid pump；B2. liquid pump is hydrogenated；G1. Working solution supply pipe；G1a. taper；G2. hydrogen feed pipe；G3. catalyst adding tube；G4. tail gas blow-down pipe；G5. condensate liquid Return duct；G6. catalyst filter general import pipe；G7. hydride outlet pipe；G8. hydriding reactor working solution recoil tube；G9. catalyst mistake Filter return header；G10. flow container efferent duct is hydrogenated；G11. compressed air hose；G12. oxidation solution efferent duct.

Embodiment

As shown in Figure 1 and Figure 2, the system of the utility model process for prepairng hydrogen peroxide by anthraquinone includes working liquid tank T1, hydrogenation instead Device, hydrogenation flow container T2 and oxidizing tower 5 are answered, working liquid tank T1 bottom is connected with the entrance for the liquid pump B1 that works, work liquid pump B1 Outlet be connected by working solution supply pipe G1 with the entrance of hydrogenation apparatus, the outlet of hydrogenation apparatus passes through hydride Outlet G7 is connected with hydrogenation flow container T2, and hydrogenation flow container T2 bottom is connected with hydrogenating liquid pump B2 entrance, hydrogenation liquid pump B2's Outlet is by hydrogenating flow container efferent duct G10, hydrogenation liquid filter L1 and hydride cooler C1 is connected with the entrance of oxidizing tower 5, The outlet of oxidizing tower 5 is connected with oxidation solution efferent duct G12.

Working solution in working liquid tank T1 is conveyed from work liquid pump B1 by working solution supply pipe G1 to hydrogenation apparatus, The hydride of hydrogenation apparatus production enters hydrogenation flow container T2 by hydride outlet pipe G7 and kept in, then by hydrogenation liquid pump B2 Hydrogenation flow container efferent duct G10 is sent into, first hydrogenated liquid filter L1 filters off the removal of impurity, and filtering accuracy is 1 μ, and hydride cools down The temperature of hydride is reduced to less than 40 DEG C by device C1, is sent into the oxidation of the row of oxidizing tower 5, and the oxidized liquid efferent duct G12 of oxidation solution is defeated Go out.

As shown in Fig. 2 hydrogenation apparatus includes hydrogenation reaction cauldron 1, it is uniformly provided with the lower circumference of hydrogenation reaction cauldron 1 Hydride outlet 1b, each hydride outlet 1b are connected with being looped around the hydride loop pipe 1h of hydrogenation reaction cauldron periphery respectively, hydrogen Change liquid loop pipe 1h be connected with catalyst filter general import pipe G6, catalyst filter general import pipe G6 respectively with each catalyst filter The filter inlet valve V3 of 4 entrances is connected；The outlet of each catalyst filter 4 is separately installed with triple valve V2, and the of triple valve V2 One outlet is connected with hydride outlet pipe G7, and triple valve V2 second outlet is connected with hydriding reactor working solution recoil tube G8；Along hydrogen The center line for changing reactor 1 is provided with agitating shaft 1f, and agitating shaft 1f is provided with stirrer paddle 1g；The bottom of each catalyst filter 4 point Be not provided with catalyst filter flow reversal valve V4, each catalyst filter flow reversal valve V4 outlet respectively with catalyst filter flow reversal house steward G9 is connected, and catalyst filter flow reversal house steward G9 lower end is connected with working solution supply pipe G1, and working solution supply pipe G1 is anti-from hydrogenation The middle part of kettle short transverse is answered to insert the inner chamber of hydrogenation reaction cauldron 1 and be bent downwardly the axis for extending to hydrogenation reaction cauldron 1；Hydrogenation The top of reactor 1 is provided with hydriding reactor gaseous phase outlet 1a and is plugged with the catalyst adding tube G3 and hydrogen extended straight down respectively Supply pipe G2, catalyst adding tube G3 upper end are added valve V1 by catalyst and are connected with the outlet of catalyst addition tank 2, hydrogen feed pipe Inwalls of the G2 along hydrogenation reaction cauldron 1 extends to the bottom of hydrogenation reaction cauldron 1 and turn extends upwardly to the bottom of hydrogenation reaction cauldron 1 Center.

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 fresh working solution enables both to mix and react rapidly with the opposite convection current of hydrogen；Work Make the anthraquinone in liquid and react generation hydrogen anthraquinone with hydrogen in the presence of powdered palladium catalyst, 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 advantageous to hydride and is uniformly flowed out in whole circumference.

Most of catalyst filters 4 are normally 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 opens catalyst filter flow reversal valve V4, is hydrogenated Hydride in kettle working solution recoil tube G8 enters the catalyst filter, the catalyst punching for being deposited in cartridge surface is fallen, through catalyst Filter flow reversal valve V4 and catalyst filter flow reversal house steward G9 enters working solution supply pipe G1, follows fresh working solution to return to hydrogenation In reactor 1, 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； Such as fluid bed is at work, a catalyst filter is kept to be in recoil state, remaining catalyst filter is in work shape State, production efficiency can be both improved, improve the yield of hydrogen anthraquinone, the filter efficiency of each catalyst filter can be ensured again, ensured The concentration of catalyst in hydrogenation reaction cauldron 1, make 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 reactor condenser 3, and the exhaust outlet of reactor condenser 3 passes through Exhaust Emission Control valve V5 is connected with tail gas blow-down pipe G4, the leakage fluid dram of reactor condenser 3 by condensate liquid return duct G5 with Center sleeve 1c top is connected.The reacted kettles of non-incoagulable gas such as the solvent vapo(u)r from hydriding reactor gaseous phase outlet 1a discharges are cold Condenser 3 turns into liquid again after condensing, and center sleeve 1c is flowed back to from condensate liquid return duct G5, continues to participate in hydrogenation reaction cauldron 1 Reaction, be advantageous to reduce material loss；Exhaust Emission Control valve V5 can control the discharge capacity of tail gas and adjust hydrogenation reaction cauldron 1 Interior pressure；Center sleeve 1c and permeability cell form fluid-tight to the gas-phase space at the top of hydrogenation reaction cauldron, by condensate liquid passage with Gas-phase space at the top of hydrogenation reaction cauldron is kept apart, and the gas at the top of hydrogenation reaction cauldron can be avoided to enter condensate liquid return duct G5, condensate liquid directly reaches the central area of reactor liquid Space after the outflow of center sleeve 1c lower end, in stirrer paddle Mix with fresh working solution rapidly under 1g agitation and spread jointly to surrounding downwards, 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 together, vertical baffle plate 1d cross section edge The diameter extension of hydrogenation reaction cauldron 1.Stirrer paddle 1g rotation, working solution can be driven to rotate, be formed in hydrogenation reaction cauldron inner chamber Circulation, stable circulation cause 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 advantageous to thoroughly destroy 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 for the pipe bend that flows back In supply pipe G1, the outlet of the pipe bend that flows back is positioned at working solution supply pipe G1 center and in the same direction with the flow direction of working solution. Catalyst from the catalyst filter flow reversal house steward G9 of each catalyst filter recoil recovery 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 spread rapidly in fresh working solution Open, play mixed uniformly effect, avoid catalyst conglomeration from entering 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 the part that liquid supply pipe G1 is located in taper G1a is provided with reduced diameter, aditus laryngis stretches to taper G1a Small end.The catalyst of catalyst filter recoil recovery 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, and pressure reduces, into taper Catalyst in G1a plays swabbing action, and catalyst is able to be uniformly dispersed rapidly in fresh working solution, avoids catalyst conglomeration from entering 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 In the lower section at annular sleeve lower port center.

Annular sleeve 1e is formed to each hydride outlet 1b and blocked, 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, which smashes and is separated into multiple bubbles, enters 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 disperseing to surrounding, the hydrogen for being advantageous to and rising Gas bubble uniformly mixes, 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 flows 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 advantageous to improve hydrogenation efficiency.

As Fig. 5 shows, the top center of oxidizing tower 5 is provided with oxidizing tower gaseous phase outlet 5a, and the upper portion side wall of oxidizing tower 5 is connected with Oxidizing tower hydride entrance 5b, oxidizing tower hydride entrance 5b are located above the liquid level line of oxidizing tower 5, and the bottom of oxidizing tower 5 is set There are air distribution device 5m, air distribution device 5m to be connected with the total air intake 5c of the oxidizing tower on oxidizing tower 5, oxidizing tower is always empty Gas entrance 5c is connected with compressed air hose G11.The bottom centre of oxidizing tower 5 is provided with oxidizing tower outlet 5d；Oxidizing tower export 5d with The G12 connections of oxidation solution efferent duct.

The horizontal oxidation tower tray 5g of multiple tracks is provided with along the short transverse of oxidizing tower 5, the oxidation tower tray 5g of adjacent layer is in level Direction, which is mutually staggered, makes the runner of working solution S-shaped.

Compressed air is distributed into numerous bubbles by the air distribution device 5m of bottom, flows from bottom to top；Hydrogen anthraquinone liquid from The oxidizing tower hydride entrance 5b on top enter oxidizing tower 5 in, fall first on the oxidation tower tray 5g of top layer, then it is S-shaped by Sulfate layer flows downhill is moved, and hydrogen anthraquinone liquid is while flow downward, while oxidation reaction generation hydrogen peroxide, work occurs with the oxygen in bubble Make liquid and air and be presented counter-current flow, it is most ozone that working solution, which flows to contacted during oxidation tower bottom, to ensure oxygen Change reaction to be properly completed, then from the oxidizing tower outlet 5d outflows of bottom.The oxidation tower tray 5g of adjacent layer is mutual in the horizontal direction Staggering makes working solution flow downward repeatedly turns back while being formed in the horizontal direction, extends the flow distance of working solution, The time of contact of working solution and oxygen is extended, be advantageous to hydrogen anthraquinone liquid turns into hydrogen peroxide by exhaustive oxidation.Oxidizing tower hydrogenates Liquid entrance 5b, which is located above liquid level line, can prevent oxidation solution and choke in hydrogen anthraquinone liquid pipe road, avoid forming upper track and pollute.

As shown in Figure 6, Figure 7, respectively oxidation tower tray 5g is circular in unfilled corner, and each middle part for aoxidizing tower tray 5g is oxide regions 5g1, Oxide regions 5g1 is uniformly densely covered with multiple oxidation tower tray air-vents 5, and oxide regions 5g1 both sides edge is parallel to each other, zoneofoxidation Domain 5g1 side is the descending liquid region 5g3 of hollow out, and oxide regions 5g1 opposite side is the liquid receiving area domain being made up of closed plate 5g2, oxide regions 5g1 are connected with inwall of the liquid receiving area domain 5g2 periphery with oxidizing tower 5；The phase in adjacent layer descending liquid region 180 ° of position difference.The working solution on upper strata falls in the liquid receiving area domain 5g2 being made up of closed plate first, then horizontal to oxide regions 5g1 flows；During air flows upwards, minute bubbles are easily mutually collided, assembled, being bonded into larger bubble, when air pocket reaches When aoxidizing below tower tray 5g oxide regions 5g1, it is oxidized tower tray air-vent 5 and is divided into numerous minute bubbles again, increase The specific surface area of bubble is added, during the oxidized region 5g1 for the treatment of fluid flow, has been in contact with countless minute bubbles, contact area is big, mixes Close good.Air pocket is oxidized tower tray 5g and is divided into tiny bubble again for several times in uphill process, substantially increases oxidation Efficiency, as long as an oxidizing tower can be properly completed the oxidation of hydrogen anthraquinone liquid, reduce equipment investment and production cost.

Edge adjacent with descending liquid region 5g3 oxidation tower tray 5g is connected with vertical baffle plate 5h, and vertical baffle plate 5h upper limb is put down Go and the lower edge higher than oxidation tower tray 5g, vertical baffle plate 5h is crossed oxidation tower tray 5g and extended downwardly.Working solution is in oxidation tower tray 5g Overflow, which flows through vertical baffle plate 5h, can just flow downward, and extend residence time of the working solution in oxide regions 5g1, be advantageous to be filled Divide oxidation；Vertical baffle plate 5h lower edge extends downwardly a segment distance simultaneously, is collectively forming with oxidation tower tray 5g and oxidizing tower barrel The air chamber of lower ending opening, by air seal below oxidation tower tray 5g, air is avoided to be flowed directly up from descending liquid region 5g3, Force air across each oxidation tower tray air-vent 5 to flow up, complete the cutting to air pocket by force.

The inner chamber of oxidizing tower is connected provided with inlet bend 5f with oxidizing tower hydride entrance 5b, is brought out under inlet bend 5f Mouth is located at below the liquid level line of oxidizing tower 5 and close to the inwall of oxidizing tower 5, top layer oxidation tower tray 5g liquid receiving area domain 5g2 Inlet bend 5f underface.Inlet bend 5f lower end outlet forms fluid-tight below the liquid level line, and hydrogen anthraquinone liquid is from entrance After bend pipe 5f lower end outlet outflow, flow downward, and fall in top layer oxidation tower tray 5g liquid receiving area domain along the inwall of oxidizing tower 5 5g2, then advection to oxide regions 5g1 aoxidized, it is ensured that all hydrogen anthraquinone liquid completely flow through oxidized region 5g1, make oxidation more thorough.

The aperture for aoxidizing tower tray air-vent 5 be 3~6mm, the centre-to-centre spacing between adjacent oxidation tower tray air-vent 5 is 35~ 40mm.Make bubble that there is very big specific surface area, and each oxidation tower tray air-vent 5, the mixing with working solution can be passed through Fully.

Oxidizing tower capturing device 5e is installed at oxidizing tower gaseous phase outlet 5a.Oxidizing tower capturing device 5e can catch bubble Foam, avoid droplets from flying out from oxidizing tower gaseous phase outlet 5a.

As shown in Figure 9, Figure 10, air distribution device 5m includes the air main being connected with the total air intake 5c of oxidizing tower 5m1, air main 5m1 along oxidizing tower diameter extension, along air main 5m1 length direction be connected to more perpendicular to Air main 5m1 air branch pipe 5m2, each air branch pipe 5m2 is parallel to each other, uniform intervals and in the approximately the same plane, empty Gas main 5m1 and each air branch pipe 5m2 top are uniformly densely covered with least two air-discharging dispensing orifice 5m3 respectively.Air enters first Enter air main 5m1, be then divided into multiple tributaries and respectively enter each air branch pipe 5m2, then the air dispensing orifice by multiple rows of multiple row 5m3 is divided into tiny air bubble, and air dispensing orifice 5m3 aperture is 3~6mm so that the diameter very little of each air bubble, increases The big specific surface area of air, expands the contact surface of air and working solution, is advantageous to improve oxidation efficiency.

As shown in Figure 5, Figure 8, each layer oxidation tower tray 5g is respectively arranged below with spiral condenser 5j.Due to hydrogen anthraquinone liquid Oxidation reaction be exothermic reaction, be respectively arranged below spiral condenser 5j in each layer oxidation tower tray 5g, can be right in time Working solution is cooled down.

The outer wall of oxidizing tower 5 is wound with multigroup semicanal condenser 5k, and half and half pipework condensation device 5k is located at adjacent two layers oxygen respectively Between changing tower tray 5g, and using the flow direction of low in and high out.Half and half pipework condensation device 5k can be cooled down paragraph by paragraph to oxidizing tower 5, be made The uniform temperature fields of whole oxidizing tower.

It the foregoing is only the preferable possible embodiments of the utility model, non-therefore limitation patent of the present utility model Protection domain.In addition to the implementation, the utility model can also have other embodiment, such as the direction of left and right can be mutual Change, all technical schemes formed using equivalent substitution or equivalent transformation, all fall within the protection domain of the requires of the utility model.This Technical characteristic of the utility model without description can be realized by or using prior art, will not be repeated here.

Claims (9)

1. a kind of system of process for prepairng hydrogen peroxide by anthraquinone, including working liquid tank, hydrogenation apparatus, hydrogenation flow container and oxidation Tower, the bottom of the working liquid tank are connected with the entrance for the liquid pump that works, and the outlet of the work liquid pump passes through working solution supply pipe It is connected with the entrance of the hydrogenation apparatus, the outlet of the hydrogenation apparatus passes through hydride outlet pipe and the hydrogenation Flow container is connected, and the bottom of the hydrogenation flow container is connected with hydrogenating the entrance of liquid pump, and the outlet of the hydrogenation liquid pump passes through hydride Tank efferent duct, hydrogenation liquid filter and hydride cooler are connected with the entrance of the oxidizing tower, and the outlet of the oxidizing tower connects It is connected to oxidation solution efferent duct, it is characterised in that：The hydrogenation apparatus includes hydrogenation reaction cauldron, under the hydrogenation reaction cauldron It is uniformly provided with hydride outlet on portion's circumference, each hydride outlet is respectively with being looped around the hydride of hydrogenation reaction cauldron periphery Loop pipe is connected, and the hydride loop pipe is connected with catalyst filter general import pipe, the catalyst filter general import pipe point Filter inlet valve not with each catalyst filter inlet is connected；The outlet of each catalyst filter is separately installed with triple valve, institute The first outlet for stating triple valve is connected with hydride outlet pipe, second outlet and the hydriding reactor working solution recoil tube of the triple valve It is connected；Agitating shaft is provided with along the center line of the hydrogenation reaction cauldron, the agitating shaft is provided with stirrer paddle；Each catalyst filter Bottom be separately installed with catalyst filter flow reversal valve, the outlet of each catalyst filter flow reversal valve respectively with catalyst filter Return header is connected, and the lower end of the catalyst filter flow reversal house steward is connected with working solution supply pipe, the working solution supply pipe Insert the inner chamber of hydrogenation reaction cauldron from the middle part of the hydrogenation reaction cauldron short transverse and be bent downwardly and extend to the hydrogenation instead Answer the axis of kettle；What the top of the hydrogenation reaction cauldron was provided with that hydriding reactor gaseous phase outlet and being plugged with respectively extends straight down touches Matchmaker's adding tube and hydrogen feed pipe, the upper end of the catalyst adding tube add the outlet company of valve and catalyst addition tank by catalyst Connect, inwall of the hydrogen feed pipe along hydrogenation reaction cauldron extends to the bottom of hydrogenation reaction cauldron and turn extend upwardly to it is described The lower central of hydrogenation reaction cauldron.

2. the system of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterised in that：The top of the agitating shaft Center sleeve is set with, the upper end of the center sleeve and the inwall closing of the hydrogenation reaction cauldron connect, the center sleeve Lower end be inserted into the liquid Space of hydrogenation reaction cauldron；The air inlet phase of the hydriding reactor gaseous phase outlet and reactor condenser Even, the exhaust outlet of the reactor condenser is connected by Exhaust Emission Control valve with tail gas blow-down pipe, the reactor condensation The leakage fluid dram of device is connected by condensate liquid return duct with the top of the center sleeve.

3. the system of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterised in that：Along the hydrogenation reaction cauldron The inwall of liquid Space prolongs at least provided with vertical baffle plate together, the cross section of the vertical baffle plate along the diameter of hydrogenation reaction cauldron Stretch.

4. the system of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterised in that：The catalyst filter returns Stream house steward lower end be connected on the big end circumference of taper, taper be sleeved on the periphery of the working solution supply pipe and With working solution supply pipe coaxial line, the big end seal of taper is closed, the small end of taper towards hydrogenation reaction cauldron and with work Liquid supply pipe is relative to be connect, and the part that the working solution supply pipe is located in taper is provided with the aditus laryngis of reduced diameter, institute State the small end that aditus laryngis stretches to taper.

5. the system of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterised in that：The hydrogenation reaction cauldron Bottom is provided with the annular sleeve with hydrogenation reaction cauldron coaxial line, the inwall interval of the circumference of the annular sleeve and the hydrogenation reaction cauldron One segment distance, each hydride outlet are located 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, and the lower stirring paddle leaf is located in the annular sleeve, in the agitating shaft Portion 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 supply The outlet of pipe is positioned at the lower section at the annular sleeve lower port center.

6. the system of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterised in that：The top of the oxidizing tower Center is provided with oxidizing tower gaseous phase outlet, and the upper portion side wall of the oxidizing tower is connected with oxidizing tower hydride entrance, the oxidizing tower Hydride entrance is located above the liquid level line of oxidizing tower, and the bottom of the oxidizing tower is provided with air distribution device, the air point It is connected with device with the total air intake of the oxidizing tower on oxidizing tower, the bottom centre of the oxidizing tower exports provided with oxidizing tower；Edge Oxidizing tower short transverse is provided with the horizontal oxidation tower tray of multiple tracks, and the oxidation tower tray of adjacent layer mutually staggers make work in the horizontal direction The runner for making liquid is S-shaped.

7. the system of process for prepairng hydrogen peroxide by anthraquinone according to claim 6, it is characterised in that：It is each it is described oxidation tower tray be in Unfilled corner is circular, and the middle part of each oxidation tower tray is oxide regions, and it is saturating that the oxide regions are uniformly densely covered with multiple oxidation tower trays Stomata, the both sides edge of the oxide regions are parallel to each other, and the sides of the oxide regions is the descending liquid region of hollow out, the oxygen The opposite side for changing region is the liquid receiving area domain that is made up of closed plate, and the periphery in the oxide regions and liquid receiving area domain is and oxidizing tower Inwall be connected；The phase in adjacent layer descending liquid region differs 180 °；The oxidation tower tray edge adjacent with descending liquid region connects Vertical baffle plate is connected to, the upper limb of the vertical baffle plate is parallel and gets over peroxidating higher than oxidation tower tray, the lower edge of the vertical baffle plate Tower tray extends downwardly.

8. the system of process for prepairng hydrogen peroxide by anthraquinone according to claim 6, it is characterised in that：The inner chamber of the oxidizing tower It is connected provided with inlet bend with the oxidizing tower hydride entrance, the lower end outlet of the inlet bend is located at the liquid level of oxidizing tower It is located at the underface of the inlet bend below line and close to the inwall of oxidizing tower, the liquid receiving area domain of top layer oxidation tower tray.

9. the system of process for prepairng hydrogen peroxide by anthraquinone according to claim 6, it is characterised in that：The oxidizing tower gas phase goes out Oxidizing tower capturing device is installed, each layer oxidation tower tray is respectively arranged below with spiral condenser, the oxidizing tower at mouthful Outer wall is wound with multigroup semicanal condenser, and each semicanal condenser is respectively between adjacent two layers oxidation tower tray, and use The flow direction of low in and high out.