CN209338117U - A kind of dioxygen water preparation apparatus - Google Patents

Abstract

A kind of technical field of the new process equipment of dioxygen water preparation apparatus and chemical production process.It cannot apply including the multiple ebullated beds being sequentially connected in series, the multiple ebullated bed constitutes sequentially connected hydrogenation tower, oxidizing tower, extraction and separation tower, decompression packed tower, the hydride that hydrogenated tower obtains flows through gas-liquid separation after oxidizing tower, working solution of the liquid after extraction and separation tower multitple extraction enters decompression packed tower, at hydrogen peroxide after decompression packed tower concentration.The application realizes operation efficiently, consumes low, energy-saving and emission-reduction, reduces side reaction, guarantees the purpose of production security.

Description

A kind of dioxygen water preparation apparatus

Technical field

This application involves the technical fields of the new process equipment of chemical production process.

Background technique

The hydrogen peroxide producer of existing domestic technique all uses fixed bed hydrogenation technique substantially.Though the operation letter of fixed bed hydrogenation technique Single, catalyst does not have to separation, but there is also obvious shortcomings, and such as each section reaction is uneven, easily forms short circuit, causes local mistake Degree hydrogenation is easy to produce working solution degradation, and catalyst utilization is low, and reaction speed is extended influence by hydrogen.

The hydrogenation technique of international major company such as Solva Interox, Evonik (Degussa), Atofina and MGC etc. are then Using ebullated bed.The catalyst that ebullated bed uses is mostly powdery, as SolvayInterox and Atofina uses powdery 2%Pd/ Al2O3-SiO2-Na2O makees catalyst；The catalyst that MGC is used then is (0.5%-2%) Pd/Al2O3.No matter also by stirring It is air-flow induced way, since these catalyst are powdery, tiny particle can spread the work in liquid relatively uniformly, effectively Ground eliminate inside diffusional resistance, fully play catalyst efficiency, thus this catalyst have it is good dispersibility, activity and Selectivity.Therefore catalyst utilization is high in entire hydrogenation process；Hydrogenation efficiency is high, H2O2 distribution coefficient when extracting in addition Greatly, extracted products concentration is high, and mass fraction is up to 40% or so；Anthraquinone less degradation.Catalysis is once put into when device starts running Dosage is few, and using adding successively, consumption volume is low, and operating cost is low.

Device production efficiency can be greatly improved using boiling bed hydrogenation technique in Hydrogen Peroxide Production, reduce catalyst and circulation Working solution dosage reduces production cost.Simultaneously as boiling bed process makes anthraquinone hydrogenation reaction uniformly, reaction process office is avoided Portion's hot spot emerges and working solution is caused to be degraded, and is conducive to improve dioxygen aquatic product quality, preferably meets the needs of different industries.

Ebullated bed mostly uses single tower, and the difficult point of operation is the filtering of catalyst, and foreign technology is substantially all using outer at present Filter type, using secondary filtration, every level-one is integrated by multiple filters, and forward filter is automatically controlled with backwash operation.

But single tower liquid level is deep, is unfavorable for being uniformly dispersed.Outer filter method complex technical process, investment are big.

4, about oxidation, extraction and laden water separation process

The oxidation process of foreign technology is carried out in a single-unit, adverse current sieve-plate tower, and hydride enters from top, compression Air enters from lower part.The air being ejected from oxidizing tower is that the tail gas containing saturated solvent is inhaled with active carbon before discharge Attached purification system is handled, and organic matter is recycled.Selecting more efficient column plate is the key that oxidation efficiency improves.

The hydrogen peroxide that oxidizing tower is formed, is all to carry out counter-current extraction acquisition with pure water in liquid-liquid sieve-plate tower both at home and abroad 's.Working solution is lower than water density, so as dispersed phase and flowing up into tower bottom, high purity water enters top, with peroxide Change hydrogen content and density is continuously increased and flows downward as continuous phase, finally obtains certain density hydrogen peroxide extract liquor.Work Make liquid (raffinate) to be flowed out by extraction tower top, direct circulation enters hydrogenation tower after water separates.Foreign technology need not use K2CO3 Drying tower and the separation of corresponding alkali match alkali, steam numerous equipment and the complex operations, control such as alkali, also without post-processing carclazyte bed, Therefore equipment largely reduces, and process greatly simplifies.

It is such as achieved with the extract liquor of higher concentration using more efficient extraction tower, the separation of grease is realized in tower, so that it may Simplify the technical process of extraction cells.Number of devices can be further reduced.

The entire production system of boiling bed process is in the operation of subacidity state, can avoid fixed-bed process because soda acid controls Unsafe accident caused by improper.

5, about the regeneration of working solution

In each plus hydrogen and oxidation cycle, certain variation occurs on physics and chemical property for anthraquinone and solvent.It must Must control hydroxyl anthrone, anthrone and epoxides quantity, with keep effective anthraquinone concentration, catalyst it is active, suitable close Degree and viscosity.Working solution is contacted with activated alumina, and epoxide therein, hydroxyl anthrone are regenerated, and anthrone forms it After be not easy to regenerate.Boiling bed process only needs the working solution of 10-20% to regenerate by carclazyte bed, and fixed-bed process then removes 100% working solution also needs 20% or so working solution to pass through hydrogenation carclazyte bed to regenerate by post-processing outside carclazyte bed.

6, foreign technology has evident characteristic and advantage

Although quickly, production technology level also increases domestic hydrogen peroxide industry development, is all in fixation in recent years Optimize on bed hydroprocessing Process ba- sis and improve, compared to the technology of domestic hydrogen dioxide solution production by anthraquinone process, foreign technology has obvious special Point and advantage, with reference to attached drawing and subordinate list 1-3.

The 6.1 maximum several companies of external hydrogen peroxide yield all form oneself unique production technology and possess matched life Device is produced, all uses boiling bed hydrogenation technique substantially, and list covering device is on a grand scale, if Solvay company 2011 is in Thailand The factory newly gone into operation, a year Hydrogen Peroxide Production scale reach 330,000 tons (with 100% densimeters), and Jilin Province, China wins wound (Germany) Corporation plan production capacity is to produce 250000 tons (with 100% densimeter) per year；China's hydrogen peroxide total productive capacity about 500 at present Ten thousand tons (with 27.5% densimeter, about 1,400,000 tons if folding 100%), fixed bed hydrogenation, and the rule of manufacturer are all used substantially Mould is not very big, 40,000 tons of maximum-norm or so (with 100% densimeter) of single set.

6.2 production efficiencys are higher.By taking certain company of subordinate list as an example, the said firm uses the working solution of high productive capacity, boiling Bed hydroprocessing and other advanced technologies, hydrogenation efficiency reaches 12g/l or more, than hydrogenation efficiency (the general 7.5- of domestic hydrogen peroxide technology It 8.5g/l) is higher by 50%, i.e., the working solution production capacity of unit volume increases by 50% in each circulation, greatly improves device production effect Rate reduces cycle working fluid dosage；Extraction tower can directly go out the hydrogen peroxide of 35-40% concentration；Process total recovery 97% at least compares Domestic manufacturer is higher by 5%.

6.3 processes are simpler, production is safer, product quality is more excellent.External Hydrogen Peroxide Production does not have K2CO3 drying tower And relevant control problem, therefore process greatly simplifies；Hydrogen peroxide is substantially eliminated because alkaline problem is decomposed in production system Security risk；Product quality is higher, and for product without the inorganic salts of acid-base neutralization, purposes is wider and favorably further produces high-purity Hydrogen peroxide, such as food-grade, electronic grade hydrogen peroxide.

6.4 is energy-saving obvious, and production cost is effectively reduced.

6.5 investments are less, and whether equipment investment, the working solution for still going into operation for the first time required and palladium catalyst are all subtracted It is few.By taking the process units of 30,000 tons/year of (100%) scales of certain company in subordinate list as an example, domestic technique, equipment and pipeline are compared Quantity is few many and much smaller, can be reduced equipment investment 20%-30%；Meanwhile the work liquid measure energy for going into operation for the first time required Reduce 30%, 2% required palladium catalyst only 600-700KG (about 2,000,000 yuan), and domestic technique usually requires 0.3% palladium catalyst 20-30 tons (about 15,000,000 yuan).

The process table of comparisons

Note: it is calculated in table for 100% content for 30,000 tons/year.

The aquatic Commercial cultivation New type high effective installation of dioxygen is reflected using ebullated bed optimization technique than existing foreign countries Technology more preferably performance.

Summary of the invention

The application purpose be to provide it is a kind of operation efficiently, consume low, energy-saving and emission-reduction, reduce side reaction, guarantee production safety The dioxygen water preparation apparatus of property.

A kind of dioxygen water preparation apparatus, including the multiple ebullated beds being sequentially connected in series, the multiple ebullated bed composition successively connects Hydrogenation tower, oxidizing tower, extraction and separation tower, the decompression packed tower connect, the hydride that hydrogenated tower obtains flow through gas-liquid after oxidizing tower Separation, working solution of the liquid after extraction and separation tower multitple extraction enter decompression packed tower, after decompression packed tower concentration At hydrogen peroxide.

1, the application is put forward for the first time in segmentation ebullated bed, and H2 reacts production hydrogen anthracene with anthraquinone under the effect of the catalyst Quinone.Bottom radial direction aeration plate and axial aeration tube are provided in every section of ebullated bed.Coil surface is microcellular structure metallic film, pipe It is tower multistage air distribution structure in disk, hydrogen, working solution and catalyst are more evenly distributed in ebullated bed.The tubular type being arranged in tower Filter and aeration tube are identical structure.DCS Staged cotrol screen pipe and aeration tube, to realize that filtering and aeration performance are cut It changes, filtering blockage can be effectively prevent.Cooling tube is axially arranged in tower, the reaction thermal energy of hydrogenation exports in time, reduces secondary anti- It answers.

Multi-segment fluidized bed series connection is conducive to the dispersion of catalyst, and the hydrogenation process of working solution is elongated, effectively prevent working solution Short circuit, hydrogenation efficiency is higher, and reduces the broken catalyst of catalyst with the outer discharge capacity of working solution, mitigates the pressure of secondary filtration.

2, it is vertical high formula membrane type tower that the application, which is put forward for the first time oxidizing tower,.Vertical membrane type is provided on oxidizing tower reaction column plate Bubble-cap, blister surface are to hate oily air ventilation membrane, and film has selective penetrated property, and gas molecule can pass through, and working solution cannot pass through, oxidation Tower has larger operating flexibility.The tower multistage air distribution structure of setting in bubble-cap.The vertical structure of bubble-cap effectively increases the table of ventilation Area strengthens gas-liquid mass transfer effect.While hydrogen oxide anthraquinone, there is heat releasing, on reaction column plate, arranges snakelike cooling The export in time of the heat of oxidation reaction is reduced side reaction by pipe.

3, the application is put forward for the first time efficient extraction and separation tower.Stirring is provided in extraction tower, stirrer paddle setting is extracting Every layer of mixing layer of tower, working solution and water mass transfer are more abundant, faster more thorough to the extraction of hydrogen peroxide；Every layer of extraction column plate setting Divide oil and divide water screen, water-oil separating is faster；Setting downspout and stalk are conducive to working solution and rise and hydrogen peroxide decline；? Top of tower setting multistage divides water filter plate to efficiently separate water in working solution, reduces the content of water in working solution；It is arranged in tower bottom more Fraction oily filter plate efficiently separates the working solution in hydrogen peroxide, guarantees the quality of hydrogen peroxide.

4, the application proposes that MVR and airless injection combine the high vacuum environment realized and run to rectifying column, using MVR And falling film evaporation technology, realize the heating and gasifying to material in tower.It is structured packing, every layer of filler upper and lower setting point in tower Liquid guide plate, making liquid distribution, more evenly gas-liquid separation is more efficient.Tower internals optimization design ensures that whole tower operation pressure drop is low.

5, DCS and SIS system is arranged in this technology controlling and process, and temperature, pressure, flow, the concentration of production process are monitored, can For combustion gas body in production process by real-time monitoring, perfect interlocking and control ensure that production security.

The advantages of the application:

1. simple process, safe operation, production elasticity are big；

2. operation is efficient, consumes low, energy-saving and emission-reduction, investment is saved；

3. being controlled using DCS and SIS, automatization level is high, process essential safety.

Detailed description of the invention

Fig. 1 is the process of preparing of the application.

Fig. 2 is the multi-segment fluidized bed structural schematic diagram of the application.

Fig. 3 is the structural schematic diagram that the application hydrogenates tower.The anthraquinone in working solution, which is hydrogenated, in this device generates hydrogen anthracene Quinone.

Fig. 4 is the structural schematic diagram of the application oxidizing tower.

Fig. 5 A is the structural schematic diagram on the application extraction and separation tower top.

Fig. 5 B is the structural schematic diagram of the application extraction and separation tower lower part.

Fig. 6 is the structural schematic diagram that the application depressurizes packed tower.

Fig. 7 is the structural schematic diagram of the application tower bottom reboiler

Specific embodiment

Below in conjunction with the attached drawing in the embodiment of the present application, clear, complete description is carried out to the technical solution of the application. Obviously, described example is only a part of example of the application, rather than whole examples.

A kind of dioxygen water preparation apparatus, including the multiple ebullated beds being sequentially connected in series, the multiple ebullated bed composition successively connects Hydrogenation tower, oxidizing tower, extraction and separation tower, the decompression packed tower connect, the hydride that hydrogenated tower obtains flow through gas-liquid after oxidizing tower Separation, working solution of the liquid after extraction and separation tower multitple extraction enter decompression packed tower, after decompression packed tower concentration At hydrogen peroxide.

The hydrogenation tower of the application includes spray thrower 1-2, and working solution enters ebullated bed from spray thrower 1-2, and catalyst passes through charging Tank 1-3, is added ebullated bed, and spiral plate 1-7 and mist eliminator 1-1 is arranged in the top of spray thrower 1-2；Hydrogen by aeration plate 1-6 to Upper aeration, by aeration tube 1-4, along tower, axially left and right is aerated hydrogen；Catalyst hydrogen, working solution Gas Stirring under in boiling State, hydrogen and anthraquinone reaction generate hydrogen anthraquinone；Hydrogen anthraquinone is dissolved in working solution to be flowed out by screen pipe 1-8；Cooling tube 1-5 It is passed through cooling water, cooling water is exchanged heat by tube wall and takes away the heat of hydrogenation production from reaction bed in time.

The oxidizing tower of the application includes spray head 2-5, and hydride enters oxidizing tower, uniform liquid separation by spray head 2-5 Vertical membrane type bubble-cap 2-6 is distributed on oxidizing tower column plate, on column plate, is provided with spiral coil cooling tube between vertical membrane type bubble-cap 2-6； Hydride on the micropore and column plate that compressed air passes through film on vertical membrane type bubble-cap 2-6 carries out gas-liquid exchange, oxygen and hydrogenation Liquid reaction generates hydrogen peroxide and anthraquinone；Reaction solution on column plate flows into downspout by overflow weir, and the reaction solution of downspout flows into Lower layer's reaction column plate connects liquid plate, and the reaction was continued on next layer of column plate；The top of oxidizing tower is provided with the first trapping according to this Device 2-1, spiral plate 2-2, the second trap 2-3, liquid baffle board 2-4, the tail gas of oxidizing tower out, by further gas-liquid separation heel row It puts.

The working solution of dissolution hydrogen peroxide is added in the lower part feed inlet 3-11 of the extraction and separation tower of the application, stirs in mixing chamber Under the action of, and from the top down by downspout 3-8 come hydrogen peroxide be sufficiently mixed, hydrogen peroxide pass through oleophylic filter plate 3- 2 further separate the working solution of hydrogen peroxide, and hydrogen peroxide flows through one section of tower reactor, and pure hydrogen peroxide is discharged from tower bottom；In mixing The small water droplet passed upward through in the 3-4 working solution of the oleophylic network of rivers of the working solution specific gravity of room is in the absorption through hydrophilic net and is polymerized to flood It drips drop, working solution in one layer of oil reservoir of hydrophilic online formation through stalk 3-6 by rising；Water is added from nozzle 3-10, passes through Downspout 3-8 enters mixing chamber, and the working solution that water and rising come under the action of stirring is mixed, and obtains mixed phase 3-5, water Hydrogen peroxide in working solution is further extracted, working solution is adsorbed and is gathered by oleophylic network of rivers 3-4 water, and working solution passes through liter Liquid pipe enters the work liquid layer of tower by the water in the further removal working solution of hydrophilic filter plate, and working solution passes through nozzle 3- 12 discharges；Fraction goes to regenerate, and most of hydrogenation tower that returns adds hydrogen；It is larger in the hydrogen peroxide specific gravity of mixing chamber, it is passing downwardly through When hydrophilic oil network 3-3, working solution droplet is poly- and floats at larger oil droplet, and dioxygen water layer A is formed in the case where dividing the network of rivers, and hydrogen peroxide passes through Downspout enters next stage extraction；Multitple extraction and separation are provided in extraction tower, concentration increases hydrogen peroxide step by step from the top down Add, forms the hydrogen peroxide of higher concentration in tower bottom；By repeatedly being extracted from bottom to top, hydrogen peroxide therein subtracts working solution step by step It is few, the hydrophilic filter plate of tower top was tied, minor amount of water is also separated, and working solution is flowed out from tower napex nozzle, and operating fluid level is by DCS Control；Pass through oleophylic filter plate in the lower part hydrogen peroxide of tower, micro oil is also separated, and hydrogen peroxide is discharged from tower bottom；In tower Fixed gas is by the gas-liquid separation of spinning liquid plate using in trap 3-1 discharge tower.

The working solution of the application in decompression packed tower tower in spray head 4-2 from spraying, by liquid separation aeroscopic plate 4-3, hydrogen peroxide It is evenly distributed and enters the regular metal packing 4-4 of corrugated plating, the moisture content in filler in hydrogen peroxide is lighter component, liquid phase hydrogen peroxide For continuous phase, gas water is discontinuous phase, and downward hydrogen peroxide concentration improves, and upward water content increases；The liquid separation arranged under filler point Gas plate declines liquid on next stage filler more evenly, and gas is upwardly into higher level's filler more evenly；Depressurize filler column overhead The spiral plate and mist eliminator of setting；The gas phase of tower top tower after steam injection extracting forms negative pressure, by the steam of injector For the hydrogen peroxide preheating to concentration.

The tower reactor hydrogen peroxide of the application enters the feed pipe 5-2 of tower bottom reboiler by pump, makes feed liquor through liquid separatnig plate 5-3 It is evenly distributed, makes film head 5-1 and diaphragm 5-7 ensures hydrogen peroxide in heat exchanger tube 5-6 inner wall homogeneous film formation again；Liquid film is heated by shell Gasify after gas heating, gas enters concentration tower air inlet pipe 4-5 by upper cover nozzle 5-10, and tower is extended down in tower in air inlet pipe Interior center is to be arranged to 45 degree of angles；The secondary steam gone out from tower bottom reboiler tower top is gone to preheat into tower object by steam injection extraction Material, the steam water interface after heat exchanger enters vapour compression machine after vapor-liquid separation out, leads to after compressor pressurizes and promotes heat content It crosses reboiler nozzle 5-4 and enters reboiler shell, compressed steam is completed the vapour-liquid after heat exchange and mixed in reboiler with hydrogen peroxide It closes object and enters compressor using vapour liquid separator；Hot water after vapor-liquid separation carries out primary preheating to feed material.

As shown in Fig. 2, a kind of dioxygen water preparation apparatus, including the multiple ebullated beds being sequentially connected in series, the multiple ebullated bed Sequentially connected hydrogenation tower, oxidizing tower, extraction and separation tower, decompression packed tower are constituted, the hydride that hydrogenated tower obtains flows through oxygen Gas-liquid separation after change tower, working solution of the liquid after extraction and separation tower multitple extraction enter decompression packed tower, fill out by decompression At hydrogen peroxide after material tower concentration.

Referring to Fig. 3, working solution enters ebullated bed A from spray thrower 1-2, and the downward spray of working solution keeps ebullated bed liquid level steady It is fixed, it reduces hydrogen and goes out entrained liquid after liquid level, spiral plate 1-7 and mist eliminator 1-1 effectively prevent entrainment of the hydrogen to working solution. Ebullated bed is added by feed pot 1-3, with working solution in catalyst.Hydrogen is aerated upwards by aeration plate 1-6, and hydrogen passes through aeration tube Along tower, axially left and right is aerated 1-4.Catalyst is in fluidized state, hydrogen and anthraquinone reaction life under the Gas Stirring of working solution in hydrogen At hydrogen anthraquinone.When hydrogen anthraquinone is dissolved in working solution through screen pipe 1-8, catalyst, which is filtered, to be stayed in ebullated bed, and work liquid hydrogen Anthraquinone enters B sections of ebullated beds.Cooling tube 1-5 is passed through cooling water, cooling water by tube wall heat exchange will hydrogenation production heat in time from It is taken away in reaction bed.The function of aeration tube and filter is switched by DCS points of journey, and hydrogen is under the purging effective guarantee of filter one The filter efficiency in period.As shown in Fig. 2, tri- sections of ebullated bed series connection of A, B, C.The liquid level of every section of ebullated bed, temperature, pressure are by DCS Control.Working solution sequentially enters B, C from bed A, and hydrogen sequentially enters B, A from bed C.Hydrogen passes through further by gas-liquid after A It is segregated into hydrogen recycle compressor.After working solution after hydrogenation flows out C, by secondary filtration, into oxidizing tower.Second level mistake Filter enters ebullated bed by catalyst feed pot by the program-controlled backwash of DCS, backwash liquor.

Referring to shown in Fig. 4, hydride enters oxidizing tower by spray head 2-5, and uniform liquid separation is on oxidizing tower column plate, tower Vertical membrane type bubble-cap is distributed on plate, is provided with spiral coil cooling tube between bubble-cap.The micropore and tower that compressed air passes through film on bubble-cap Hydride on plate carries out gas-liquid exchange, and oxygen and hydride reaction generate hydrogen peroxide and anthraquinone.Cooling in spiral coil cooling tube Water takes away reaction heat.Reaction solution on column plate flows into downspout by overflow weir, and the reaction solution of downspout flows into lower layer's reaction Column plate connects liquid plate, and the reaction was continued on next layer of column plate.No entrainment of the gas of reaction to reaction solution in order to prevent, tower Top is provided with the first trap 2-1, spiral plate 2-2, the second trap 2-3, liquid baffle board 2-4.The tail gas of oxidizing tower out passes through It is discharged after further gas-liquid separation.The reaction solution being discharged from oxidation tower reactor enters extraction tower and is separated.

Referring to shown in Fig. 5 A, Fig. 5 B, the working solution for dissolving hydrogen peroxide is added from extraction and separation tower lower part feed inlet 3-11, It is sufficiently mixed under the action of mixing chamber stirring, and from the top down by the hydrogen peroxide that downspout 3-8 comes, hydrogen peroxide is by close The filter plate 3-2 of oil further separates the working solution of hydrogen peroxide, and hydrogen peroxide retains standing by one section in tower reactor, and pure is double Oxygen water is discharged from tower bottom；Oleophylic net 3-4 is passed upward through the working solution specific gravity of mixing chamber is small, and working solution droplet is poly- and at larger oil droplet It floats up, in order to accelerate the floating of working oil, is provided with stalk 3-6；In oleophylic web tier due to the effect shape of oleophylic net At one layer of oil reservoir.Water is added from nozzle 3-10, enters mixing chamber by downspout 3-8, and water and rising come under the action of stirring Working solution mixed, obtain mixed phase 3-5, water further extracts the hydrogen peroxide in working solution, and working solution passes through oleophylic It nets 3-4 to float, enters the work liquid layer of tower by the water in the further removal working solution of hydrophilic filter plate by stalk, Working solution is discharged by nozzle 3-12；Fraction goes to regenerate, and most of hydrogenation tower that returns adds hydrogen；In the hydrogen peroxide specific gravity of mixing chamber Larger, when passing downwardly through hydrophilic net 3-3, hydrogen peroxide droplet is poly- and at big water droplet, and dioxygen water layer A is formed in the case where dividing the network of rivers；? Multitple extraction and separation are provided in extraction tower, concentration increases hydrogen peroxide step by step from the top down, forms higher concentration in tower bottom Hydrogen peroxide；Working solution tied the hydrophilic mistake of tower top by being reduced step by step by the repeatedly extraction hydrogen peroxide therein of water from bottom to top Filter plate, minor amount of water are also separated, and working solution is flowed out from tower napex nozzle, and operating fluid level is controlled by DCS；Fixed gas warp in tower It crosses in extraction and separation tower trap 3-1 discharge tower.

As shown in fig. 6, the needs in order to be suitble to higher concentration dioxygen aquatic products device, the hydrogen peroxide come out from extraction tower is by subtracting Packed tower is pressed to carry out rectifying.Hydrogen peroxide in tower in spray head 4-2 from spraying, and by liquid separation aeroscopic plate 4-3, hydrogen peroxide is evenly distributed Into the regular metal packing 4-4 of corrugated plating, the moisture content in filler in hydrogen peroxide is lighter component, and liquid phase hydrogen peroxide is continuous phase, Gas water is discontinuous phase, and upward hydrogen peroxide concentration improves, and upward water content increases.The liquid separation air dividing plate 4-3 arranged under filler, makes On next stage filler more evenly, gas is upwardly into higher level's filler more evenly for liquid decline.In order to be arranged in concentrated effect tower Multistage filler.The spiral plate 4-1 and mist eliminator 4-7 of tower top setting, to prevent the entrainment of gas-liquid.Liquid after rectifying is from row Liquid mouth 4-6 discharge, the gas phase of tower top tower after steam injection extracting form negative pressure, are used for by the steam of injector to concentration Hydrogen peroxide preheating.

As shown in fig. 7, tower reactor hydrogen peroxide enters tower bottom reboiler feed pipe 5-2 by pump, make feed liquor through liquid separatnig plate 5-3 It is evenly distributed, makes film head 5-1 and diaphragm 5-7 ensures hydrogen peroxide in heat exchanger tube 5-6 inner wall homogeneous film formation again.Liquid film is heated by shell Gasify after gas heating, gas enters concentration tower air inlet pipe 4-5 by upper cover nozzle 5-10, is extended down in tower in air inlet pipe Center is to be arranged to 45 degree of angles in tower, to prevent influence of the dropping liq to gas.Because rectifying column negative pressure is run, reboiler gasification Temperature is lower, and the secondary steam gone out from tower top is sprayed by steam to be extracted out, goes to preheat into tower material, out the steam-water mixing after heat exchanger Object enters vapour compression machine after vapor-liquid separation, pressurizes to enter by reboiler nozzle 5-4 after promoting heat content to compressor and boil again Device shell, liquid-vapor mixture of the compressed steam in reboiler and after hydrogen peroxide completion heat exchange enter using vapour liquid separator Compressor.Hot water after vapor-liquid separation carries out primary preheating to feed material.The hydrogen peroxide of preparation is flowed out from liquid outlet 5-9.

The preferable specific embodiment of the above, only the application, but the protection scope of the application is not limited thereto, Which describe more core equipments multiple application innovative points.Other production processes and any it is familiar with the art Technical staff within the technical scope of the present application, according to the technical solution of the application and its application design equally replaced It changes or changes, should all cover within the scope of protection of this application.

Claims (6)

1. a kind of dioxygen water preparation apparatus, it is characterised in that including the multiple ebullated beds being sequentially connected in series, the multiple ebullated bed structure At sequentially connected hydrogenation tower, oxidizing tower, extraction and separation tower, decompression packed tower, the hydride that hydrogenated tower obtains flows through oxidation Gas-liquid separation after tower, working solution of the liquid after extraction and separation tower multitple extraction enter decompression packed tower, by depressurizing filler At hydrogen peroxide after tower concentration.

2. dioxygen water preparation apparatus according to claim 1, it is characterised in that above-mentioned hydrogenation tower includes spray thrower (1-2), Working solution enters ebullated bed from spray thrower (1-2), and ebullated bed is added by feed pot (1-3) in catalyst, spray thrower (1-2) it is upper Side's setting spiral plate (1-7) and mist eliminator (1-1)；Hydrogen is aerated upwards by aeration plate (1-6), and hydrogen passes through aeration tube (1- 4) along tower, axially left and right is aerated；Catalyst hydrogen, working solution Gas Stirring under be in fluidized state, hydrogen and anthraquinone reaction generate Hydrogen anthraquinone；Hydrogen anthraquinone is dissolved in working solution to be flowed out by screen pipe (1-8)；Cooling tube (1-5) is passed through cooling water, and cooling water is logical Tube wall heat exchange is crossed to take away the heat of hydrogenation production from reaction bed in time.

3. dioxygen water preparation apparatus according to claim 1, it is characterised in that above-mentioned oxidizing tower includes spray head (2-5), Hydride enters oxidizing tower by spray head (2-5), and vertical membrane type is distributed in uniform liquid separation on oxidizing tower column plate, on column plate Bubble-cap (2-6) is provided with spiral coil cooling tube between vertical membrane type bubble-cap (2-6)；Compressed air passes through on vertical membrane type bubble-cap (2-6) Hydride on the micropore and column plate of film carries out gas-liquid exchange, and oxygen and hydride reaction generate hydrogen peroxide and anthraquinone；On column plate Reaction solution downspout is flowed by overflow weir, what the reaction solution of downspout flowed into lower layer's reaction column plate connects liquid plate, and next The reaction was continued on layer column plate；The top of oxidizing tower is provided with the first trap (2-1), spiral plate (2-2), the second trap according to this (2-3), liquid baffle board (2-4), the tail gas of oxidizing tower, is discharged after further gas-liquid separation out.

4. dioxygen water preparation apparatus according to claim 1, it is characterised in that the lower part feed inlet of above-mentioned extraction and separation tower The working solution of dissolution hydrogen peroxide is added in (3-11), under the action of mixing chamber stirring, and passes through downspout (3-8) from the top down The hydrogen peroxide come is sufficiently mixed, and hydrogen peroxide further separates the working solution of hydrogen peroxide by the filter plate (3-2) of oleophylic, dioxygen Water flows through one section of tower reactor, and pure hydrogen peroxide is discharged from tower bottom；The oleophylic network of rivers is passed upward through the working solution specific gravity of mixing chamber is small Water droplet in (3-4) working solution is in the absorption through hydrophilic net and is polymerized to flood and drips drop, and working solution passes through in hydrophilic online shape Rise at one layer of oil reservoir through stalk (3-6)；Water is added from nozzle (3-10), enters mixing chamber by downspout (3-8), is stirring Water and rise the working solution come under the action of mixing and mixed, obtains mixed phase (3-5), water is by the hydrogen peroxide in working solution into one Step extraction, working solution is adsorbed and gathers by the oleophylic network of rivers (3-4) water, working solution by stalk pass through hydrophilic filter plate into Water in one step removal working solution enters the work liquid layer of tower, and working solution is discharged by nozzle (3-12)；Fraction goes to regenerate, Most of hydrogenation tower that returns adds hydrogen；It is larger in the hydrogen peroxide specific gravity of mixing chamber, when passing downwardly through hydrophilic oil network (3-3), work Liquid droplet is poly- and floats at larger oil droplet, forms dioxygen water layer (A) in the case where dividing the network of rivers, and hydrogen peroxide enters next stage extraction by downspout It takes；Multitple extraction and separation are provided in extraction tower, concentration increases hydrogen peroxide step by step from the top down, is formed in tower bottom more highly concentrated The hydrogen peroxide of degree；By repeatedly being extracted from bottom to top, hydrogen peroxide therein is reduced working solution step by step, ties the hydrophilic mistake of tower top Filter plate, minor amount of water are also separated, and working solution is flowed out from tower napex nozzle, and operating fluid level is controlled by DCS；In the lower part dioxygen of tower Water passes through oleophylic filter plate, and micro oil is also separated, and hydrogen peroxide is discharged from tower bottom；Fixed gas in tower passes through spinning liquid plate gas-liquid Separation is using in trap (3-1) discharge tower.

5. dioxygen water preparation apparatus according to claim 1, it is characterised in that working solution spray head out of decompression packed tower tower Sprinkling in (4-2), by liquid separation aeroscopic plate (4-3), hydrogen peroxide is evenly distributed into the regular metal packing of corrugated plating (4-4), Moisture content in filler in hydrogen peroxide is lighter component, and liquid phase hydrogen peroxide is continuous phase, and gas water is discontinuous phase, and downward hydrogen peroxide is dense Degree improves, and upward water content increases；The liquid separation air dividing plate arranged under filler declines liquid on next stage filler more evenly, Gas is upwardly into higher level's filler more evenly；Depressurize the spiral plate and mist eliminator of the setting of filler column overhead；The gas phase of tower top is passed through Tower forms negative pressure after steam injection extracting, is used to preheat to the hydrogen peroxide of concentration by the steam of injector.

6. dioxygen water preparation apparatus according to claim 1, it is characterised in that tower reactor hydrogen peroxide enters tower bottom again by pump The feed pipe (5-2) for boiling device, makes feed liquor be evenly distributed through liquid separatnig plate (5-3), makes film head (5-1) and again diaphragm (5-7) guarantee pair Oxygen water is in heat exchanger tube (5-6) inner wall homogeneous film formation；Liquid film gasifies after by shell heated gas heats, and gas passes through upper cover nozzle (5-10) enters concentration tower air inlet pipe (4-5), and it is to be arranged to 45 degree of angles that center in tower is extended down in tower in air inlet pipe；Again from tower bottom The secondary steam that boiling device tower top goes out is gone to preheat into tower material by steam injection extraction, and the steam water interface after heat exchanger is through vapour-liquid out Enter vapour compression machine after separation, reboiler shell is entered by reboiler nozzle (5-4) to after compressor pressurizes and promotes heat content Layer, liquid-vapor mixture of the compressed steam in reboiler and after hydrogen peroxide completion heat exchange enter compression using vapour liquid separator Machine；Hot water after vapor-liquid separation carries out primary preheating to feed material.