CN210885309U - Hydrogenation tower double-tower system in anthraquinone method fixed bed hydrogen peroxide production process - Google Patents
Hydrogenation tower double-tower system in anthraquinone method fixed bed hydrogen peroxide production process Download PDFInfo
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- CN210885309U CN210885309U CN201921905718.XU CN201921905718U CN210885309U CN 210885309 U CN210885309 U CN 210885309U CN 201921905718 U CN201921905718 U CN 201921905718U CN 210885309 U CN210885309 U CN 210885309U
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Abstract
A hydrogenation tower double-tower system in a process for producing hydrogen peroxide by an anthraquinone method fixed bed relates to the technical field of industrially producing hydrogen peroxide by the anthraquinone method fixed bed, and comprises a hydrogen main pipe, a working liquid main pipe, a clay bed, a filter, a first hydrogenation tower and a second hydrogenation tower, wherein hydrogen inlets of the first hydrogenation tower and the second hydrogenation tower are connected in parallel and then connected with the hydrogen main pipe; working liquid inlets of the first hydrogenation tower and the second hydrogenation tower are connected in parallel and then are connected with a working liquid main pipe; the first hydrogenation tower and the hydrogenation liquid outlet of the second hydrogenation tower are connected in parallel and then connected with a filter, and the hydrogenation liquid outlet of the first hydrogenation tower is connected with the working liquid inlet of the second hydrogenation tower through a hydrogenation tower delivery pump; a circulating regeneration hydrogenation liquid outlet of the first hydrogenation tower is connected with a working liquid inlet through a first circulating pump, and a circulating regeneration hydrogenation liquid outlet of the second hydrogenation tower is connected with the working liquid inlet through a second circulating pump; the first circulating pump is connected with the second circulating pump in parallel and then is connected with the carclazyte bed. Not only can save investment cost, but also can ensure the requirement of green production.
Description
Technical Field
The utility model relates to a technical field with the hydrogen peroxide solution of anthraquinone process fixed bed industrial production, concretely relates to anthraquinone hydrogenation and with the hydrogenation liquid after the hydrogenation regeneration 2-ethyl anthraquinone (2-ethyl anthraquinone and 2-ethyl tetrahydro anthraquinone) technique of regeneration to the epoxy degradation thing through the effect of hydrogenation carclazyte bed active alumina.
Background
Industrial scale production of hydrogen peroxide (H)2O2) The traditional method is a fixed bed hydrogen peroxide production process by an anthraquinone method, and mainly comprises a hydrogenation process, an oxidation process, an extraction and purification process and a regeneration process.
The hydrogenation reaction mechanism is: under the catalytic action of palladium (Pd), 2-ethyl anthraquinone and 2-ethyl tetrahydroanthraquinone react with hydrogen respectively to generate 2-ethyl hydroanthraquinone and 2-ethyl tetrahydroanthraquinone.
The traditional hydrogenation process is: the working fluid from the regenerated liquid pump passes through the working fluid heat exchanger and the working fluid preheater after solid impurities possibly carried by the working fluid are filtered by the two-stage working fluid filter, and is preheated to the required temperature, and then enters the top of the hydrogenation tower together with the hydrogen purified by the hydrogen filter and the water separated by the hydrogen buffer tank. The whole hydrogenation tower consists of three sections of catalyst beds, and the top of each section of the tower is provided with a liquid distributor and a gas-liquid distributor so as to ensure that gas and liquid entering the tower are uniformly distributed. Depending on the process requirements, any one (single) or two (series) of the three catalyst beds can be used for hydrogenation, and if necessary, three (series) beds can be used simultaneously, which depends mainly on the requirements of hydrogenation efficiency and production capacity and catalyst activity. For example, when the upper section and the middle section are used, the working liquid and the hydrogen firstly enter the top of the upper section tower, flow downwards through the catalyst layer in the tower, flow out from the bottom of the upper section tower, enter the top of the middle section tower through the communicating pipe outside the tower, flow out from the bottom of the middle section tower and enter the hydrogenation liquid-gas separator.
The hydrogenation liquid and unreacted hydrogen (called hydrogenation tail gas) from the hydrogenation tower enter a hydrogenation liquid-gas separator for gas-liquid separation, the tail gas is discharged from the top of the separator, and enters a condensate metering tank after being condensed by a hydrogenation tail gas condenser, and the solvent is remained in the condensate metering tank. The tail gas is directly discharged after the flow rate of the tail gas is controlled by a tail gas flowmeter, the hydrogenated liquid in a hydrogenated liquid gas-liquid separator is separated by 10 percent by virtue of the pressure in a hydrogenation tower after a certain liquid level is controlled by an automatic control instrument, the hydrogenated liquid flows through a hydrogenated liquid white soil bed, then passes through a hydrogenated liquid filter together with the rest 90 percent, then passes through a hydrogenated liquid security filter to filter a small amount of catalyst powder and alumina powder possibly carried in the hydrogenated liquid, and then passes through a working liquid heat exchanger to transfer the heat of the working liquid to the working liquid from a regenerated liquid pump, and then enters a hydrogenated liquid storage tank. In this case, a small amount of hydrogen dissolved in the hydrogenation liquid is desorbed and is discharged via a blow-down condenser, a hydrogenation liquid seal and a flame arrester.
Part of the hydrogenated liquid in the hydrogenated liquid gas-liquid separator is returned to the hydrogenation tower from a regenerated liquid inlet pipeline by a circulating hydrogenated liquid pump, the spray density in the tower is increased so as to ensure that the temperature in the tower is uniform, the hydrogenation efficiency is stable, oxygen in the hydrogenation tower is consumed, and the operation is safe.
In the traditional hydrogenation process, each section of the bed layer of the hydrogenation tower is generally one layer or two layers, working liquid firstly enters a liquid distributor at the top of the section of the hydrogenation tower, and then is distributed downwards by a gas-liquid distribution disc with hydrogen from the outside, and then the working liquid is sprayed downwards to a catalyst layer to carry out hydrogenation reaction with the hydrogen discharged from a gas-liquid distribution disc downcomer; if the catalyst layer is two layers, a gas-liquid redistribution disc is needed to be added in the middle, and the hydrogenated liquid which initially participates in the reaction and hydrogen react in the catalyst on the lower layer.
It can be seen that the following disadvantages exist in a single hydrogenation column in a conventional hydrogenation process:
1. in the traditional process, a single hydrogenation tower needs to be large in volume and large in catalyst loading amount; taking 10 ten thousand tons of 27.5 percent hydrogen peroxide produced annually as an example, the diameter of a hydrogenation tower in the traditional process is 3.5 meters, the height is about 35 meters, the total volume is 220 cubic meters (no gas-liquid separator is included), the loading amount of the catalyst is also large, and two sections are generally filled with 30-36 tons (15-18 tons per section).
2. In the traditional process, the hydrogenation tower can only select the mode of operating an open single tower or operating an upper tower and a lower tower in series: the general catalyst filling mode of the tower is a bulk type, and the working fluid is easy to generate phenomena such as bias flow, channeling and the like when the bulk type catalyst participates in hydrogenation reaction. The degradation of anthraquinone is serious, the consumption of anthraquinone is high, and the consumption of 27.5 percent of hydrogen peroxide anthraquinone per ton is about 0.5 kg. The hydrogen efficiency control of the single-tower operation is generally controlled to be about 6.0-7.5g/l, the two towers can only be operated in series generally, and the control is difficult when the two towers are operated in series; when hydrogen is added from the upper tower, the upper tower consumes more hydrogen for reaction, and the lower section of tower has less light weight and serious bias flow; when hydrogen enters two sections of towers simultaneously, the lower section of tower has large resistance and unsmooth lower liquid of the upper section of tower; the two phenomena are poor in hydrogen efficiency control, severe in degradation, and easy to generate catalyst agglomeration at the bottom of the catalyst layer of the lower tower, so that bias flow is more severe, the catalyst needs to be regenerated in time, and the time from the beginning of use to the regeneration of the catalyst in the conventional process is 3-6 months.
3. In the traditional process, the outlet pressure of a regenerative liquid pump, a hydrogenation liquid circulating pump and a hydrogenation tower is higher, and the height of the hydrogenation tower is about 35 meters, so that the regenerative liquid pump and the hydrogenation liquid circulating pump need to overcome the height of the hydrogenation tower, the power of the pump is higher, and electric energy is wasted.
In a word, the traditional single-tower three-section production process of the hydrogenation process cannot meet the requirement of green production and is not beneficial to saving production.
Disclosure of Invention
The utility model aims at overcoming the defect that the three sections of the single tower are connected in parallel in the traditional process, and providing the hydrogenation tower double-tower system in the process of producing hydrogen peroxide by the anthraquinone method fixed bed, which can save the investment cost and ensure the requirement of green production.
The purpose of the utility model is realized like this: the double-tower system of the hydrogenation tower in the technology for producing hydrogen peroxide by the anthraquinone method fixed bed comprises a hydrogen main pipe, a working liquid main pipe, a clay bed, a filter, a hydrogenation liquid cooler and a hydrogenation liquid storage tank, wherein the filter, the hydrogenation liquid cooler and the hydrogenation liquid storage tank are sequentially connected in series; the hydrogen inlet of the first hydrogenation tower is connected with the hydrogen inlet of the second hydrogenation tower in parallel and then is connected with the hydrogen main pipe; the working fluid inlet of the first hydrogenation tower is connected with the working fluid inlet of the second hydrogenation tower in parallel and then is connected with the working fluid main pipe; a hydrogenated liquid outlet of the first hydrogenation tower is connected with a hydrogenated liquid outlet of the second hydrogenation tower in parallel and then connected with a filter, the hydrogenated liquid outlet of the first hydrogenation tower is also connected with a hydrogenation tower delivery pump, and a liquid outlet of the hydrogenation tower delivery pump is connected with a working liquid inlet of the second hydrogenation tower; the outlet of the hydrogenation tail gas of the first hydrogenation tower and the outlet of the hydrogenation tail gas of the second hydrogenation tower are both connected with respective hydrogenation tail gas condensers, and the outlet of each hydrogenation tail gas condenser is connected with a respective hydrogenation tail gas condensate receiving tank; a circulating regeneration hydrogenation liquid outlet of the first hydrogenation tower is connected with a working liquid inlet of the first hydrogenation tower through a first circulating pump, and a circulating regeneration hydrogenation liquid outlet of the second hydrogenation tower is connected with a working liquid inlet of the second hydrogenation tower through a second circulating pump; the liquid outlet of the first circulating pump is connected with the liquid outlet of the second circulating pump in parallel and then is connected with the liquid inlet of the clay bed, and the liquid outlet of the clay bed is connected with the liquid inlet of the filter.
The utility model discloses there are two hydrogenation towers, all are furnished with the control valve on every way pipeline, and every tower can the exclusive use, can establish ties or parallelly connected use according to the actual demand of production between two towers. When the hydrogenation tower is used during the original start-up, a single hydrogenation tower can be used independently due to better catalytic activity, generally, a first hydrogenation tower (main tower) is used firstly, and when the catalytic activity of the first hydrogenation tower is poor, the first hydrogenation tower needs to be cut out for regeneration, and a second hydrogenation tower can be used independently; when the catalytic activity of the two towers is poor, the operation of tower combination (closing a transfer pump of the hydrogenation tower) or tower combination (opening the transfer pump of the hydrogenation tower) can be carried out according to actual needs, the tower combination operation is carried out when the catalytic resistance is large, and the tower combination operation is required when high hydrogen efficiency is required; when two hydrogenation towers are operated in series, a hydrogenation tower transfer pump is arranged in the middle for pressurizing and sending the hydrogenation liquid of the first hydrogenation tower to the second hydrogenation tower; in addition to the above operations, the series-parallel operation can be simultaneously carried out according to the requirements, part of the materials fed into the first hydrogenation tower is properly reduced and is directly sent into the second hydrogenation tower, and the hydrogenated materials of the first hydrogenation tower and part of the unhydrogenated materials are mixed and enter the second hydrogenation tower for hydrogenation reaction; no matter which tower is started, a hydrogenation liquid circulating pump needs to be started to ensure proper spraying density.
The hydrogenation tail gas separated from the hydrogenation tower contains a certain amount of heavy aromatic solvent and needs to be recycled, the separated hydrogenation tail gas is condensed by a hydrogenation tail gas condenser and then enters a condensate receiving tank to recycle part of the heavy aromatic solvent, and the tail gas is decompressed by a decompression valve and then is discharged at high altitude or recycled; each hydrogenation tower is provided with an independent tail gas system, so that the safety problem caused by gas cross and gas cross is prevented.
The hydrogenation regeneration pipeline is characterized in that 20-30% of flow is separated from an outlet of the circulation regeneration hydrogenation liquid and flows into a filter of the hydrogenation liquid together with a main material pipeline (a pipeline of the outlet of the hydrogenation liquid); the purpose of regenerating the pipeline is to regenerate epoxy degradation products generated by oxidation reaction, and the purpose of heating the hydrogenated liquid to 65-75 ℃ is to ensure that the regeneration capacity of the active alumina is stronger at the temperature.
The utility model discloses a liquid outlet of first circulating pump is connected with heat exchanger's plate heat exchanger cold side import after parallelly connected with the liquid outlet of second circulating pump, and heat exchanger's plate heat exchanger cold side exit linkage heater, the inlet of clay bed is connected to the working solution liquid outlet of heater, the liquid outlet of clay bed with heat exchanger's hot side inlet is connected, heat exchanger's hot side liquid outlet with the inlet of filter is connected. The working fluid heat exchanger is used for the purpose of recovering part of the heat.
The first hydrogenation tower and the second hydrogenation tower of the utility model both comprise a catalyst section tower body, three layers of catalyst frame components are arranged in the catalyst section tower body along the height direction, a gas-liquid distributor is arranged above each layer of catalyst frame components, the gas-liquid distributors are fixed with the catalyst section tower body, and a hydrogen inlet and a working liquid inlet are arranged at the top of the catalyst section tower body; each layer of catalyst frame component has the same structure and comprises a support grid plate, a lower packing layer, a plurality of vertical pipes and an upper packing layer which are sequentially arranged from bottom to top, wherein the support grid plate is connected with the inner wall of the catalyst section tower body, and the plurality of vertical pipes are arranged in a honeycomb shape and are fixed with each other. The palladium catalyst is arranged in the honeycomb vertical pipe, the honeycomb vertical pipe divides the inner cavity of the catalyst section tower body into a plurality of small channels to form a bias flow prevention combined internal part, and the phenomena of bias flow, channeling, wall flow and the like in the hydrogenation process of the catalyst layer of the working solution are prevented. Compared with the traditional process, the hydrogenation reaction is more stable and uniform, and the side reaction of local degradation is greatly reduced; the consumption of anthraquinone in the system is greatly reduced, and the consumption of anthraquinone is only 60 percent of that of the traditional process. Compared with the traditional hydrogenation equipment, the catalyst has higher utilization rate and less catalyst usage amount. The catalyst is only 50% of the traditional process.
The utility model discloses a gas-liquid distributor sprays board and a plurality of downcomer including supporting otter board, working solution, the interior wall connection of supporting otter board and catalyst section tower body, the working solution sprays the board and connects in the below of supporting the otter board, the equal vertical arrangement of every downcomer, the upper portion and the supporting otter board fixed connection of every downcomer stretch out supporting otter board, all connect the block in the upper end of every downcomer, be equipped with the clearance and cover in the top of downcomer between the last mouthful of every block of board and corresponding downcomer, the lower extreme of every downcomer all sprays board fixed connection and stretches out the working solution with the working solution and. When gas and liquid are distributed, the working liquid flows to the working liquid spraying plate from the supporting screen plate and sprays downwards, and hydrogen enters the downcomer from the gap between the cover cap and the downcomer and is discharged downwards from the lower opening. The working solution flows downward uniformly, and the hydrogen also flows downward uniformly, and the reaction is carried out under the action of the palladium catalyst.
The utility model discloses the gas-liquid separation section tower body is connected to the lower extreme of catalyst section tower body, and the hydrogenated tail gas export sets up on the upper portion of gas-liquid separation section tower body, and the hydrogenated liquid export sets up in the lower part of gas-liquid separation section tower body, and the export of circulation regeneration hydrogenated liquid sets up the bottom of gas-liquid separation section tower body.
The utility model discloses the top of the tower internal connection working solution diffuser plate of catalyst section tower body, the working solution diffuser plate is located the working solution and enters the mouth under, and the diameter of working solution diffuser plate is greater than the diameter that the working solution entered the mouth. The working solution is uniformly distributed above the porous plate to form a liquid seal layer after being diffused, and then flows downwards through the small holes of the working solution diffusion plate.
The hydrogen inlet of the first hydrogenation tower and the hydrogen inlet of the second hydrogenation tower of the utility model are respectively connected with the first control valve, and the two first control valves are connected in parallel and then connected with the outlet of the hydrogen main pipe; the working fluid inlet of the first hydrogenation tower and the working fluid inlet of the second hydrogenation tower are respectively connected with a second control valve, and the two second control valves are connected in parallel and then connected with the outlet of the working fluid main pipe; the hydrogenated liquid outlet of the first hydrogenation tower and the hydrogenated liquid outlet of the second hydrogenation tower are respectively connected with third control valves, and the two third control valves are connected with the filter in parallel; a liquid outlet of the hydrogenation tower conveying pump is connected with a fourth control valve, and a liquid outlet of the fourth control valve is connected with a working liquid inlet of the second hydrogenation tower; and a liquid outlet of the fifth control valve is connected with a liquid outlet of the sixth control valve in parallel and then is connected with a cold side inlet of the plate heat exchanger of the heat exchanger.
Drawings
Fig. 1 is a flow chart of the present invention.
FIG. 2 is a schematic structural diagram of a first hydrogenation column.
Fig. 3 is an enlarged view of a portion a of fig. 2.
Fig. 4 is a view from B-B in fig. 3.
Fig. 5 is an enlarged view of the gas-liquid distributor of fig. 2.
Fig. 6 is an enlarged view of the portion C in fig. 5.
Detailed Description
As shown in fig. 1, a hydrogenation tower double-tower system in a fixed bed hydrogen peroxide production process by an anthraquinone process includes a first hydrogenation tower 14 and a second hydrogenation tower 15 which have the same structure, and the first hydrogenation tower 14 and the second hydrogenation tower 15 are respectively provided with a hydrogen inlet 1, a working solution inlet 2, a hydrogenation solution outlet 9, a hydrogenation tail gas outlet 12 and a circularly regenerated hydrogenation solution outlet 10. The double column system also includes a hydrogen manifold 16, a working fluid manifold 13.
The hydrogen inlet 1 of the first hydrogenation tower 14 and the hydrogen inlet 1 of the second hydrogenation tower 15 are respectively connected with a first control valve 29, and the two first control valves 29 are connected with the outlet of the hydrogen main pipe 16 after being connected in parallel. The working fluid inlet 2 of the first hydrogenation tower 14 and the working fluid inlet 2 of the second hydrogenation tower 15 are respectively connected with a second control valve 30, the two second control valves 30 are connected in parallel and then connected with the outlet of the working fluid main pipe 13, and the inlet of the working fluid main pipe 13 is connected with a temperature regulator 17. The hydrogenated liquid outlet 9 of the first hydrogenation tower 14 and the hydrogenated liquid outlet 9 of the second hydrogenation tower 15 are respectively connected with third control valves 31, the two third control valves 31 are connected with a filter 18 after being connected in parallel, and the filter 18, the hydrogenated liquid cooler 19 and the hydrogenated liquid storage tank 20 are sequentially connected in series. The hydrogenated liquid outlet 9 of the first hydrogenation tower 14 is also connected with a hydrogenation tower transfer pump 25, the liquid outlet of the hydrogenation tower transfer pump 25 is connected with a fourth control valve 32, and the liquid outlet of the fourth control valve 32 is connected with the working liquid inlet 2 of the second hydrogenation tower 15. Hydrogenation tail gas outlet 12 of first hydrogenation tower 14 and hydrogenation tail gas outlet 12 of second hydrogenation tower 15 all connect hydrogenation tail gas condenser 26, and the export of every hydrogenation tail gas condenser 26 all is connected hydrogenation tail gas condensate and is received groove 27, and two hydrogenation tail gas condensates receive groove 27 and connect in parallel the back and carry to oil removal recovery pond. The outlet 10 of the first hydrogenation tower 14 is connected with the working fluid inlet 2 of the first hydrogenation tower 14 through a first circulating pump 24, and the outlet 10 of the second hydrogenation tower 15 is connected with the working fluid inlet 2 of the second hydrogenation tower 15 through a second circulating pump 28. A liquid inlet of the fifth control valve 33 is connected with a liquid outlet of the first circulating pump 24, a liquid inlet of the sixth control valve 34 is connected with a liquid outlet of the second circulating pump 28, a liquid outlet of the fifth control valve 33 is connected with a liquid outlet of the sixth control valve 34 in parallel and then connected with a cold side inlet of the plate heat exchanger of the heat exchanger 21, a cold side outlet of the plate heat exchanger of the heat exchanger 21 is connected with the heater 22, a working liquid outlet of the heater 22 is connected with a liquid inlet of the clay bed 23, a liquid outlet of the clay bed 23 is connected with a hot side liquid inlet of the heat exchanger 21, and a hot side liquid outlet of the heat exchanger.
As shown in fig. 2 to 6, each of the first hydrogenation tower 14 and the second hydrogenation tower 15 includes a gas-liquid separation section tower 8 at a lower section of the catalyst section tower 5 at an upper section, a hydrogen inlet 1 and a working fluid inlet 2 are provided at a top of the catalyst section tower 5, a hydrogenated tail gas outlet 12 is provided at an upper portion of the gas-liquid separation section tower 8, a hydrogenated liquid outlet 9 is provided at a lower portion of the gas-liquid separation section tower 8, a recycled and regenerated hydrogenated liquid outlet 10 is provided at a bottom of the gas-liquid separation section tower 8, and a pure water vapor inlet 11 for catalyst regeneration is further provided at the gas-liquid separation section tower 8.
Connect working solution diffuser plate 6 through the support in the top of the tower of catalyst section tower body 5, set up a plurality of aperture on working solution diffuser plate 6, working solution diffuser plate 6 is located working solution and enters 2 under, and working solution diffuser plate 6's diameter is greater than the diameter that working solution entered 2.
Three layers of catalyst frame components 4 are arranged in the catalyst section tower body 5 along the height direction, and a gas-liquid distributor 3 is arranged above each layer of catalyst frame component 4. Each layer of catalyst frame component 4 has the same structure and comprises a catalyst mounting seat 4-1, a support grid plate 4-2, a lower packing layer 4-3, a plurality of vertical pipes 4-4 and an upper packing layer 4-5 which are sequentially arranged from bottom to top, wherein the catalyst mounting seat 4-1 is fixedly connected with the inner wall of a catalyst section tower body 5, the support grid plate 4-2 is arranged above the catalyst mounting seat 4-1, the plurality of vertical pipes 4-4 are arranged in a honeycomb shape and are fixed with each other, and a palladium catalyst is arranged in the vertical pipes 4-4.
The gas-liquid distributor 3 comprises a distributor mounting seat 3-1, a supporting screen plate 3-2, a working liquid spraying plate 3-5 and a plurality of downcast pipes 3-3, the distributor mounting seat 3-1 is fixedly connected with the inner wall of the catalyst section tower body 5, the supporting screen plate 3-2 is arranged above the distributor mounting seat 3-1 and is connected with the distributor mounting seat 3-6 through bolts, and a sealing ring 3-7 is arranged between the supporting screen plate 3-2 and the distributor mounting seat 3-1. The working liquid spraying plate 3-5 is connected below the supporting screen plate 3-2, a plurality of small holes are formed in the working liquid spraying plate 3-5, each air reducing pipe 3-3 is vertically arranged, the upper portion of each air reducing pipe 3-3 is fixedly connected with the supporting screen plate 3-2 and extends out of the supporting screen plate 3-2, a cover cap 3-4 is connected to the upper end of each air reducing pipe 3-3, a gap is formed between each cover cap 3-4 and the upper opening of the corresponding air reducing pipe 3-3 and covers the upper portion of the air reducing pipe 3-3, and the lower end of each air reducing pipe 3-3 is fixedly connected with the working liquid spraying plate 3-5 and extends out of the working liquid spraying plate 3-5.
When the catalyst works, working solution from a regeneration process enters the upper part of a hydrogenation tower after the temperature of the working solution is regulated by a temperature regulator, the temperature regulator of the working solution is simultaneously provided with a steam pipeline and a circulating water pipeline, and when the activity of the catalyst is higher in the initial use stage, the working solution needs to be cooled by circulating cooling water to control the reaction temperature of the hydrogenation tower; when the activity of the catalyst is reduced in the later period of use, in order to ensure the hydrogenation efficiency, the working solution needs to be heated by steam to ensure the reaction activity temperature of the catalyst, the hydrogenation tower is divided into two towers, the catalyst in each tower is divided into three sections, in order to ensure the uniform distribution of the working solution, a gas-liquid distribution device is arranged on the upper part of each catalyst, hydrogen with pressure is also added from the upper part of each section of the hydrogenation tower after impurities are filtered by a hydrogen buffer filter, the working solution and the hydrogen flow downwards in a catalyst layer under certain reaction pressure and temperature, the reaction pressure of the hydrogenation tower is automatically controlled by using an adjusting valve according to the adding amount of the hydrogen under the action of a palladium catalyst in the flowing process, the hydrogen performs hydrogenation reaction with part of 2-ethyl anthraquinone and tetrahydro 2-ethyl anthraquinone in the working solution to generate the hydrogen anthraquinone, the working solution is changed into hydrogenation solution, and the hydrogenation solution, the hydrogen and other gases, the method is characterized in that the separation of hydrogenated tail gas and hydrogenated liquid is completed in a gas-liquid separation section, the hydrogen content of the tail gas is controlled by an adjusting valve, the tail gas is condensed by a hydrogenated tail gas condenser and a hydrogenated tail condensation liquid in a groove to recover heavy aromatic hydrocarbon solvent in the tail gas and then is discharged in high altitude through a flame arrester or returns to a torch system, the separated hydrogenated liquid controls the liquid level by the adjusting valve, and then a part of the liquid passes through a hydrogenated liquid filter and a hydrogenated liquid cooler and then enters a hydrogenated liquid storage tank to prevent catalyst powder from being brought to an oxidation process. The other part of the hydrogenated liquid is regenerated, the purpose of regeneration is to keep the cleanliness of the working liquid and reduce the consumption of anthraquinone, and the regenerant is activated alumina. The regenerated hydrogenated liquid exchanges heat with hydrogenated liquid at the outlet of the hydrogenated clay bed through a hydrogenated liquid heat exchanger, part of heat is recovered, the regenerated hydrogenated liquid enters a hydrogenated liquid clay bed after entering a hydrogenated liquid heater for heating, then enters a hydrogenated liquid filter together with the other part of hydrogenated liquid after passing through the hydrogenated liquid heat exchanger and low-temperature hydrogenated liquid heat exchange, and enters a hydrogenated liquid storage tank after being cooled by a hydrogenated liquid cooler. In order to make the hydrogenation reaction temperature more uniform and stable and increase the content of tetrahydro 2-ethylanthraquinone in the working solution at the initial start of the vehicle, a hydrogenation solution circulating pump (a first circulating pump and a second circulating pump) is arranged in the system, part of the hydrogenation solution is returned to the hydrogenation tower to be reacted with the working solution from the regeneration process in the hydrogenation tower, and the partial circulation of the hydrogenation solution is also a safety measure.
According to the production load of the system and the activity of the palladium catalyst, the catalyst can be produced by a single tower, and can also be produced by two towers in series or in parallel. When the catalytic activity of the two towers is poor, the operation of tower combination or tower series can be carried out according to the actual requirement, when the catalytic resistance is large, the operation of tower combination is carried out, and when high hydrogen efficiency is required, the operation of tower series is required; when two hydrogenation towers are operated in series, a hydrogenation tower conveying pump needs to be started in the middle to pressurize and send the hydrogenation liquid of the first hydrogenation tower to the second hydrogenation tower, and a hydrogenation liquid circulating pump needs to be started to ensure proper spraying density no matter which tower is started.
When a single column is being produced, the hydrogenation column transfer pump 25 and the fourth control valve 32 are closed, all control valves on one of the columns are closed, and all control valves on the other column are opened.
When the series of columns is produced, the hydrogenation column transfer pump 25 and the fourth control valve 32 are opened, the third control valve 31 of the first hydrogenation column 14 is closed, and the remaining control valves on both columns are opened.
When the parallel columns are produced, the hydrogenation column transfer pump 25 and the fourth control valve 32 are closed, and all the control valves on both columns are opened.
When operating in series-parallel, the hydrogenation column transfer pump 25 and the fourth control valve 32 are opened, opening all the control valves on both columns.
The utility model has the advantages that:
① the utility model discloses use equipment such as hydrogenation tower, first circulating pump, second circulating pump, hydrogenation tower delivery pump, clay bed to be less, the equipment investment is few, and 10 ten thousand tons of hydrogen peroxide of annual output are for example single hydrogenation tower be the diameter 2.4 meters, high 19 meters, and the double tower total volume is 180 cubes, and catalyst loading is also less 15-18 tons, is favorable to saving the investment, the utility model discloses in the hydrogenation technology production, because hydrogenation tower has used the inclined to one side flow prevention internals (cellular standpipe), the volume that produces the degradation thing is less compared with traditional technology, the consumption of anthraquinone is less than traditional technology, and the quantity that needs to load (regenerate hydrogenation anthraquinone degradation thing) active alumina is few, and the consumption of same active alumina reduces by a wide margin.
② the utility model can be operated in a single tower, the single tower has better effect and lower consumption, and can control the hydrogen effect to be 8.5-9.5g/l, the double tower operation can be divided into three modes, namely, the first hydrogenation tower is connected with the second hydrogenation tower, the two towers are simultaneously opened for hydrogen hydrogenation, the mode is basically the same as the single tower operation effect, and the distribution of the working solution and the hydrogenation of the working solution in the catalyst layer are not influenced, the double tower parallel working solution is averagely distributed in the two hydrogenation towers, as long as the amount of the hydrogenation solution circulating pump is increased to reach the proper spraying density, the effect of the single tower is the same as the effect of the single tower opening, the distribution of the working solution is not influenced, the two towers are simultaneously opened for hydrogen control of the hydrogen amount for hydrogenation, the double towers have both connected towers, as long as the spraying amount of each tower is well controlled, the hydrogen amount is well controlled as the effect of the single tower opening, the three operation modes are well controlled, the hydrogen effect is well controlled, the generated degradation amount is basically not greatly different from the consumption of the single tower opening, the double tower opening hydrogen peroxide solution consumption and the single tower consumption is lower.
③ the utility model is safer when the single tower is operated and the other tower is regenerated, because the two towers are independent devices, the valves capable of communicating gas are few, and the three tower sections are not overlapped together like the traditional process, the outside is provided with the outside tower communicating pipe, and the valves are shared to easily generate hydrogen or the working liquid is communicated with the spare tower section from the production tower section to cause explosion accidents.
The new double tower is compared with the traditional single tower in three-section type by taking 10 ten thousand tons of 27.5 percent hydrogen peroxide produced annually as an example:
Claims (7)
1. hydrogenation tower double tower system in anthraquinone process fixed bed production hydrogen peroxide solution technology, including hydrogen house steward, working solution house steward, clay bed, filter, hydrogenation liquid cooler and hydrogenation liquid storage tank concatenate its characterized in that in proper order: the double-tower system also comprises a first hydrogenation tower and a second hydrogenation tower which have the same structure, and the first hydrogenation tower and the second hydrogenation tower are respectively provided with a hydrogen inlet, a working solution inlet, a hydrogenation solution outlet, a hydrogenation tail gas outlet and a circulating regeneration hydrogenation solution outlet; the hydrogen inlet of the first hydrogenation tower is connected with the hydrogen inlet of the second hydrogenation tower in parallel and then is connected with the hydrogen main pipe; the working fluid inlet of the first hydrogenation tower is connected with the working fluid inlet of the second hydrogenation tower in parallel and then is connected with the working fluid main pipe; a hydrogenated liquid outlet of the first hydrogenation tower is connected with a hydrogenated liquid outlet of the second hydrogenation tower in parallel and then connected with a filter, the hydrogenated liquid outlet of the first hydrogenation tower is also connected with a hydrogenation tower delivery pump, and a liquid outlet of the hydrogenation tower delivery pump is connected with a working liquid inlet of the second hydrogenation tower; the outlet of the hydrogenation tail gas of the first hydrogenation tower and the outlet of the hydrogenation tail gas of the second hydrogenation tower are both connected with respective hydrogenation tail gas condensers, and the outlet of each hydrogenation tail gas condenser is connected with a respective hydrogenation tail gas condensate receiving tank; a circulating regeneration hydrogenation liquid outlet of the first hydrogenation tower is connected with a working liquid inlet of the first hydrogenation tower through a first circulating pump, and a circulating regeneration hydrogenation liquid outlet of the second hydrogenation tower is connected with a working liquid inlet of the second hydrogenation tower through a second circulating pump; the liquid outlet of the first circulating pump is connected with the liquid outlet of the second circulating pump in parallel and then is connected with the liquid inlet of the clay bed, and the liquid outlet of the clay bed is connected with the liquid inlet of the filter.
2. The double-tower system of the hydrogenation tower in the anthraquinone process fixed bed hydrogen peroxide production process according to claim 1, which is characterized in that: the liquid outlet of the first circulating pump is connected with the liquid outlet of the second circulating pump in parallel and then is connected with the cold side inlet of the plate heat exchanger of the heat exchanger, the cold side outlet of the plate heat exchanger of the heat exchanger is connected with the heater, the working liquid outlet of the heater is connected with the liquid inlet of the clay bed, the liquid outlet of the clay bed is connected with the liquid inlet of the hot side of the heat exchanger, and the liquid outlet of the hot side of the heat exchanger is connected with the liquid inlet of the.
3. The double-tower system of the hydrogenation tower in the anthraquinone process fixed bed hydrogen peroxide production process according to claim 1, which is characterized in that: the first hydrogenation tower and the second hydrogenation tower respectively comprise a catalyst section tower body, three layers of catalyst frame assemblies are arranged in the catalyst section tower body along the height direction, a gas-liquid distributor is arranged above each layer of catalyst frame assembly, the gas-liquid distributors are fixed with the catalyst section tower body, and a hydrogen inlet and a working liquid inlet are arranged at the top of the catalyst section tower body; each layer of catalyst frame component has the same structure and comprises a support grid plate, a lower packing layer, a plurality of vertical pipes and an upper packing layer which are sequentially arranged from bottom to top, wherein the support grid plate is connected with the inner wall of the catalyst section tower body, and the plurality of vertical pipes are arranged in a honeycomb shape and are fixed with each other.
4. The double-tower system of the hydrogenation tower in the anthraquinone process fixed bed hydrogen peroxide production process according to claim 3, which is characterized in that: the gas-liquid distributor comprises a supporting screen plate, a working liquid spraying plate and a plurality of air reducing pipes, the supporting screen plate is connected with the inner wall of the catalyst section tower body, the working liquid spraying plate is connected below the supporting screen plate, the upper portion of each air reducing pipe is fixedly connected with the supporting screen plate and stretches out the supporting screen plate, the upper end of each air reducing pipe is connected with a cap, a gap is arranged between each cap and the upper opening of the corresponding air reducing pipe, the cap covers the upper portion of the air reducing pipe, and the lower end of each air reducing pipe is fixedly connected with the working liquid spraying plate and stretches out the working liquid spraying plate.
5. The double-tower system of the hydrogenation tower in the anthraquinone process fixed bed hydrogen peroxide production process according to claim 3, which is characterized in that: the lower end of the catalyst section tower body is connected with the gas-liquid separation section tower body, the hydrogenated tail gas outlet is arranged at the upper part of the gas-liquid separation section tower body, the hydrogenated liquid outlet is arranged at the lower part of the gas-liquid separation section tower body, and the circularly regenerated hydrogenated liquid outlet is arranged at the bottom of the gas-liquid separation section tower body.
6. The double-tower system of the hydrogenation tower in the anthraquinone process fixed bed hydrogen peroxide production process according to claim 3, which is characterized in that: the top of the tower of the catalyst section tower body is internally connected with a working liquid diffusion plate, the working liquid diffusion plate is positioned right below a working liquid inlet, and the diameter of the working liquid diffusion plate is larger than that of the working liquid inlet.
7. The double-tower system of the hydrogenation tower in the anthraquinone process fixed bed hydrogen peroxide production process according to claim 2, which is characterized in that: the hydrogen inlet of the first hydrogenation tower and the hydrogen inlet of the second hydrogenation tower are respectively connected with a first control valve, and the two first control valves are connected in parallel and then connected with the outlet of the hydrogen main pipe; the working fluid inlet of the first hydrogenation tower and the working fluid inlet of the second hydrogenation tower are respectively connected with a second control valve, and the two second control valves are connected in parallel and then connected with the outlet of the working fluid main pipe; the hydrogenated liquid outlet of the first hydrogenation tower and the hydrogenated liquid outlet of the second hydrogenation tower are respectively connected with third control valves, and the two third control valves are connected with the filter in parallel; a liquid outlet of the hydrogenation tower conveying pump is connected with a fourth control valve, and a liquid outlet of the fourth control valve is connected with a working liquid inlet of the second hydrogenation tower; and a liquid outlet of the fifth control valve is connected with a liquid outlet of the sixth control valve in parallel and then is connected with a cold side inlet of the plate heat exchanger of the heat exchanger.
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| CN201921905718.XU CN210885309U (en) | 2019-11-07 | 2019-11-07 | Hydrogenation tower double-tower system in anthraquinone method fixed bed hydrogen peroxide production process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113769698A (en) * | 2021-10-29 | 2021-12-10 | 阜阳安固锅炉压力容器制造有限公司 | Hydrogenation tower |
| CN114956006A (en) * | 2021-12-13 | 2022-08-30 | 安徽国泰化工有限公司 | Pure water heating energy-saving system for supplementing hydrogen peroxide extraction tower |
-
2019
- 2019-11-07 CN CN201921905718.XU patent/CN210885309U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113769698A (en) * | 2021-10-29 | 2021-12-10 | 阜阳安固锅炉压力容器制造有限公司 | Hydrogenation tower |
| CN114956006A (en) * | 2021-12-13 | 2022-08-30 | 安徽国泰化工有限公司 | Pure water heating energy-saving system for supplementing hydrogen peroxide extraction tower |
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Address after: Room 101, Building 11, Jinrong Science and Technology Park, No. 158 Ji'an South Road, High tech Development Zone, Yangzhou City, Jiangsu Province, 225128 Patentee after: Jiangsu Zhongxu Technology Co.,Ltd. Address before: No. 4, Huagang Road, Hanjiang Industrial Park, Yangzhou, Jiangsu 225128 Patentee before: Yangzhou Rongxiang Technology Development Co.,Ltd. |