CN212864142U

CN212864142U - Fixed bed hydrogen peroxide solution apparatus for producing

Info

Publication number: CN212864142U
Application number: CN202020845729.XU
Authority: CN
Inventors: 向家勇; 向能; 李晓峰; 吴婷
Original assignee: Jiangsu Huda Chemical Technology Co ltd
Current assignee: Jiangsu Huda Chemical Technology Co ltd
Priority date: 2020-05-19
Filing date: 2020-05-19
Publication date: 2021-04-02
Anticipated expiration: 2030-05-19

Abstract

The utility model relates to a fixed bed hydrogen peroxide solution apparatus for producing, including hydrogenation tower, oxidation tower and extraction tower, hydrogen and working solution are through the pipe-line transport hydrogenation tower separately, hydrogen and working solution take place hydrogenation reaction in the hydrogenation tower, obtain the hydrogenation liquid mixture, the hydrogenation liquid mixture passes through the discharge tube and discharges, discharge pipe way connection vapour and liquid separator, vapour and liquid separator intercommunication has gas discharge pipe and hydrogenation liquid transmission pipe, vapour and liquid separator discharges gas separation from gas discharge pipe, the hydrogenation liquid of separation is discharged from the hydrogenation liquid transmission pipe, get into oxidation tower and extraction tower in proper order and react. The utility model arranges 3 sections of catalyst bed layers in the fixed bed hydrogenation tower, and arranges annular baffling plates at intervals on the inner wall of the catalyst bed layer, thereby reducing wall flow, ensuring that gas-liquid flow at the inner wall is uniform, having high catalytic efficiency and ensuring that working liquid can be uniformly hydrogenated; 5-30% of the hydrogenation liquid is circulated to the hydrogen dissolving mixer and then enters a fixed bed hydrogenation tower to increase the fluidity of reactants in a catalyst bed layer and the amount of dissolved hydrogen.

Description

Fixed bed hydrogen peroxide solution apparatus for producing

Technical Field

The utility model relates to a fixed bed hydrogen peroxide solution apparatus for producing belongs to hydrogen peroxide solution manufacture equipment technical field.

Background

The hydrogen peroxide is also called as hydrogen peroxide, is an important green chemical product, and can not pollute the environment in the using process, so the hydrogen peroxide serving as an oxidant, a bleaching agent and a disinfectant is widely applied to the industries of chemical industry, papermaking, environmental protection, electronics and the like. The prior production method of hydrogen peroxide adopts an anthraquinone method and mainly comprises the working procedures of hydrogenation, oxidation, extraction and purification. The hydrogen peroxide production process is divided into a fixed bed process and a fluidized bed process according to different hydrogenation reactors. In China, a fixed bed hydrogenation process is mostly adopted, working liquid and hydrogen carry out gas-liquid-solid three-phase reaction in a fixed bed reactor filled with a catalyst, and the quality of the hydrogenation process directly influences the quality and the yield of products. In the hydrogenation process, gas is a continuous phase, liquid is a dispersed phase, and the whole process is influenced by the gas-liquid mass transfer process. The fixed bed hydrogenation tower has 2 to 3 tower sections which are connected in series from top to bottom. In the production process, the catalyst bed layer gradually generates the phenomena of sinking, compaction and agglomeration to cause channeling, bias flow and short circuit, so that the catalyst cannot be completely wetted, the working solution is unevenly distributed on the surface of the catalyst, the hydrogenation process is uneven, the catalyst efficiency is reduced, and side reaction occurs. The side reaction produces degradation products, influences the yield of hydrogen peroxide, influences the density, viscosity and surface tension of the working solution, increases the consumption of anthraquinone, and has adverse effects on subsequent oxidation, extraction and working solution regeneration. The hydrogen anthraquinone in hydrogenated liquid after hydrogenation is oxidized by air to generate hydrogen peroxide, in the existing hydrogen peroxide oxidation process, 2-3 oxidation towers are adopted for series operation, so that in order to ensure that the hydrogenated liquid is completely oxidized, longer reaction time is needed, side reaction is caused and hydrogen peroxide is decomposed, and meanwhile, the oxidation tower is larger in equipment. In the extraction process, the oxidation liquid enters the extraction tower from the tower bottom, flows upwards as a dispersed phase to small droplets, water is added from the tower top and flows downwards as a continuous phase, and hydrogen peroxide is obtained at the tower bottom. The density difference between the organic phase and the water phase is small, the mass transfer driving force is small, and the extraction effect is not good.

Disclosure of Invention

In order to solve the technical problem, the utility model provides a fixed bed hydrogen peroxide solution apparatus for producing, its concrete technical scheme as follows:

the fixed bed hydrogen peroxide production device comprises a hydrogenation tower, an oxidation tower and an extraction tower, wherein the hydrogenation tower is communicated with a hydrogen input pipeline, a working liquid input pipeline and a discharge pipeline, hydrogen and working liquid are conveyed to the hydrogenation tower through respective pipelines, hydrogenation reaction is carried out on the hydrogen and the working liquid in the hydrogenation tower to obtain a hydrogenated liquid mixture, the hydrogenated liquid mixture is discharged through the discharge pipeline, the discharge pipeline is connected to a gas-liquid separator, the gas-liquid separator is communicated with a gas discharge pipe and a hydrogenated liquid transmission pipe, the gas-liquid separator separates gas and discharges the gas from the gas discharge pipe, the separated hydrogenated liquid is discharged from the hydrogenated liquid transmission pipe, the hydrogenated liquid transmission pipe is connected to the oxidation tower, the hydrogenated liquid transmission pipe is connected with an air inlet pipe, air is conveyed to the hydrogenated liquid transmission pipe from the air inlet pipe, is mixed with the hydrogenated liquid and then is simultaneously conveyed to the oxidation tower, and the oxidation tower is communicated with a tail, the primary product output pipeline is connected with a mixer, the mixer is provided with a nozzle, the nozzle of the mixer is connected to a liquid inlet of the extraction tower, the extraction tower is provided with a hydrogen peroxide discharge pipeline and a working liquid discharge pipeline in a penetrating mode, the pre-heater further comprises a dissolved hydrogen mixer and a pre-heater, the pre-heater is connected with the dissolved hydrogen mixer through a pipeline, the dissolved hydrogen mixer is further provided with a hydrogen gas inlet and a gas-liquid mixture transmission pipe, the hydrogen gas inlet is connected with a hydrogen input pipeline, the gas-liquid mixture transmission pipe is connected to the hydrogenation tower, the hydrogen gas and the working liquid heated by the pre-heater are conveyed to the dissolved hydrogen mixer, the dissolved hydrogen mixer outputs a hydrogen-saturated gas-liquid mixture through the gas-liquid mixture transmission pipe, and the hydrogen-saturated.

Further, the gas-liquid separator is also connected with a circulating pump, and 5% -30% of the hydrogenated liquid in the gas-liquid separator is circularly conveyed to the dissolved hydrogen mixer by the circulating pump.

Furthermore, the hydrogenation tower is internally provided with 3 sections of catalyst bed layers, and the inner wall of each catalyst bed layer is provided with an annular baffling baffle with holes.

Furthermore, a metal wire mesh filler is orderly arranged in the hydrogen dissolving mixer.

Further, the extraction tower is a plate tower or a packed tower.

Furthermore, the annular baffling plates are arranged in the catalyst bed layer at equal intervals, the number of the annular baffling plates is not more than 5, the width of each annular baffling plate is 0.5% -5% of the diameter of the catalyst bed layer, and the diameter of each opening is 2-5 times of the particle size of the catalyst.

The utility model has the advantages that:

the utility model has the advantages that 3 sections of catalyst bed layers are arranged in the hydrogenation tower, and the annular baffling plates are arranged on the inner walls of the catalyst bed layers at intervals, so that the wall flow is reduced, the gas-liquid flow at the inner walls is uniform, the catalysis efficiency is high, and the working liquid can be uniformly hydrogenated; 5% -30% of the hydrogenation liquid circulates to the dissolved hydrogen mixer and then enters a fixed bed hydrogenation tower, so that the fluidity of reactants in a catalyst bed layer and the amount of dissolved hydrogen are increased, and the stability and the reaction rate of the catalyst bed layer are improved; the metal wire mesh packing is arranged in the hydrogen dissolving mixer in order to ensure that the hydrogen and the working solution are mixed quickly and uniformly; the oxidation mixed liquid and air are fully mixed in the mixer and then are sprayed into the bottom of the extraction tower through the nozzle, so that the working liquid is dispersed into tiny liquid drops, and meanwhile, the turbulence is promoted by the bubbles of the liquid phase, so that the liquid drops are broken less, and the mass transfer efficiency is improved.

Drawings

FIG. 1 is a schematic diagram showing the connection of the reaction apparatus of the present invention,

wherein, 1-hydrogen input pipeline, 2-hydrogenation tower, 3-gas-liquid separator, 4-circulating pump 4, 5-dissolved hydrogen mixer, 6-preheater, 7-oxidation tower, 8-mixer, 9-extraction tower.

Detailed Description

The present invention will now be described in further detail with reference to the accompanying drawings. These drawings are simplified schematic drawings and illustrate the basic structure of the present invention only in a schematic manner, and thus show only the components related to the present invention.

As shown in figure 1, the utility model discloses a fixed bed hydrogen peroxide solution apparatus for producing, including hydrogenation tower 2, oxidation tower 7 and extraction tower 9, 2 sections series connection formation fixed bed hydrogenation towers in two hydrogenation towers. The hydrogenation tower 2 is internally provided with 3 sections of catalyst bed layers, and the inner wall of each catalyst bed layer is provided with a perforated annular baffling baffle. The annular baffling plates are arranged in the catalyst bed layer at equal intervals, the number of the annular baffling plates is not more than 5, the width of each annular baffling plate is 0.5-5% of the diameter of the catalyst bed layer, and the diameter of each opening is 2-5 times of the particle size of the catalyst. The hydrogenation tower 2 is communicated with a hydrogen input pipeline 1, a working solution input pipeline and a discharge pipeline, hydrogen and working solution are conveyed to the hydrogenation tower 2 through respective pipelines, the hydrogen and the working solution are subjected to hydrogenation reaction in the hydrogenation tower 2 to obtain a hydrogenated solution mixture, the hydrogenated solution mixture is discharged through the discharge pipeline, the discharge pipeline is connected to a gas-liquid separator 3, the gas-liquid separator 3 is communicated with a gas discharge pipe and a hydrogenated solution transmission pipe, the gas-liquid separator 3 separates gas and discharges the gas from the gas discharge pipe, the separated hydrogenated solution is discharged from the hydrogenated solution transmission pipe, the gas-liquid separator 3 is further connected with a circulating pump 4, and 5% -30% of the hydrogenated solution in the gas-liquid separator 3 is circularly conveyed to a hydrogen dissolving mixer 5 through the circulating pump 4. Hydrogenated liquid duct connection is to oxidation tower 7, hydrogenated liquid duct connection has the air to advance the pipe, the air advances the pipe from the air and carries the hydrogenated liquid conveyer pipe, mix with hydrogenated liquid, then carry oxidation tower 7 simultaneously, oxidation tower 7 intercommunication has tail gas exhaust pipeline and first product output pipeline, first product output pipeline is connected to the inlet of extraction tower 9, extraction tower 9 has link up hydrogen peroxide solution exhaust pipeline and working solution exhaust pipeline, still including dissolving hydrogen mixer 5 and pre-heater 6, in 5 neatly being provided with wire mesh filler in dissolving hydrogen mixer. The preheater 6 is connected with the hydrogen dissolving mixer 5 through a pipeline, the hydrogen dissolving mixer 5 is further provided with a hydrogen gas inlet and a gas-liquid mixture transmission pipe, the hydrogen gas inlet is connected with the hydrogen gas input pipeline 1, the gas-liquid mixture transmission pipe is connected to the hydrogenation tower 2, hydrogen gas and working liquid heated by the preheater 6 are transmitted to the hydrogen dissolving mixer 5, the hydrogen dissolving mixer 5 outputs a hydrogen-saturated gas-liquid mixture through the gas-liquid mixture transmission pipe, and the hydrogen-saturated gas-liquid mixture is input to the hydrogenation tower 2.

As shown in fig. 1, in the actual reaction process, the working solution, part of the hydrogenated liquid at the outlet of the gas-liquid separator 3 and the hydrogen gas enter the hydrogen-dissolved mixer 5, and the gas phase and the liquid phase are efficiently mixed, so that the insoluble hydrogen gas is dispersed into a large amount of micro bubbles in the working solution, and the solubility of the hydrogen gas in the working solution reaches a saturated state, thereby forming a gas-liquid mixture. Wherein, the hydrogen dissolved in the hydrogen dissolving mixer 5 accounts for 1-30% of the total hydrogen, and regular wire mesh packing is filled in the hydrogen dissolving mixer 5 to ensure that the hydrogenation and the working solution are quickly and uniformly mixed. Hydrogen is supplemented to enter a hydrogenation tower 2 through a hydrogen input pipeline 1, the hydrogenation tower 2 is provided with 1-3 sections of catalyst bed layers, annular baffling baffles with holes are arranged on the inner wall of each catalyst bed layer to play a role in reducing wall flow and enabling gas-liquid flow at the inner wall to be uniform, the number of the baffles is 1-5, the baffles are equidistantly arranged in the catalyst bed layers, the width of each baffle is 0.5-5% of the diameter of each catalyst bed layer, the diameter of each opening is 2-5 times of the particle size of the catalyst, and the hydrogen and hydrogen-dissolved working solution from a hydrogen-dissolved mixer 5 enter the catalyst bed layers to react. The hydrogenation tower 2 outputs a gas-liquid mixture to the gas-liquid separator 3, the gas-liquid mixture is separated in the gas-liquid separator 3 to form gas and hydrogenated liquid, the gas is recycled by the gas recovery device, part of the hydrogenated liquid is circularly conveyed to the dissolved hydrogen mixer 5 by the circulating pump 4, and the rest of the hydrogenated liquid enters the oxidation tower 7. Part of the hydrogenated liquid output by the gas-liquid separator 3 is circulated to an inlet of a dissolved hydrogen mixer 5 to increase the fluidity of the materials in the catalyst bed layer and the amount of dissolved hydrogen, improve the stability and the reaction rate of the catalyst bed layer, and the circulated hydrogenated liquid accounts for 5-30% of the total hydrogenated liquid. Wherein, the improvement of the dissolved hydrogen and the reaction pressure is helpful for increasing the solution of the hydrogen in the working solution and accelerating the reaction rate, but the hydrogen concentration is too high to easily cause deep hydrogenation, and the reaction pressure is controlled to be 0.2-0.5 MPa. The working solution takes 2-ethylanthraquinone and tetrahydro 2-ethylanthraquinone or 2-amylanthraquinone and tetrahydro 2-ethylanthraquinone as solutes, heavy aromatic hydrocarbon as anthraquinone solvent, and one or more of trioctyl phosphate, tetrabutyl urea, diisobutyl methanol and methyl cyclohexyl acetate as hydroanthraquinone solvent. The hydrogenated liquid and air enter an oxidation tower 7 for oxidation reaction, the volume flow ratio of the air to the hydrogenated liquid is 3: 1-20: 1, and the adding amount of the air is properly controlled to prevent excessive oxygen. Part of gas at the outlet of the oxidation tower 7 and the oxidation liquid are mixed in the mixer 8 and are sprayed into the bottom of the extraction tower 9 through a nozzle on the mixer 8, so that the working liquid is dispersed into tiny liquid drops, and meanwhile, the turbulence is promoted through bubbles of the liquid phase, so that the liquid drops are broken smaller, and the mass transfer efficiency is improved. A small amount of unreacted materials in the extraction tower 9 further react with oxygen, so that the oxidation effect is improved, air is fully utilized, the hydrogenation liquid is completely oxidized, and the oxygen content in the discharged tail gas is low. The extraction efficiency is improved by 20-50% compared with the simple liquid-liquid extraction, and the height of the extraction tower 9 can be effectively reduced. The working temperature of the oxidation tower 7 is 40-60 ℃, the pressure is 0.2-0.3MPa, the oxidation time is 5-20 minutes, the working temperature of the extraction tower 9 is 50-55 ℃, the normal pressure is achieved, and the gas-liquid volume flow ratio of the feeding at the bottom of the tower is 0.1: 1-2: 1.

The utility model has the advantages that 3 sections of catalyst bed layers are arranged in the fixed bed hydrogenation tower, and the annular baffling plates are arranged on the inner wall of the catalyst bed layers at intervals, so that the wall flow is reduced, the gas-liquid flow at the inner wall is uniform, the catalysis efficiency is high, and the working liquid can be uniformly hydrogenated; 5% -30% of the hydrogenation liquid circulates to the dissolved hydrogen mixer and then enters a fixed bed hydrogenation tower, so that the fluidity of reactants in a catalyst bed layer and the amount of dissolved hydrogen are increased, and the stability and the reaction rate of the catalyst bed layer are improved; the metal wire mesh packing is arranged in the hydrogen dissolving mixer in order to ensure that the hydrogen and the working solution are mixed quickly and uniformly; the oxidation mixed liquid and air are fully mixed in the mixer and then are sprayed into the bottom of the extraction tower through the nozzle, so that the working liquid is dispersed into tiny liquid drops, and meanwhile, the turbulence is promoted by the bubbles of the liquid phase, so that the liquid drops are broken less, and the mass transfer efficiency is improved.

In light of the foregoing, it will be apparent to those skilled in the art from this disclosure that various changes and modifications can be made without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.

Claims

1. A fixed bed hydrogen peroxide production device comprises a hydrogenation tower (2), an oxidation tower (7) and an extraction tower (9), wherein the hydrogenation tower (2) is communicated with a hydrogen input pipeline (1), a working solution input pipeline and a discharge pipeline, hydrogen and working solution are conveyed to the hydrogenation tower (2) through respective pipelines, hydrogenation reaction is carried out on the hydrogen and the working solution in the hydrogenation tower (2) to obtain a hydrogenation solution mixture, the hydrogenation solution mixture is discharged through the discharge pipeline, the discharge pipeline is connected to a gas-liquid separator (3), the gas-liquid separator (3) is communicated with a gas discharge pipe and a hydrogenation solution transmission pipe, the gas-liquid separator (3) separates gas and discharges the gas from the gas discharge pipe, the separated hydrogenation solution is discharged from the hydrogenation solution transmission pipe, the hydrogenation solution transmission pipe is connected to the oxidation tower (7), the hydrogenation solution transmission pipe is connected with an air inlet pipe, and air is conveyed to the hydrogenation solution transmission pipe from the air inlet pipe, mix with hydrogenation liquid, then carry oxidation tower (7) simultaneously, oxidation tower (7) intercommunication has exhaust emission pipeline and initial product output pipeline, and initial product output pipeline is connected with blender (8), blender (8) are provided with the nozzle, and the nozzle of blender (8) is connected to the inlet of extraction tower (9), extraction tower (9) are link up hydrogen peroxide solution discharge pipe and working solution discharge pipe, its characterized in that: the hydrogen dissolving mixer is characterized by further comprising a hydrogen dissolving mixer (5) and a preheater (6), wherein the preheater (6) is connected with the hydrogen dissolving mixer (5) through a pipeline, the hydrogen dissolving mixer (5) is further provided with a hydrogen gas inlet and a gas-liquid mixture transmission pipe, the hydrogen gas inlet is connected with a hydrogen gas input pipeline (1), the gas-liquid mixture transmission pipe is connected to the hydrogenation tower (2), hydrogen gas and working liquid heated by the preheater (6) are conveyed to the hydrogen dissolving mixer (5), the hydrogen dissolving mixer (5) outputs a hydrogen-saturated gas-liquid mixture through the gas-liquid mixture transmission pipe, and the hydrogen-saturated gas-liquid mixture is input to the hydrogenation tower (2).

2. The fixed bed hydrogen peroxide production device according to claim 1, characterized in that: the gas-liquid separator (3) is also connected with a circulating pump (4), and 5-30% of hydrogenated liquid in the gas-liquid separator (3) is circularly conveyed to the dissolved hydrogen mixer (5) by the circulating pump (4).

3. The fixed bed hydrogen peroxide production device according to claim 1, characterized in that: the hydrogenation tower (2) is internally provided with 3 sections of catalyst bed layers, and the inner wall of each catalyst bed layer is provided with a perforated annular baffling baffle.

4. The fixed bed hydrogen peroxide production device according to claim 1, characterized in that: and the dissolved hydrogen mixer (5) is orderly provided with a metal wire mesh filler.

5. The fixed bed hydrogen peroxide production device according to claim 1, characterized in that: the extraction tower (9) is a plate tower or a packed tower.

6. The fixed bed hydrogen peroxide production device according to claim 3, characterized in that: the annular baffling plates are arranged in the catalyst bed layer at equal intervals, the number of the annular baffling plates is not more than 5, the width of each annular baffling plate is 0.5-5% of the diameter of the catalyst bed layer, and the diameter of each opening is 2-5 times of the particle size of the catalyst.