CN217829949U - System for preparing hydrogen peroxide by anthraquinone process - Google Patents
System for preparing hydrogen peroxide by anthraquinone process Download PDFInfo
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- CN217829949U CN217829949U CN202221389232.7U CN202221389232U CN217829949U CN 217829949 U CN217829949 U CN 217829949U CN 202221389232 U CN202221389232 U CN 202221389232U CN 217829949 U CN217829949 U CN 217829949U
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Abstract
The utility model provides a system for preparing hydrogen peroxide by anthraquinone process, which comprises a reaction kettle, a hydrogenation liquid filter, a hydrogenation liquid storage tank, an oxidation tower, a gas-liquid separator and an extraction tower which are connected in sequence, wherein the raffinate phase of the extraction tower is connected to a circulating working liquid tank; this reation kettle is suspension reation kettle, and the working solution in circulation work cistern is added from reation kettle's bottom, and the reation kettle bottom still is equipped with hydrogen and nitrogen gas and adds the pipeline, and suspension reation kettle upper portion ejection of compact is connected to hydrogenation liquid filter. The utility model discloses an adopt suspension reation kettle's form, can make the material be in fluidized state, hydrogenation reaction efficiency is high, the condition is mild, the accessory substance is few, the anthraquinone consumption is low. The system can also realize effective recycling of the catalyst.
Description
Technical Field
The utility model belongs to the chemical industry field relates to the production of hydrogen peroxide, specifically is a system for preparing hydrogen peroxide by anthraquinone process.
Background
Most of domestic hydrogen peroxide production devices at present adopt an anthraquinone method fixed bed process, 2-ethyl anthraquinone is adopted as a carrier, several of C9-C10 heavy aromatics, trioctyl phosphate, o-methyl cyclohexyl acetate and tetrabutyl urea are adopted as solvents to prepare a working solution, and industrial-grade hydrogen peroxide products are obtained through the processes of hydrogenation, oxidation, extraction, purification and the like.
In the anthraquinone process fixed bed process, hydrogen and working solution react on the surface of a catalyst bed layer, and due to the existence of fluid distribution and bias flow conditions, the catalyst in the fixed bed has low utilization rate and deep hydrogenation products, so that the hydrogenation side reactions are more, the consumption of 2-ethyl anthraquinone raw materials is large, and the expected effect is difficult to achieve particularly when the catalyst is applied to a large-scale hydrogen peroxide production device.
Disclosure of Invention
The utility model provides a system for hydrogen peroxide is made to anthraquinone process, hydrogenation reaction efficiency is high, the condition is mild, the accessory substance is few, and the anthraquinone consumption is low.
The technical scheme of the utility model is that the system for preparing hydrogen peroxide by the anthraquinone method comprises a reaction kettle, a hydrogenation liquid filter, a hydrogenation liquid storage tank, an oxidation tower, a gas-liquid separator and an extraction tower which are connected in sequence, wherein the raffinate phase of the extraction tower is connected to a circulating working liquid tank; this reation kettle is suspension reation kettle, and the working solution in circulation work cistern is added from reation kettle's bottom, and the reation kettle bottom still is equipped with hydrogen and nitrogen gas and adds the pipeline, and suspension reation kettle upper portion ejection of compact is connected to hydrogenation liquid filter.
Further, the system also comprises a catalyst adding tank, and filter residues filtered by the hydrogenation liquid filter are connected to the lower part of the catalyst adding tank through a pipeline.
Furthermore, the circulating working liquid tank is connected to the bottom of the reaction kettle through a circulating working liquid pump and a pipeline, and the catalyst adding tank is connected to a pipeline between the circulating working liquid pump and the reaction kettle through a pipeline.
Furthermore, a plurality of hydrogenation liquid filters are arranged between the reaction kettle and the hydrogenation liquid storage tank in parallel and/or in series in the system.
Further, the number of the hydrogenation liquid filters is at least 3, and at least one of the filters is arranged in parallel.
Furthermore, a hydrogenated liquid pump is arranged between the hydrogenated liquid storage tank and the oxidation tower, the hydrogenated liquid pump is connected to the upper part of the oxidation tower through a pipeline, and an air feeding pipeline is arranged at the lower part of the oxidation tower.
Furthermore, the hydrogenated liquid pump is also connected to a filtrate outlet of the hydrogenated liquid filter through a back flush pipeline, and a filter residue outlet of the hydrogenated liquid filter is connected to the lower part of the reaction kettle through the back flush pipeline.
The utility model discloses following beneficial effect has:
1. the utility model discloses an adopt suspension reation kettle's form, can make the material be in fluidized state, can realize the intensive mixing of catalyst, working solution and hydrogen solid-liquid gas three-phase, hydrogenation reaction is efficient, the condition is mild, the accessory substance is few, the anthraquinone consumption is low.
2. The hydrogenation liquid filter arranged in the system can effectively intercept powder carried out by the hydrogenation liquid, and the precision of the filter is 0.5-5 mu m; meanwhile, the arrangement of a plurality of hydrogenation liquid filters can be switched as required, and a back-washing pipeline of the hydrogenation liquid filters is also arranged, so that the catalyst powder on the surfaces of the filter elements is back-washed by the hydrogenation liquid pump, the catalyst is effectively recycled, and the utilization rate of the catalyst is improved.
3. The utility model is provided with the catalyst adding tank, on one hand, the catalyst recovered by the hydrogenation liquid filter can be collected for recycling, and simultaneously, the catalyst can be added through the outside; and the catalyst adding tank is connected to a pipeline between the circulating working solution and the reaction kettle, so that the catalyst can be added in a driving state, and the control is flexible.
Drawings
Fig. 1 is a schematic structural diagram of the system of the present invention. The device comprises a reaction kettle 1, a reaction kettle 2, a hydrogenation liquid filter 3, a hydrogenation liquid tank 4, an oxidation tower 5, a gas-liquid separator 6, an extraction tower 7, a circulating working liquid tank 8, a catalyst feeding tank 9, a hydrogen pipeline 10, a nitrogen pipeline 11, an air pipeline 12, a hydrogenation liquid pump 13 and a circulating working liquid pump.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
The utility model discloses a system for preparing hydrogen peroxide by anthraquinone process, which comprises a reaction kettle, a hydrogenation liquid filter, a hydrogenation liquid storage tank, an oxidation tower, a gas-liquid separator and an extraction tower which are connected in sequence, wherein the raffinate phase of the extraction tower is connected to a circulating working liquid tank; this reation kettle is suspension reation kettle, and the working solution in circulation work cistern is added from reation kettle's bottom, and the reation kettle bottom still is equipped with hydrogen and nitrogen gas and adds the pipeline, and suspension reation kettle upper portion ejection of compact is connected to hydrogenation liquid filter.
In a preferred embodiment, the system further comprises a catalyst feeding tank, and filter residue filtered by the hydrogenation liquid filter is connected to the lower part of the catalyst feeding tank through a pipeline. Taking the palladium catalyst as an example, the palladium catalyst can be effectively recycled, and the utilization rate of the catalyst is improved.
In a further preferred scheme, the circulating working liquid tank is connected to the bottom of the reaction kettle through a circulating working liquid pump and a pipeline, and the catalyst adding tank is connected to the pipeline between the circulating working liquid pump and the reaction kettle through a pipeline. The continuous online adding of the catalyst can be realized, and the mixing can be more uniform.
Preferably, the hydrogenation liquid filter in the system is in a plurality of sets, and is arranged between the reaction kettle and the hydrogenation liquid storage tank in parallel and/or in series. The accuracy of the hydrogenation liquid filter is 0.5-5 μm, the number n is more than or equal to 3, wherein, less filters are arranged in parallel and are switched periodically, and the catalyst powder on the surface of the filter element is back-flushed by the hydrogenation liquid pump.
Preferably, a hydrogenation liquid pump is arranged between the hydrogenation liquid storage tank and the oxidation tower, the hydrogenation liquid pump is connected to the upper part of the oxidation tower through a pipeline, and an air feeding pipeline is arranged at the lower part of the oxidation tower.
Preferably, the hydrogenation liquid pump is also connected to a filtrate outlet of the hydrogenation liquid filter through a back flushing pipeline, and a filter residue outlet of the hydrogenation liquid filter is connected to the lower part of the reaction kettle through a back flushing pipeline.
The specific process conditions are as follows:
the working solution consists of C10 heavy aromatic hydrocarbon, trioctyl phosphate, tetrabutyl urea/o-methylcyclohexyl acetate and 2-ethylanthraquinone/2-amylanthraquinone, and the specific proportion is that the concentration of the C10 heavy aromatic hydrocarbon is 400-800g/kg, the concentration of the trioctyl phosphate is 100-300g/kg, the concentration of the tetrabutyl urea/o-methylcyclohexyl acetate is 50-200g/kg, and the concentration of the 2-ethylanthraquinone/2-amylanthraquinone is 150-400g/kg.
The catalyst is palladium powder catalyst, the palladium content is 1-3%, the stacking weight is 0.4-0.8g/mL, and the particle size is 20-150 μm.
In order to ensure that the catalyst is in a fluidized state in the suspension reaction kettle, the gas-liquid ratio is controlled to be within 30 to 100.
The hydrogenation reaction conditions are that the temperature is 45-70 ℃, the pressure is 0.1-0.3MPa, and the liquid phase space velocity is 10-100 m/s.
The oxidation reaction conditions are that the temperature is 50-60 ℃, the pressure is 0.4-0.45MPa, and air and hydrogenation liquid are in countercurrent contact reaction.
In the process of preparing hydrogen peroxide by adopting the anthraquinone method by adopting the system, firstly C10 heavy aromatics, trioctyl phosphate and tetrabutyl urea are compounded into a working solvent according to the proportion, and 2-ethyl anthraquinone is added into the working solvent to prepare working solution. Adjusting the nitrogen flow to enable the suspension reaction kettle to be in a fluidized state, starting a circulating working fluid pump 13 to control the flow to enter the suspension reaction kettle 1, adding a palladium catalyst into the suspension reaction kettle through a catalyst feeding tank 8, intercepting the palladium catalyst through a hydrogenation liquid filter 2 after discharging the suspension reaction kettle 1, then entering a hydrogenation liquid tank 3, starting a hydrogenation liquid pump 12, pumping the palladium catalyst into an oxidation tower 4 to perform countercurrent oxidation with air, after the working liquid comes out from the bottom and enters a gas-liquid separator 5 to perform gas-liquid separation, allowing the liquid to enter an extraction tower 6 to complete extraction to obtain an extraction phase hydrogen peroxide aqueous solution and an extraction raffinate phase working liquid, returning the extract raffinate phase to a circulating working fluid tank 7, and after the oxygen content is qualified, adding hydrogen to perform reaction, thereby realizing the whole circulating reaction.
In a specific case, the flow rate of the working fluid is 100L/h, and the gas carrying capacity of the hydrogen and the nitrogen is 3Nm 3 H, the hydrogenation efficiency is 14g/L, the hydrogenation pressure is 0.05-0.2MPa, the pressure of an oxidation tower is 0.42MPa, the oxidation efficiency is 13.5g/L, the hydrogenation temperature is 50-70 ℃, the temperature of the oxidation tower is 50-70 ℃, and the oxidation yield is 96.43 percent.
Claims (7)
1. A system for preparing hydrogen peroxide by an anthraquinone process is characterized in that: the device comprises a reaction kettle, a hydrogenated liquid filter, a hydrogenated liquid storage tank, an oxidation tower, a gas-liquid separator and an extraction tower which are sequentially connected, wherein the raffinate phase of the extraction tower is connected to a circulating working liquid tank; this reation kettle is suspension reation kettle, and the working solution in circulation work cistern is added from reation kettle's bottom, and the reation kettle bottom still is equipped with hydrogen and nitrogen gas and adds the pipeline, and suspension reation kettle upper portion ejection of compact is connected to hydrogenation liquid filter.
2. The system of claim 1, wherein: the system also comprises a catalyst adding tank, and filter residues filtered by the hydrogenation liquid filter are connected to the lower part of the catalyst adding tank through a pipeline.
3. The system of claim 2, wherein: the circulating working liquid groove is connected to the bottom of the reaction kettle through a circulating working liquid pump and a pipeline, and the catalyst adding tank is connected to the pipeline between the circulating working liquid pump and the reaction kettle through a pipeline.
4. The system of claim 1, wherein: the hydrogenation liquid filter in the system is in a plurality of parallel and/or series connection and is arranged between the reaction kettle and the hydrogenation liquid storage tank.
5. The system of claim 4, wherein: the number of the hydrogenation liquid filters is at least 3, and at least one of the hydrogenation liquid filters is arranged in parallel.
6. The system of claim 1, wherein: a hydrogenated liquid pump is arranged between the hydrogenated liquid storage tank and the oxidation tower, the hydrogenated liquid pump is connected to the upper part of the oxidation tower through a pipeline, and an air adding pipeline is arranged at the lower part of the oxidation tower.
7. The system of claim 6, wherein: the hydrogenated liquid pump is also connected to a filtrate outlet of the hydrogenated liquid filter through a back flush pipeline, and a filter residue outlet of the hydrogenated liquid filter is connected to the lower part of the reaction kettle through the back flush pipeline.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221389232.7U CN217829949U (en) | 2022-06-06 | 2022-06-06 | System for preparing hydrogen peroxide by anthraquinone process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202221389232.7U CN217829949U (en) | 2022-06-06 | 2022-06-06 | System for preparing hydrogen peroxide by anthraquinone process |
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| CN202221389232.7U Active CN217829949U (en) | 2022-06-06 | 2022-06-06 | System for preparing hydrogen peroxide by anthraquinone process |
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