CN220258054U - Regeneration device for anthraquinone degradation products in anthraquinone process hydrogen peroxide production - Google Patents
Regeneration device for anthraquinone degradation products in anthraquinone process hydrogen peroxide production Download PDFInfo
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- CN220258054U CN220258054U CN202321578434.0U CN202321578434U CN220258054U CN 220258054 U CN220258054 U CN 220258054U CN 202321578434 U CN202321578434 U CN 202321578434U CN 220258054 U CN220258054 U CN 220258054U
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- anthraquinone
- regeneration
- hydrogen peroxide
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- filter
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- 230000008929 regeneration Effects 0.000 title claims abstract description 57
- 238000011069 regeneration method Methods 0.000 title claims abstract description 57
- 150000004056 anthraquinones Chemical class 0.000 title claims abstract description 51
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 title claims abstract description 50
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000007857 degradation product Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000012530 fluid Substances 0.000 claims abstract description 41
- 239000012224 working solution Substances 0.000 claims abstract description 39
- 238000009835 boiling Methods 0.000 claims abstract description 20
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 16
- 238000003860 storage Methods 0.000 claims abstract description 16
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000004927 clay Substances 0.000 description 8
- 238000011010 flushing procedure Methods 0.000 description 3
- 230000001172 regenerating effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000011001 backwashing Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The application relates to the technical field of anthraquinone degradation product regeneration, and provides a regeneration device of anthraquinone degradation product in anthraquinone process hydrogen peroxide production, which comprises the following components: a working solution storage tank, a working solution pump, a preheater, a boiling bed, a regeneration filter and a hydrogenation reactor which are sequentially connected through a main pipeline; the fluidized bed is movably filled with micro activated alumina balls, the top of the regenerated filter is connected with a backwash pipe, the backwash pipe is connected with the working solution storage tank, a backwash pump is arranged on the backwash pipe, and a return pipe is arranged between the bottom of the regenerated filter and the bottom of the fluidized bed for communication. Heating by a preheater, and then fully mixing with the micro activated alumina balls to realize the regeneration of anthraquinone degradation products; the phenomenon of uneven regeneration distribution and bias flow of working fluid is effectively avoided, and the regeneration efficiency is improved; and simultaneously, the regenerated filter is backwashed through a backwash pump, a backwash pipe and a return pipe, so that the utilization rate of the miniature activated alumina balls is improved, and the use amount of the miniature activated alumina balls is reduced.
Description
Technical Field
The application belongs to the technical field of anthraquinone degradation product regeneration, and particularly relates to a regeneration device of an anthraquinone degradation product in the production of hydrogen peroxide by an anthraquinone process.
Background
Clay beds are used industrially for the regeneration of anthraquinone degradation products. The regeneration device of the prior art is shown in figure 1, and comprises a base tower 1, a base separator 2, a plurality of parallel post-treatment clay beds 3, a working solution receiving tank 4, a working solution pump 5, a working solution filter 6, a working solution heat exchanger 7 and a hydrogenation reactor 8 which are sequentially connected, wherein a plurality of clay beds are filled with a large amount of activated alumina balls (gamma-Al) with diameters of 3-5mm 2 O 3 ) The working solution enters from the bottom of the clay bed and flows out from the upper part of the clay bed through the activated alumina bed layer, thereby completing regeneration and regenerating partial degradation products of the working solution into effective anthraquinone.
The regeneration device has the following defects: 1. because the activated alumina balls are fixedly filled in the clay bed, the problems of low utilization rate and low regeneration efficiency of the activated alumina caused by uneven distribution and bias flow of working fluid in the clay bed are necessarily caused; 2. the porous structure arranged on the surface of the activated alumina ball causes that a large amount of working fluid is absorbed in the pores and is difficult to recycle, and each ton of activated alumina ball absorbs the working fluidThe liquid volume is about 0.5m 3 A set of hydrogen peroxide fixed bed process device with the volume of 10 ten thousand tons/year consumes 500 tons of active alumina each year, and the working solution lost by changing the active alumina each year is about 250m 3 The cost of the working solution is about 2 ten thousand yuan/m 3 The cost is increased by 50 yuan for each ton of hydrogen peroxide; 3. the diameter of the activated alumina sphere is larger, and the effective active ingredient (gamma-Al in the sphere 2 O 3 ) Is not fully used; 4. the waste activated alumina in the clay bed contains a large amount of organic matters, belongs to hazardous waste matters, causes great harm to the environment, is complex in subsequent treatment, has high treatment cost and increases the cost.
Disclosure of Invention
In order to solve the problems in the prior art, an object of an embodiment of the present application is to provide a regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by an anthraquinone process.
In order to achieve the above purpose, the technical scheme adopted in the application is as follows: provides a regeneration device of anthraquinone degradation products in the production of hydrogen peroxide by an anthraquinone process, which comprises the following steps: a working solution storage tank, a working solution pump, a preheater, a boiling bed, a regeneration filter and a hydrogenation reactor which are sequentially connected through a main pipeline; the fluidized bed is characterized in that miniature activated alumina balls are movably filled in the fluidized bed, the top of the regenerated filter is connected with a backwash pipe, the backwash pipe is connected with a working solution storage tank, a backwash pump is arranged on the backwash pipe, and a return pipe is arranged between the bottom of the regenerated filter and the bottom of the fluidized bed for communication.
In one embodiment, the ebullated bed is provided with at least two in parallel.
In one embodiment, a heat exchanger is provided on the main conduit between the filter and the hydrogenation reactor.
In one embodiment, a working fluid filter is provided on the main conduit between the heat exchanger and the hydrogenation reactor.
In one embodiment, the regeneration device of anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process further comprises a shunt pipe, one end of the shunt pipe is connected to the main pipeline between the working fluid pump and the preheater, and the other end of the shunt pipe is connected to the main pipeline between the heat exchanger and the working fluid filter.
In one embodiment, porous flowmeters are provided on both the main conduit and the shunt conduit.
In one embodiment, the micro activated alumina spheres have a diameter of 50 to 200 μm.
In one embodiment, the pre-heat temperature of the pre-heater is 60-90 ℃.
The regeneration device for anthraquinone degradation products in anthraquinone process hydrogen peroxide production has the beneficial effects that: the working solution flows through the working solution pump, is heated by the preheater and enters the boiling bed to be fully mixed with the micro activated alumina balls, so that the regeneration of anthraquinone degradation products is realized; because the miniature activated alumina balls are in an active state and the temperature is raised, the regeneration of the effective anthraquinone can be improved, the phenomenon of uneven regeneration distribution and bias flow of working solution can be effectively avoided, and the regeneration efficiency is improved; and simultaneously, the regenerated filter is backwashed through a backwash pump, a backwash pipe and a return pipe, so that the micro activated alumina balls can be ensured to reenter the boiling bed for use, the utilization rate of the micro activated alumina balls is improved, and the use amount of the micro activated alumina balls is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following description will briefly introduce the drawings that are needed in the embodiments or the description of the prior art, it is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a simplified schematic diagram of a prior art anthraquinone degradation product regeneration apparatus;
fig. 2 is a simplified schematic structural diagram of a regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process according to the embodiment of the present application.
Wherein, each reference sign in the figure:
1. a working solution storage tank; 2. a working fluid pump; 3. a preheater; 4. a ebullated bed; 5. regenerating the filter; 6. a heat exchanger; 7. a working fluid filter; 8. a hydrogenation reactor; 9. a backwash pump; 10. a backwashing pipe; 11. a return pipe; 12. a shunt; 13. a porous flow meter; 14. and a main pipeline.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved by the present application more clear, the present application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the present application.
It will be understood that when an element is referred to as being "mounted" or "disposed" on another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It is to be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present application and simplify description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be configured and operated in a particular orientation, and therefore should not be construed as limiting the present application.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Referring to FIG. 2, a device for regenerating degradation products of anthraquinone in the production of hydrogen peroxide by anthraquinone process will now be described. The regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by an anthraquinone process comprises the following steps: a working fluid storage tank 1, a working fluid pump 2, a preheater 3, a boiling bed 4, a regeneration filter 5, a heat exchanger 6, a working fluid filter 7 and a hydrogenation reactor 8.
The working solution storage tank 1 is connected with an alkali tower or a vacuum dehydration system, and the working solution from the extraction process is dehydrated by the alkali tower or the vacuum dehydration system and then directly enters the working solution storage tank 1.
Wherein, the working solution storage tank 1, the working solution pump 2, the preheater 3, the ebullated bed 4, the regeneration filter 5, the heat exchanger, the working solution filter 7 and the hydrogenation reactor 8 are sequentially connected through the main pipeline 14; wherein valves are arranged on the main pipelines 14 in the inlet direction and the outlet direction of the preheater 3, the boiling bed 4, the regeneration filter 5, the heat exchanger 6 and the working fluid filter 7. The working fluid enters from the bottom of the boiling bed 4 and flows out from the top; the micro activated alumina balls are movably filled in the boiling bed 4, and when the working fluid enters the boiling bed 4, the micro activated alumina balls are driven to stir, so that the fluid characteristic is formed, and the full contact between the working fluid and the micro activated alumina balls is ensured. The regeneration filter 5 is used for blocking the micro activated alumina balls carried out of the boiling bed 4 by the working fluid. The top of the regeneration filter 5 is connected with a backwash pipe 10, the backwash pipe 10 is connected with a working fluid storage tank 1, a backwash pump is arranged on the backwash pipe 10, and a return pipe 11 is arranged between the bottom of the regeneration filter 5 and the bottom of the ebullated bed 4 for communication; after a plurality of micro activated alumina balls are blocked in the regeneration filter 5, a valve in the outlet direction of the regeneration filter 5 is closed, a backwash pump is started, working fluid enters from the top of the regeneration filter 5 to backwash, and the micro activated alumina balls enter the boiling bed 4 again from the bottom of the boiling bed 4 through a return pipe 11 during backwash, so that the utilization rate of the micro activated alumina is improved.
The working fluid pump 2 is used for providing power for the flow of the working fluid in the main pipeline 14, the preheater 3 is used for heating the working fluid, and the working fluid after heating can improve the regeneration of effective anthraquinone; the micro active alumina balls movably filled in the boiling bed 4 are used for realizing the regeneration of the effective anthraquinone; the heat exchanger is used for cooling the regenerated working solution according to the requirement. The working fluid filter 7 filters the working fluid to prevent other impurities from entering the hydrogenation reactor 8.
In this embodiment, at least two ebullated beds 4 are arranged in parallel, and four ebullated beds 4 are arranged in parallel as shown in fig. 2, and the purpose of the ebullated beds 4 is to achieve on-line backwash without affecting the regeneration of the effective anthraquinones. For example: the valve in the outlet direction of one of the ebullated beds 4 is closed and then back flushing is performed; the rest of the ebullated bed 4 is working normally; and by analogy, each boiling bed 4 is backwashed one by one, so that the filtering effect and the flow rate of the regenerated filter 5 are ensured.
Preferably, the regeneration device of anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process further comprises a shunt tube 12, one end of the shunt tube 12 is connected to a main pipeline 14 between the working fluid pump 2 and the preheater 3, and the other end of the shunt tube 12 is connected to the main pipeline 14 between the heat exchanger 6 and the working fluid filter 7. The working solution flowing out of the working solution storage tank 1 is divided into two parts, one part (A part) enters the boiling bed 4 for regeneration after passing through the storage tank through the preheater 3, and the other part (B part) enters the hydrogenation reactor 8 after being directly filtered by the working solution filter 7 through the shunt pipe 12.
In this embodiment, porous flowmeters 13 are provided on both the main pipe 14 and the shunt pipe 12 for confirming the flow conditions of the working fluid in the main pipe 14 and the shunt pipe 12.
In this embodiment, the diameter of the micro activated alumina balls is 50-200 μm, so that the micro activated alumina balls are small in volume and can be fully utilized, thereby reducing the usage amount of activated alumina. Meanwhile, the surface of the miniature active alumina ball is smooth, and no porous structure is arranged, so that the loss of working fluid is avoided. Wherein, AL in the micro-active alumina balls 2 O 3 The content is more than or equal to 92 percent, ma 2 The O content is less than or equal to 0.5 percent, and the specific surface area is 150 to 180m 2 .g -1 The abrasion rate is less than or equal to 15 percent.
In this embodiment, the preheating temperature of the preheater 3 is 60 to 90 ℃.
In this embodiment, the working procedure is as follows: the working solution from the working solution storage tank 1 is split into two parts after being pressurized by the working solution pump 2, and one part of the working solution passes through the working solution filter 7 by the split pipe 12 and then directly enters the hydrogenation reactor 8 to carry out the hydrogenation process; the other working solution enters the boiling bed 4 from the bottom after being heated by the preheater 3 through the main pipeline 14, enters the boiling bed 4, is mixed with micro active alumina balls therein for regeneration, flows out from the top of the boiling bed 4, is filtered by the regeneration filter 5 to block the micro active alumina balls, then is subjected to heat exchange through the heat exchanger, and then is converged with the working solution flowing in the shunt pipe 12 before the working solution filter 7, and finally flows into the hydrogenation reactor 8. The working fluid storage tank 1 is back-flushed with a (C-stream) working fluid introduced through a back-flushing pipe 10 to regenerate the filter 5, and then re-enters the ebullated bed 4 through a back-flushing pipe 11.
In specific implementation, the flow rates of two working fluids (the main pipe 14 is the A strand and the shunt pipe 12 is the B strand) can be adjusted according to the working condition of the regeneration device, and if the working condition is poor (the regeneration amount is small), the flow rate of the working fluid passing through the ebullated bed 4 can be properly adjusted.
The ebullated bed 4 is based on the working fluid flowing from bottom to top, such that the micro activated alumina spheres are suspended to have fluid characteristics such that the working fluid is in sufficient contact with the micro activated alumina spheres. The control of the two flows is confirmed by the porous flowmeters which are respectively arranged, and then the opening of the valve on the corresponding pipeline is regulated.
In the embodiment, the fluidized bed 4 has high reverse efficiency compared with a fixed bed, so that the number of regenerated beds is reduced, the labor intensity of workers is lightened, the miniature activated alumina balls can not adsorb working fluid, the discharge of dangerous solid wastes is reduced, and good economic benefit is brought to hydrogen peroxide enterprises.
In the embodiment, after the temperature is raised and the ebullated bed 4 is regenerated, the active alumina consumption of the hydrogen peroxide device on the same scale is 70% less than that of the original regeneration process, the treatment capacity of the waste active alumina is reduced by 70%, the adsorption working fluid of the waste active alumina is reduced in the same ratio, and the economic and environmental benefits are obvious.
The foregoing description of the preferred embodiments of the present application is not intended to be limiting, but is intended to cover any and all modifications, equivalents, and alternatives falling within the spirit and principles of the present application.
Claims (8)
1. The regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by an anthraquinone process is characterized by comprising the following components: a working solution storage tank (1), a working solution pump (2), a preheater (3), a boiling bed (4), a regeneration filter (5) and a hydrogenation reactor (8) which are sequentially connected through a main pipeline (14); the fluidized bed is characterized in that micro activated alumina balls are movably filled in the fluidized bed (4), a backwash pipe (10) is connected to the top of the regeneration filter (5), the backwash pipe (10) is connected with the working solution storage tank (1), a backwash pump is arranged on the backwash pipe (10), and a return pipe (11) is arranged between the bottom of the regeneration filter (5) and the bottom of the fluidized bed (4) for communication.
2. The regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process according to claim 1, wherein: at least two boiling beds (4) are arranged in parallel.
3. The regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process according to claim 2, wherein: a heat exchanger (6) is arranged on the main pipe (14) between the filter and the hydrogenation reactor (8).
4. The regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process according to claim 3, wherein: and a working fluid filter (7) is arranged on the main pipeline (14) between the heat exchanger (6) and the hydrogenation reactor (8).
5. The regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process according to claim 4, wherein: the device further comprises a shunt pipe (12), one end of the shunt pipe (12) is connected to the main pipeline (14) between the working fluid pump (2) and the preheater (3), and the other end of the shunt pipe (12) is connected to the main pipeline (14) between the heat exchanger (6) and the working fluid filter (7).
6. The regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process according to claim 5, wherein: porous flowmeters (13) are arranged on the main pipeline (14) and the shunt pipe (12).
7. The regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process according to any one of claims 1 to 6, characterized in that: the diameter of the micro activated alumina balls is 50-200 mu m.
8. The regeneration device for anthraquinone degradation products in the production of hydrogen peroxide by the anthraquinone process according to claim 7, wherein: the preheating temperature of the preheater (3) is 60-90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321578434.0U CN220258054U (en) | 2023-06-20 | 2023-06-20 | Regeneration device for anthraquinone degradation products in anthraquinone process hydrogen peroxide production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321578434.0U CN220258054U (en) | 2023-06-20 | 2023-06-20 | Regeneration device for anthraquinone degradation products in anthraquinone process hydrogen peroxide production |
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| Publication Number | Publication Date |
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| CN220258054U true CN220258054U (en) | 2023-12-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202321578434.0U Active CN220258054U (en) | 2023-06-20 | 2023-06-20 | Regeneration device for anthraquinone degradation products in anthraquinone process hydrogen peroxide production |
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| CN (1) | CN220258054U (en) |
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- 2023-06-20 CN CN202321578434.0U patent/CN220258054U/en active Active
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