CN206676347U - A kind of inner circulation fluidized bed reaction device of anthraquinone legal system hydrogen peroxide gas-liquid-solid three-phase - Google Patents
A kind of inner circulation fluidized bed reaction device of anthraquinone legal system hydrogen peroxide gas-liquid-solid three-phase Download PDFInfo
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- CN206676347U CN206676347U CN201720178903.8U CN201720178903U CN206676347U CN 206676347 U CN206676347 U CN 206676347U CN 201720178903 U CN201720178903 U CN 201720178903U CN 206676347 U CN206676347 U CN 206676347U
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Abstract
The utility model discloses a kind of inner circulation fluidized bed reaction device of anthraquinone legal system hydrogen peroxide gas-liquid-solid three-phase, reactor shell bottom is provided with circulating air import, working solution import, middle and upper part exports provided with multiple circulation fluids, top is exported provided with circulating air, and tower inner draft tube is provided with inside reactor shell.Guide shell is provided with concentric circulating air distributor pipe between reactor shell.A circle working solution charging distributor pipe is provided with the top of circulating air distributor pipe, guide shell bottom is provided with reaction solution outlet and removes outer circulation cooling device, the middle and upper part of (conversion zone) is provided with concentric circulating cooling liquid import distribution endless tube between guide shell and reactor shell, and the reaction solution after cooling comes back to reactor by being distributed cooling ring vessel.Middle and upper part is provided with closed hydrogenation agent feeding device.The utility model can solve the technical problems such as low production efficiency, poor product quality, unit product production consumption is high, production equipment is heavy, big, the production operation security difference of investment.
Description
Technical field
It the utility model is related to gas-liquid-solid three-phase fluid bed reactor, and in particular to a kind of gas of anthraquinone legal system hydrogen peroxide
The solid three phase inner circulation fluidized bed reactor assembly of liquid.
Background technology
In the prior art, the preparation of hydrogen peroxide is typically realized by anthraquinone.It is anthraquinone using 2- EAQs as
Carrier, palladium (or nickel) is catalyst, by H2And O2Directly it is combined to H2O2.It is divided into four hydrogenation, oxidation, extraction, post processing works
Sequence.
Hydrogenation process therein typically uses fixed-bed process, pungent with heavy aromatics, four tricresyl phosphates using alkyl-anthraquinone as carrier
Fat is that solvent forms working solution.Working solution in the presence of certain pressure, temperature and catalyst, with hydrogen hydrogenate instead
Should, solution (abbreviation hydride) of the generation containing corresponding alkyl hydrogen anthraquinone.Its reaction equation is as follows：
Fixed bed reactors carry out anthraquinones hydrogenation, although yield is larger, also show low production efficiency,
Poor product quality, unit product production consumption height, heavy, big, the production operation security difference of investment of production equipment etc. are more to be lacked
Point.
The content of the invention
The purpose of this utility model in provide it is a kind of using three phase fluidized bed for the anthracene in anthraquinone legal system hydrogen peroxide
The gas-liquid-solid three-phase fluidized bed reactor that quinone is hydrogenated, produced with solving low production efficiency, poor product quality, unit product
The technical problems such as consumption is high, production equipment is heavy, big, the production operation security difference of investment.
To achieve these goals, the technical solution adopted in the present invention is as follows：
A kind of anthraquinone legal system hydrogen peroxide inside circulation triphase fluidized bed reactor, including reactor shell and inside reactor
Component；Reactor shell bottom is provided with working solution import (13), and circulating air import (10) is arranged below in working solution import (13), in
Top is provided with multiple hydride discharging openings (14), and top is provided with circulating air outlet (17), is provided with inside reactor shell and follows certainly
Ring liquid inner draft tube (4), the frid (3) of annular is fixed with along inwall in reactor internal upper part, annular frid (3) bottom is opened
There are 6~20 outages, annular frid (3) medium design gas passage, passage top is provided with umbellate form baffle plate (2), umbellate form
Demister (1) is provided with above baffle plate (2), the flushing liquor distribution apparatus (16) of anti-anthraquinone condensation is provided with above demister (1),
Self-loopa liquid inner draft tube (4) below the frid (3) of annular, the inwall different height of guide shell be provided with 6~12 groups of metals or
The built-in membrane tube filter (8) of ceramics, 2~3 circles that are provided between reactor shell of self-loopa liquid inner draft tube (4) circulate
Nitrogen hydrogen is distributed endless tube (12) with one heart, and the top for being distributed endless tube (12) with one heart in cyclic nitrogen hydrogen is provided with a circle and working solution import
(13) the working solution charging distributor pipe (9) of connection, self-loopa liquid inner draft tube (4) top is provided with 6~12 groups of reaction solution discharge rings
Manage (5), reaction solution outlet endless tube (5) merges adjusted rear discharging by 6~12 groups of hydride discharging openings (14)；Self-loopa
The middle and upper part of conversion zone of the liquid inner draft tube (4) between reactor shell is provided with circulating cooling liquid import distribution endless tube (6), by
Enter hydride outer circulation cooler (7), the hydrogen after cooling after hydrogenated liquid outer circulation cooling pump (11) pressurization of reactor bottom
Change liquid and reactor is come back to by circulating cooling liquid import distribution endless tube (6), effective controlling reaction temperature is come with this；
The top of reactor shell is provided with closed catalyst feeder (15)；Three reactions of gas-liquid-solid are in self-loopa liquid inner draft tube
(4) the reaction zone reaction between reactor enclosure body wall, it is gas-liquid separation circulating reflux area that self-loopa liquid inner draft tube (4) is interior,
It is downward through self-loopa liquid inner draft tube containing catalyst liquid from reaction zone, then enter reaction zone in the presence of air lift, formed from
Circulating reaction system.
Built-in membrane tube filter (8) is provided with self-loopa liquid inner draft tube (4).
Outer circulation cooling device includes hydride outer circulation cooling pump (11) and hydride outer circulation cooler (7).
The advantages of the utility model, is as follows：Hydrogenation fluidized-bed process of the fluidized-bed reactor for anthraquinone legal system hydrogen peroxide
Good Equipment Foundations are provided, the inner draft tube of inside reactor and built-in film filter can accelerate reaction rate, and greatly
Raising catalyst utilization rate and efficiency, external circulation fluid pipe heat exchanger being capable of effective controlling reaction temperature.Using this
The solution-air solid three-phase fluid bed reactor of utility model coordinates related hydrogenation process, can be in existing domestic fixed bed hydrogenation technique
On the basis of improve production efficiency 30~40%, and production principle and technique substantially solve production in hazards,
Product design can be made to improve more than 40% by 30%, and product quality leading indicator such as organic carbon content, nonvolatile matter contain
Amount etc. is better than the product that fixed-bed process is produced.
Brief description of the drawings
Fig. 1 is the structural representation of fluidized-bed reactor of the present utility model.
Numbered in figure：1. demister, 2. umbellate form baffle plates, the frid of 3. annulars, 4. self-loopa liquid inner draft tubes, 5. reaction solutions
Export endless tube, 6. circulating cooling liquid imports distribution endless tube, 7. hydride outer circulation coolers, 8. built-in membrane tube filters (one
Level filtering), 9. working solutions charging distribution endless tube, 10. circulating air imports, 11. hydride outer circulation cooling pumps, 12. circulation (nitrogen
Hydrogen) gas is distributed endless tube with one heart, and 13. working solution imports, 14. hydride discharging openings, 15. closed catalyst feeders, 16. rinse
Liquid distribution apparatus, the outlet of 17 circulating air.
Embodiment
Hereinafter, be described further in conjunction with the embodiments with accompanying drawing for the utility model, embodiment be only used for explain without
For limiting the scope of protection of the utility model.Upper and lower, left and right in embodiment are relative position rather than absolute position.
The fluidized-bed reactor structure of the present embodiment is as follows：
As shown in figure 1, a kind of anthraquinone legal system hydrogen peroxide inside circulation triphase fluidized bed reactor, including reactor shell and
Reactor internal components；Reactor shell bottom is provided with working solution import (13), and circulating air is arranged below in working solution import (13)
Import (10), middle and upper part are provided with multiple hydride discharging openings (14), and top is provided with circulating air outlet (17), it is characterised in that
Self-loopa liquid inner draft tube (4) is provided with inside reactor shell, the annular of annular is fixed with along inwall in reactor internal upper part
Frid (3), annular frid (3) bottom are provided with 6~20 outages, and annular frid (3) medium design gas passage, this is logical
Umbellate form baffle plate (2) is provided with above road, demister (1) is provided with above baffle plate, anti-anthraquinone condensation is provided with above demister (1)
Flushing liquor distribution apparatus (16), for self-loopa liquid inner draft tube (4) below the frid (3) of annular, the inwall of guide shell is different high
Degree provided with 6~12 groups of metals or the built-in membrane tube filter (8) of ceramics, self-loopa liquid inner draft tube (4) and reactor shell
Between be provided with 2~3 circle cyclic nitrogen hydrogen be distributed endless tube (12) with one heart, be distributed above endless tube (12) and set with one heart in cyclic nitrogen hydrogen
There is a circle working solution to feed distributor pipe (9), self-loopa liquid inner draft tube (4) top is provided with 6~12 groups of reaction solutions and exports endless tube
(5), reaction solution outlet endless tube (5) merges adjusted rear discharging by 6~12 groups of hydride discharging openings (14)；Self-loopa liquid
The middle and upper part of conversion zone of the inner draft tube (4) between reactor shell is provided with concentric circulating cooling liquid import distribution endless tube (6),
By entering hydride outer circulation cooler (7) after hydrogenated liquid outer circulation cooling pump (11) pressurization of reactor bottom, after cooling
Hydride comes back to reactor by being distributed cooling ring vessel, carrys out effective controlling reaction temperature with this；In the upper of reactor shell
Portion is provided with closed catalyst feeder (15)；Three reactions of gas-liquid-solid are in self-loopa liquid inner draft tube (4) and reactor shell
Reaction zone reaction between wall, is gas-liquid separation circulating reflux area in self-loopa liquid inner draft tube, containing catalyst liquid from reaction
Area, it is downward through self-loopa liquid inner draft tube, then enter reaction zone in the presence of air lift, form self-loopa reaction system；
Lower method can be used using the hydrogenation process of this reactor：The anthraquinone working solution one that will be dissolved in working material
Or multiple imports are sent into fluidized-bed reactor by reactor bottom, are mixed hydrogen or nitrogen hydrogen by least one other entrance
Close gas and be sent into liquefied bed bottom, gaseous mixture, working solution and catalyst three-phase cocurrent are upward in the reactor, therebetween with working solution
Mutually mixed in a fluidized bed reactor with catalyst, in the presence of hydrogen recycle compressor air lift, hydrogen, working solution is in catalyst
In the presence of rise and react between guide shell and reactor shell, gas phase separates in tower head with guide shell epimere, liquid-solid two-phase
Reaction zone is downwardly into by middle guide shell, working solution self-loopa hydrogenation reaction is so formed, so as to be dissolved in working solution
Anthraquinone, hydrogen react generation hydrogen anthraquinone in the presence of catalyst, which part hydride is by gas-liquid separation, filtering, cold
But enter hydride degassing tank, prepare the redox reaction of next process, most of recirculate is returned from inner draft tube bottom
Hydrogenation is participated in again in reaction zone.Hydrogen and nitrogen mixture therein are in reactor head through separating, condensing, dividing again
From, filtering enter reactor bottom pair in the lump with fresh supplemented hydrogen or nitrogen after hydrogen recycle compressor pressurizes again again
Working solution and catalyst mixed liquid in reactor are carried out fluidizing stirring and reacted.From reactor bottom extraction part hydride warp
Hydride circulating pump, tubular heat exchanger come back to inside reactor, and so reactor reaction temperature effectively can be controlled
System.
Claims (3)
1. a kind of inner circulation fluidized bed reaction device of anthraquinone legal system hydrogen peroxide gas-liquid-solid three-phase, including reactor shell and reaction
Device internals；Reactor shell bottom is provided with working solution import (13), and circulating air import is arranged below in working solution import (13)
(10), middle and upper part is provided with multiple hydride discharging openings (14), and top is provided with circulating air outlet (17), it is characterised in that is reacting
Device enclosure interior is provided with self-loopa liquid inner draft tube (4), is fixed with the frid (3) of annular, ring along inwall in reactor internal upper part
Frid (3) bottom of type is provided with 6~20 outages, annular frid (3) medium design gas passage, and passage top is provided with
Umbellate form baffle plate (2), demister (1) is provided with above umbellate form baffle plate (2), rushing for anti-anthraquinone condensation is provided with above demister (1)
Wash liquid distribution device (16), self-loopa liquid inner draft tube (4) is below the frid (3) of annular, the inwall different height of guide shell
Provided with 6~12 groups of metals or ceramics built-in membrane tube filter (8), self-loopa liquid inner draft tube (4) and reactor shell
Between be provided with 2~3 circle cyclic nitrogen hydrogen be distributed endless tube (12) with one heart, be distributed above endless tube (12) and set with one heart in cyclic nitrogen hydrogen
There is the working solution charging distributor pipe (9) that a circle is connected with working solution import (13), self-loopa liquid inner draft tube (4) top is provided with 6
~12 groups of reaction solution outlet endless tubes (5), reaction solution outlet endless tube (5) merge warp by 6~12 groups of hydride discharging openings (14)
Discharged after regulation；The middle and upper part of conversion zone of the self-loopa liquid inner draft tube (4) between reactor shell is provided with circulating cooling liquid
Import distribution endless tube (6), it is cold by entering hydride outer circulation after hydrogenated liquid outer circulation cooling pump (11) pressurization of reactor bottom
But device (7), the hydride after cooling are distributed endless tube (6) by the circulating cooling liquid import and come back to reactor, come with this
Effective controlling reaction temperature；Closed catalyst feeder (15) is provided with the top of reactor shell；Three reactions of gas-liquid-solid
Reaction zone reaction between self-loopa liquid inner draft tube (4) and reactor enclosure body wall, it is gas that self-loopa liquid inner draft tube (4) is interior
Liquid separation circulating reflux area, it is downward through self-loopa liquid inner draft tube containing catalyst liquid from reaction zone, then in the presence of air lift
Into reaction zone, self-loopa reaction system is formed.
2. a kind of inner circulation fluidized bed reaction device of anthraquinone legal system hydrogen peroxide gas-liquid-solid three-phase as claimed in claim 1, its
It is characterised by, built-in membrane tube filter (8) is provided with self-loopa liquid inner draft tube (4).
3. a kind of inner circulation fluidized bed reaction device of anthraquinone legal system hydrogen peroxide gas-liquid-solid three-phase as claimed in claim 1, its
It is characterised by, outer circulation cooling device includes hydride outer circulation cooling pump (11) and hydride outer circulation cooler (7).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720178903.8U CN206676347U (en) | 2017-02-27 | 2017-02-27 | A kind of inner circulation fluidized bed reaction device of anthraquinone legal system hydrogen peroxide gas-liquid-solid three-phase |
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| CN201720178903.8U CN206676347U (en) | 2017-02-27 | 2017-02-27 | A kind of inner circulation fluidized bed reaction device of anthraquinone legal system hydrogen peroxide gas-liquid-solid three-phase |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675265A (en) * | 2018-07-05 | 2018-10-19 | 浙江工程设计有限公司 | A kind of after-treatment device of process for prepairng hydrogen peroxide by anthraquinone technique |
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2017
- 2017-02-27 CN CN201720178903.8U patent/CN206676347U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675265A (en) * | 2018-07-05 | 2018-10-19 | 浙江工程设计有限公司 | A kind of after-treatment device of process for prepairng hydrogen peroxide by anthraquinone technique |
| CN108675265B (en) * | 2018-07-05 | 2023-09-15 | 浙江工程设计有限公司 | Post-treatment device for hydrogen peroxide production process by anthraquinone process |
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