CN111410176A - Hydrogenation tower tubular reactor for producing hydrogen peroxide - Google Patents

Hydrogenation tower tubular reactor for producing hydrogen peroxide Download PDF

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Publication number
CN111410176A
CN111410176A CN202010405205.3A CN202010405205A CN111410176A CN 111410176 A CN111410176 A CN 111410176A CN 202010405205 A CN202010405205 A CN 202010405205A CN 111410176 A CN111410176 A CN 111410176A
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CN
China
Prior art keywords
tubular reactor
hydrogenation
hydrogen peroxide
hydrogenation tower
tower
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Pending
Application number
CN202010405205.3A
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Chinese (zh)
Inventor
李琪
吴道斌
瞿亚平
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Fujian Eversun Technology Co ltd
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Fujian Eversun Technology Co ltd
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Priority to CN202010405205.3A priority Critical patent/CN111410176A/en
Publication of CN111410176A publication Critical patent/CN111410176A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/01Hydrogen peroxide
    • C01B15/022Preparation from organic compounds
    • C01B15/023Preparation from organic compounds by the alkyl-anthraquinone process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The invention provides a hydrogenation tower tubular reactor for producing hydrogen peroxide. The hydrogenation tower tubular reactor for producing the hydrogen peroxide comprises a hydrogenation tower; the two pore plates are fixedly arranged in the hydrogenation tower, and a space is arranged between the two pore plates; the gas-liquid distributor is arranged in the hydrogenation tower and is positioned above the pore plate; a plurality of tubular reactors mounted between two of the orifice plates; the liquid outlet pipe is arranged at the bottom side of the hydrogenation tower and communicated with the interior of the hydrogenation tower; the liquid inlet pipe is arranged on the top side of the hydrogenation tower and communicated with the interior of the hydrogenation tower. The hydrogenation tower tubular reactor for producing hydrogen peroxide provided by the invention has the advantages of preventing bias flow and having high heat exchange efficiency.

Description

Hydrogenation tower tubular reactor for producing hydrogen peroxide
Technical Field
The invention relates to the technical field of hydrogen peroxide production, in particular to a tubular reactor of a hydrogenation tower for producing hydrogen peroxide.
Background
The production process of hydrogen peroxide is mainly a palladium catalyst anthraquinone process, and the domestic production process of hydrogen peroxide by the palladium catalyst anthraquinone process comprises five procedures of hydrogenation, oxidation, extraction, purification and post-treatment.
The structure of the domestic original hydrogenation tower is shown in figure 6: the working liquid and hydrogen enter from the upper part of the hydrogenation tower, gas and liquid are uniformly distributed through a gas-liquid distributor, the liquid trickles to a catalyst layer in the tower, under the catalytic action of a palladium catalyst, 2-ethyl anthraquinone in the working liquid and the hydrogen undergo hydrogenation reaction under the catalytic action of the palladium catalyst to generate anthraquinone, the anthraquinone undergoes oxidation reaction to generate hydrogen peroxide, and the hydrogen peroxide is extracted by desalted water in an extraction tower to form a hydrogen peroxide product.
When the catalyst of the hydrogenation tower is filled, a layer of ceramic balls, a layer of palladium catalyst and a layer of ceramic balls are used for jacking, the catalyst is naturally accumulated, and gas and liquid which are excessively high in accumulation form bias flow on the catalyst layer, so that local excessive reaction is caused, the catalyst is agglomerated, and the service life and the production of the catalyst are influenced.
The catalyst has good activity in the early stage of use, needs low reaction temperature, needs a working fluid heat exchanger to be filled with circulating water for cooling, has poor activity in the later stage, needs high reaction temperature, and needs a working fluid heat exchanger to be filled with steam for heating.
In the practical application process, in order to avoid bias flow, a common method is to take 2 meters as one layer of catalyst, divide the catalyst into two to three layers in a tower, and add a redistributor in the middle to prevent bias flow. However, this approach increases the height of the tower invisibly, and has high requirements for the redistributor, and there will still be bias flow of different degrees during the use, resulting in that the catalyst activity can not be fully exerted, or the service life is shortened.
Therefore, there is a need to provide a new hydrogenation column tubular reactor for producing hydrogen peroxide to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a hydrogenation tower tubular reactor for producing hydrogen peroxide, which can prevent bias current and has high heat exchange efficiency.
In order to solve the above technical problems, the present invention provides a hydrogenation column tubular reactor for producing hydrogen peroxide, comprising:
a hydrogenation column;
the two pore plates are fixedly arranged in the hydrogenation tower, and a space is arranged between the two pore plates;
the gas-liquid distributor is arranged in the hydrogenation tower and is positioned above the pore plate;
a plurality of tubular reactors mounted between two of the orifice plates;
the liquid outlet pipe is arranged at the bottom side of the hydrogenation tower and communicated with the interior of the hydrogenation tower;
the liquid inlet pipe is arranged on the top side of the hydrogenation tower and communicated with the interior of the hydrogenation tower.
Preferably, a plurality of trepanning are formed in the pore plate, the trepanning is in sealed sleeve joint with the tubular reactor, the top end of the tubular reactor penetrates through the corresponding trepanning and extends to the position above the pore plate located above, and the bottom end of the tubular reactor penetrates through the corresponding trepanning and extends to the position below the pore plate located below.
Preferably, a catalyst is filled in the tubular reactor, ceramic balls are paved on the top side and the bottom side of the catalyst, wire meshes are arranged between the ceramic balls and the catalyst and on the side, away from the catalyst, of the ceramic balls, and a grid is arranged between the pore plate below and the wire meshes.
Preferably, the number of the tubular reactors is the same as that of the trepanning, and the tubular reactors are connected with the pore plate through fastening bolts.
Preferably, the top end of the hydrogenation tower is provided with a vent pipe, and the vent pipe is communicated with the interior of the hydrogenation tower.
Preferably, a collector is arranged at the bottom side of the interior of the hydrogenation tower and is communicated with the liquid outlet pipe.
Preferably, the outer wall of the hydrogenation tower is provided with a seal head which is connected by a large flange bolt.
Preferably, a first horizontal conduit and a second horizontal conduit are respectively installed on the inner wall of the hydrogenation tower between the two pore plates, the first horizontal conduit and the second horizontal conduit both extend out of the hydrogenation tower, and the horizontal height of the first horizontal conduit is higher than that of the second horizontal conduit.
Preferably, two fixing rings are fixedly installed in the tubular reactor, the two fixing rings are respectively contacted with the two wire meshes on the top side and the bottom side of the catalyst, a pressure pipe is installed on the top side of the tubular reactor through threads, and the bottom end of the pressure pipe extends into the tubular reactor and is contacted with the uppermost wire mesh.
Preferably, the bottom side of the tubular reactor is threadedly provided with a sleeve, the top side of the sleeve extends into the tubular reactor and is in contact with the wire mesh positioned at the lowest part, and the grid is arranged in the sleeve.
Compared with the related art, the tubular reactor of the hydrogenation tower for producing hydrogen peroxide provided by the invention has the following beneficial effects:
the invention provides a tubular reactor of a hydrogenation tower for producing hydrogen peroxide, wherein the tubular reactor is arranged in the hydrogenation tower, so that working solution and hydrogen are contacted with a catalyst in a small-diameter pipeline to prevent bias flow; circulating water or steam can be introduced outside the tubular reactor for direct heat exchange, so that the efficiency is higher, and the generation of degradation products can be reduced under constant-temperature reaction conditions.
Drawings
FIG. 1 is a schematic structural diagram of a tubular reactor of a hydrogenation tower for producing hydrogen peroxide according to a preferred embodiment of the present invention;
FIG. 2 is a schematic view of the structure of the tubular reactor shown in FIG. 1;
FIG. 3 is a schematic top view of the orifice plate shown in FIG. 1;
FIG. 4 is a schematic structural diagram of a second embodiment of a hydrogenation column tubular reactor for producing hydrogen peroxide according to the present invention;
FIG. 5 is a schematic view of the combination of the sleeve and the grid of FIG. 4;
FIG. 6 is a schematic diagram of the prior art hydrogenation tower, in which the tower has two catalyst layers, each of which is, from top to bottom: distributor, 300mm porcelain ball, clamping ring, 14 mesh screen, palladium catalyst, clamping ring, 14 mesh screen, 300mm porcelain ball, 4 mesh screen, grid plate.
Reference numbers in the figures: 1. a hydrogenation column; 2. an orifice plate; 3. a grid; 4. a wire mesh; 5. a catalyst; 6. a gas-liquid distributor; 7. a porcelain ball; 8. a tubular reactor; 9. a liquid outlet pipe; 10. a liquid inlet pipe; 11. an emptying pipe; 12. fastening a bolt; 13. a collector; 14. sealing the end; 15. trepanning; 16. a first horizontal conduit; 17. a second horizontal conduit; 18. a fixing ring; 19. a sleeve; 20. and (5) pressing the pipe.
Detailed Description
The invention is further described with reference to the following figures and embodiments.
The first embodiment:
referring to fig. 1 to 3 in combination, in a first embodiment of the present invention, a hydrogenation column tubular reactor for producing hydrogen peroxide includes: a hydrogenation column 1;
the two pore plates 2 are fixedly arranged in the hydrogenation tower 1, and a gap is arranged between the two pore plates 2;
the gas-liquid distributor 6 is installed in the hydrogenation tower 1, and the gas-liquid distributor 6 is positioned above the orifice plate 2;
a plurality of tubular reactors 8, the tubular reactors 8 being mounted between two of the perforated plates 2;
the liquid outlet pipe 9 is arranged at the bottom side of the hydrogenation tower 1, and the liquid outlet pipe 9 is communicated with the interior of the hydrogenation tower 1;
the liquid inlet pipe 10 is arranged on the top side of the hydrogenation tower 1, and the liquid inlet pipe 10 is communicated with the interior of the hydrogenation tower 1.
A plurality of trepanning 15 have been seted up on orifice plate 2, trepanning 15 with tubular reactor 8 is sealed to be cup jointed, tubular reactor 8's top is run through the correspondence trepanning 15 extends to the top that is located the orifice plate 2 of top, tubular reactor 8's bottom is run through the correspondence trepanning 15 extends to the below that is located the orifice plate 2 of below, and many tubular reactor 8 are parallel all with the distribution, increase reaction area of contact for reaction rate.
The tubular reactor 8 is internally provided with a catalyst 5, ceramic balls 7 are respectively paved on the top side and the bottom side of the catalyst 5, wire nets 4 are respectively arranged between the ceramic balls 7 and the catalyst 5 and on the side, away from the catalyst 5, of the ceramic balls 7, a grid 3 is arranged between the pore plate 2 and the wire nets 4 positioned below, and no space capable of deflecting working solution and hydrogen enters the grid, so that the deflecting is effectively prevented, the utilization rate of the catalyst 5 is improved, and the filling amount of the catalyst 5 can be reduced; the heat exchange medium outside the tubular reactor 8 can directly act circulating water or steam on the catalyst, the heat exchange effect is more efficient and direct, energy can be effectively saved, the constant temperature of the whole tower is more favorable for the catalyst 5 to react under mild reaction conditions, and the generation of degradation products is reduced.
The number of the tubular reactors 8 is the same as that of the trepanning 15, the tubular reactors 8 are connected with the pore plate 2 through fastening bolts 12, and the diameter of the trepanning 15 is 200 mm.
And a vent pipe 11 is arranged at the top end of the hydrogenation tower 1, and the vent pipe 11 is communicated with the interior of the hydrogenation tower 1.
The bottom side of the interior of the hydrogenation tower 1 is provided with a collector 13, the collector 13 is communicated with the liquid outlet pipe 9, and the collector 13 is used for preventing solid impurities from entering the liquid outlet pipe 9.
And a seal head 14 is arranged on the outer wall of the hydrogenation tower 1, and the seal head 14 is connected by a large flange bolt.
The four screen meshes 4 are respectively a 4-mesh screen mesh, a 14-mesh screen mesh and a 4-mesh screen mesh from top to bottom.
A first horizontal conduit 16 and a second horizontal conduit 17 are respectively arranged on the inner wall of the hydrogenation tower 1 between the two pore plates 2, the first horizontal conduit 16 and the second horizontal conduit 17 both extend out of the hydrogenation tower 1, the level of the first horizontal conduit 16 is higher than that of the second horizontal conduit 17, the first horizontal conduit 16 can be used for leading cooling water out and leading steam in, the second horizontal conduit 17 can be used for leading cooling water in and leading steam out, because the cooling water enters the hydrogenation tower 1 from the second horizontal conduit 17 and then flows out from the first horizontal conduit 16, the cooling water can fill the inside of the hydrogenation tower 1, the steam has low density, therefore, the cooling water needs to enter from the first horizontal conduit 16 and flow out from the second horizontal conduit 17, the outside of the tubular reactor 8 can directly exchange heat with circulating water or steam, the generation of degradation products can be reduced under more efficient and constant temperature reaction conditions, circulating water or steam can be led outside the pipeline reactor 8 of the hydrogenation tower 1, circulating water or steam can be led to for temperature prevention or steam heating can be selected according to different activities of the catalyst 5 and the required temperature, heat exchange directly acts on the catalyst 5, and the heat exchanger is more efficient than an original external working solution heat exchanger.
The working principle of the hydrogenation tower tubular reactor for producing hydrogen peroxide provided by the invention is as follows:
the working liquid and hydrogen are distributed by a gas-liquid distributor at the top of the tower and then drip to a lower ceramic ball, and contact reaction is carried out on the working liquid and the hydrogen and a catalyst below the working liquid after the working liquid and the hydrogen are buffered by the ceramic ball to generate hydrogenated liquid. In order to avoid the condition, the prior art uses catalyst to be filled layer by layer, each layer is filled to be no more than two meters, then a redistributor is arranged below each layer, and because the redistributor and a separation space below the redistributor need to have a certain layer height, ineffective space of a hydrogenation tower is reduced, and a bias flow phenomenon still exists. In order to control the hydrogenation reaction, the working liquid entering the tower can be subjected to temperature control according to the activity of the catalyst, and the adopted method is that a heat exchanger is added before the working liquid enters the hydrogenation tower, and circulating water or steam is introduced into the heat exchanger according to the required reaction temperature (40-70 ℃).
Compared with the related art, the tubular reactor of the hydrogenation tower for producing hydrogen peroxide provided by the invention has the following beneficial effects:
the invention provides a tubular reactor of a hydrogenation tower for producing hydrogen peroxide, wherein a tubular reactor 8 is arranged in a hydrogenation tower 1, so that working solution and hydrogen are contacted with a catalyst 5 in a small-diameter pipeline to prevent bias flow; circulating water or steam can be introduced outside the tubular reactor 8 for direct heat exchange, so that the efficiency is higher, and the generation of degradation products can be reduced under the constant-temperature reaction condition.
Second embodiment:
based on the hydrogenation tower tubular reactor for producing hydrogen peroxide provided in the first embodiment of the present application, the second embodiment of the present application proposes another hydrogenation tower tubular reactor for producing hydrogen peroxide. The second embodiment is merely a preferred way of the first embodiment, and the implementation of the second embodiment does not affect the implementation of the first embodiment alone.
The second embodiment of the present invention will be further described with reference to the drawings and the following description.
Referring to fig. 4-5, this embodiment is different from the first embodiment in that two fixing rings 18 are fixedly installed in the tubular reactor 8, the two fixing rings 18 are respectively in contact with the two wire nets 4 on the top and bottom sides of the catalyst 5, the top side of the tubular reactor 8 is threadedly installed with a pressure pipe 20, and the bottom end of the pressure pipe 20 extends into the tubular reactor 8 and is in contact with the uppermost wire net 4.
The bottom side of the tubular reactor 8 is threadedly fitted with a sleeve 19, the top side of the sleeve 19 extends into the tubular reactor 8 and contacts the lowermost wire mesh 4, and the grid 3 is fitted within the sleeve 9.
When the porcelain ball 7 or the catalyst 5 needs to be replaced or the silk screen 4 needs to be disassembled and cleaned, the tubular reactor 8 is only required to be taken down from the two pore plates 2, the sleeve 19 is unscrewed, and the pressure pipe 20 is pressed, so that the silk screen 4, the porcelain ball 7 and the catalyst 5 can be disassembled and replaced, the operation is convenient, and the disassembly and the assembly are convenient.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. A hydrogenation column tube reactor for producing hydrogen peroxide, comprising:
a hydrogenation column;
the two pore plates are fixedly arranged in the hydrogenation tower, and a space is arranged between the two pore plates;
the gas-liquid distributor is arranged in the hydrogenation tower and is positioned above the pore plate;
a plurality of tubular reactors mounted between two of the orifice plates;
the liquid outlet pipe is arranged at the bottom side of the hydrogenation tower and communicated with the interior of the hydrogenation tower;
the liquid inlet pipe is arranged on the top side of the hydrogenation tower and communicated with the interior of the hydrogenation tower.
2. The tubular reactor of hydrogenation tower for producing hydrogen peroxide according to claim 1, wherein the perforated plate has a plurality of holes, the holes are hermetically sleeved with the tubular reactor, the top end of the tubular reactor penetrates through the corresponding holes and extends to the upper part of the perforated plate located above, and the bottom end of the tubular reactor penetrates through the corresponding holes and extends to the lower part of the perforated plate located below.
3. A hydrogenation tower tubular reactor for producing hydrogen peroxide as claimed in claim 1, wherein the tubular reactor is filled with catalyst, ceramic balls are laid on the top and bottom sides of the catalyst, wire mesh is arranged between the ceramic balls and the catalyst and on the side of the ceramic balls far away from the catalyst, and a grid is arranged between the lower hole plate and the wire mesh.
4. A hydrogenation column tubular reactor for producing hydrogen peroxide according to claim 2, characterized in that the number of tubular reactors is the same as the number of said trepan boring, and said tubular reactors are connected with the orifice plate by fastening bolts.
5. A hydrogenation column pipe reactor for producing hydrogen peroxide according to claim 1, characterized in that the top end of the hydrogenation column is equipped with a blow pipe, which communicates with the interior of the hydrogenation column.
6. A hydrogenation column tube reactor for producing hydrogen peroxide according to claim 1, characterized in that a collector is installed at the bottom side of the interior of the hydrogenation column, and the collector is communicated with the liquid outlet pipe.
7. The tubular reactor for the hydrogenation tower for producing hydrogen peroxide according to claim 1, wherein the outer wall of the hydrogenation tower is provided with a head, and the head is connected by a large flange bolt.
8. A hydrogenation tower tubular reactor for producing hydrogen peroxide as claimed in claim 1, wherein the inner wall of the hydrogenation tower between the two perforated plates is respectively provided with a first horizontal conduit and a second horizontal conduit, the first horizontal conduit and the second horizontal conduit both extend out of the hydrogenation tower, and the level of the first horizontal conduit is higher than that of the second horizontal conduit.
9. A hydrogenation column tubular reactor for producing hydrogen peroxide according to claim 3, wherein two fixing rings are fixedly installed in the tubular reactor, the two fixing rings are respectively in contact with the two wire nets on the top and bottom sides of the catalyst, the top side of the tubular reactor is threadedly installed with a pressing pipe, and the bottom end of the pressing pipe extends into the tubular reactor and is in contact with the wire net positioned uppermost.
10. A hydrogenation column tubular reactor for the production of hydrogen peroxide according to claim 3, characterized in that the bottom side of the tubular reactor is threadedly fitted with a sleeve, the top side of the sleeve extending into the tubular reactor and contacting the wire mesh located lowermost, the grid being fitted within the sleeve.
CN202010405205.3A 2020-05-14 2020-05-14 Hydrogenation tower tubular reactor for producing hydrogen peroxide Pending CN111410176A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010405205.3A CN111410176A (en) 2020-05-14 2020-05-14 Hydrogenation tower tubular reactor for producing hydrogen peroxide

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CN202010405205.3A CN111410176A (en) 2020-05-14 2020-05-14 Hydrogenation tower tubular reactor for producing hydrogen peroxide

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9001802D0 (en) * 1989-01-27 1990-03-28 Kemira Oy A process for the preparation of hydrogen peroxide
CN102161475A (en) * 2009-11-02 2011-08-24 郑国玉 Concentration method in production of hydrogen peroxide by anthraquinone method
WO2011134345A1 (en) * 2010-04-29 2011-11-03 扬州惠通化工技术有限公司 Hydrogenating system for producing hydrogen peroxide
CN205973791U (en) * 2016-08-29 2017-02-22 江山市双氧水有限公司 Hydrogen peroxide solution production hydrogenation uses novel fixed bed
CN109876740A (en) * 2019-04-03 2019-06-14 江山市双氧水有限公司 A kind of pipe type hydrogenator for hydrogenation in oxydol production apparatus
CN210419239U (en) * 2019-07-15 2020-04-28 湖北三宁化工股份有限公司 Variable load system for anthraquinone process hydrogen peroxide production device

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9001802D0 (en) * 1989-01-27 1990-03-28 Kemira Oy A process for the preparation of hydrogen peroxide
CN102161475A (en) * 2009-11-02 2011-08-24 郑国玉 Concentration method in production of hydrogen peroxide by anthraquinone method
WO2011134345A1 (en) * 2010-04-29 2011-11-03 扬州惠通化工技术有限公司 Hydrogenating system for producing hydrogen peroxide
CN205973791U (en) * 2016-08-29 2017-02-22 江山市双氧水有限公司 Hydrogen peroxide solution production hydrogenation uses novel fixed bed
CN109876740A (en) * 2019-04-03 2019-06-14 江山市双氧水有限公司 A kind of pipe type hydrogenator for hydrogenation in oxydol production apparatus
CN210419239U (en) * 2019-07-15 2020-04-28 湖北三宁化工股份有限公司 Variable load system for anthraquinone process hydrogen peroxide production device

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
全国安全生产教育培训教材编审委员会: "《过氧化工艺作业》", 31 October 2012, 徐州:中国矿业大学出版社 *
刘国柱等: "蒽醌法制过氧化氢用氢化反应器的研究进展", 《现代化工》 *
王雪琦等: "蒽醌法制过氧化氢主要塔设备设计进展", 《化学推进剂与高分子材料》 *

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Application publication date: 20200714