CN103964394A - Hydrogenation system for hydrogen peroxide production - Google Patents
Hydrogenation system for hydrogen peroxide production Download PDFInfo
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- CN103964394A CN103964394A CN201410191991.6A CN201410191991A CN103964394A CN 103964394 A CN103964394 A CN 103964394A CN 201410191991 A CN201410191991 A CN 201410191991A CN 103964394 A CN103964394 A CN 103964394A
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Abstract
The invention relates to a hydrogenation system for hydrogen peroxide production. The hydrogenation system comprises two hydrogenation towers and is characterized in that the two hydrogenation towers are provided with tower kettles; an inlet of the tower top of the first tower is connected with an outlet of a first working liquid cooler, and a hydrogen inlet in the upper part of the tower kettle of the first tower is connected with a hydrogen source; one outlet of the kettle bottom of the first tower is connected with an inlet of the first working liquid cooler, and the inlet of the first working liquid cooler is connected with a circulation working liquid source; another outlet of the kettle bottom is connected with an inlet of a second working liquid cooler, and an outlet of the second working liquid cooler is connected with a hydrogenated liquid inlet in the tower top of the second tower; an outlet of the kettle bottom of the second tower is connected with the inlet of the second working liquid cooler through a second hydrogenated liquid circulating pump, and another outlet of the tower kettle is connected with a hydrogenated liquid filter; the hydrogenated liquid filter is connected with a hydrogenated liquid storage tank, and the hydrogenated liquid storage tank is connected with a hydrogenated liquid cooler; the hydrogenated liquid cooler is connected with an oxidizing tower. The hydrogenation system solves the problems that gas and liquid do not flow uniformly in a static bed, and local working liquid flows obliquely and is in retention, which cause that anthraquinone is excessively hydrogenated to be degraded.
Description
Technical field
The present invention relates to a kind of hydrogenation system for hydrogen peroxide manufacture, belong to hydrogen peroxide manufacture equipment technology field.
Background technology
The fixed bed hydrogenation technique that the existing hydrogen peroxide obtained by anthraquinone process of China is produced, be gas and liquid flowing type palladium catalyst technique for fixing, be typically the three tower cascade connected technique in upper, middle and lower of Liming chemical Inst's exploitation, and the described two tower tandem process up and down with side cooler of Chinese invention patent: ZL201010160053.1.Hydrogen and working fluid as raw material are all to be entered by tower top, gas-liquid two-phase and stream by catalyst layer and under.Owing to having loaded solid catalyst (being fixed bed) in hydrogenation tower, gas, liquid is mobile concurrent biochemical reaction between catalyst grains, thereby the filling situation of catalyst and temperature of reaction control, most important on the impact of hydrogenation.Existing processing condition have limited hydrogenation efficiency, and chemical cost is high with respect to fluidized-bed is low to cause efficiency.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of hydrogenation system for hydrogen peroxide manufacture is provided, having solved gas-liquid mobile uneven in fixed bed, because bias current, delay cause anthraquinone excessive hydrogenation, there is the phenomenon of side reaction in local working fluid; And improve hydrogenation efficiency.
According to technical scheme provided by the invention, a kind of hydrogenation system for hydrogen peroxide manufacture, comprises the first working fluid water cooler, the second working fluid water cooler, hydrogenation tower, hydride strainer and hydride storage tank, feature is: described hydrogenation tower is divided into the first tower and the second tower, described the first tower and the second tower horizontal series or be arranged in parallel, the working fluid import of the first column overhead connects the outlet of the first working fluid water cooler, the hydrogen inlet on hydrogenation tower tower reactor top all connects the sources of hydrogen from hydrogen filter, at the bottom of the first tower reactor first outlet connects the import of the first working fluid water cooler through hydride recycle pump, the import of the first working fluid water cooler also connects working fluid source through the first hydride recycle pump, at the bottom of the first tower reactor second outlet connects the import of the second working fluid water cooler through the second hydride recycle pump, the outlet of the second working fluid water cooler connects the hydride import of the second column overhead, outlet at the bottom of the second tower reactor connects the import of the second working fluid water cooler through the second hydride recycle pump, at the bottom of the second tower reactor, another outlet connects the import of hydride strainer, the outlet of hydride strainer connects the import of hydride storage tank, the outlet of hydride storage tank connects the import of hydride water cooler through hydrogenation liquid pump, the outlet of hydride water cooler connects oxidizing tower.
The hydrogenation tail gas outlet of described hydrogenation column overhead connects respectively the first hydrogenation tail gas condenser and the second hydrogenation tail gas condenser.
Described the first tower and the second tower are horizontally disposed with or are setting up and down.
The present invention has the following advantages: it is mobile uneven in fixed bed that (1) the present invention has more thoroughly overcome gas-liquid, and local working fluid, because bias current, delay cause anthraquinone excessive hydrogenation, the phenomenon that side reaction causes anthraquinone to degrade occurs; (2) hydrogenation efficiency of catalyst service efficiency and working fluid, under identical condition, improves approximately 50%.
Brief description of the drawings
fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with concrete accompanying drawing, the invention will be further described.
As shown in Figure 1: the described hydrogenation system for hydrogen peroxide manufacture comprises the first working fluid water cooler E1101A, the second working fluid water cooler E1101B, the first tower T1101A, the second tower T1101B, hydride strainer X1103, hydride storage tank V1104, hydride water cooler E1102, the first hydrogenation tail gas condenser E1103A, the second hydrogenation tail gas condenser E1103B, the first hydride recycle pump P1, the second hydride recycle pump P2, draw-off pump P3 etc.
As shown in Figure 1, the present invention includes the first working fluid water cooler E1101A, the second working fluid water cooler E1101B, hydrogenation tower, hydride strainer X1103 and hydride storage tank V1104; described hydrogenation tower be divided into be horizontally disposed with or setting up and down can be in parallel or the first tower T1101A and the second tower T1101B of series connection, the working fluid import of the first tower T1101A tower top connects the outlet of the first working fluid water cooler E1101A, the hydrogen inlet on hydrogenation tower tower reactor top all connects the sources of hydrogen from hydrogen filter, at the bottom of the first tower T1101A tower reactor first outlet connects the import of the first working fluid water cooler E1101A through the first hydride recycle pump P1, the import of the first working fluid water cooler E1101A also connects working fluid source through the first hydride recycle pump P1, at the bottom of the first tower T1101A still second outlet connects the import of the second working fluid water cooler E1101B through the second hydride recycle pump P2, the outlet of the second working fluid water cooler E1101B connects the hydride import of the second tower T1101B tower top, outlet at the bottom of the second tower T1101B still connects the import of the second working fluid water cooler E1101B through the second hydride recycle pump P2, at the bottom of the second tower T1101B still, connect the import of hydride strainer X1103, the outlet of hydride strainer X1103 connects the import of hydride storage tank V1104, the outlet of hydride storage tank V1104 connects the import of hydride water cooler E1102 through draw-off pump P3, the outlet of hydride water cooler E1102 connects oxidizing tower,
The hydrogenation tail gas outlet of described the first tower T1101A and the second tower T1101B top of tower is connected respectively the first hydrogenation tail gas condenser E1103A and the second hydrogenation tail gas condenser E1103B;
The import of described the first working fluid water cooler E1101A, the second working fluid water cooler E1101B, hydrogenation tower, hydride strainer X1103, hydride storage tank V1104, hydride water cooler E1102, the first hydrogenation tail gas condenser E1103A and the second hydrogenation tail gas condenser E1103B and outlet all can arrange corresponding valve, part valve can be level control valve, pressure controlled valve, temperature-sensing valve etc., to control corresponding flow, pressure and temperature.
Principle of work of the present invention: after the first circulation hydride exporting mixes at the bottom of the cycle working fluid being come by working fluid pumping and the first tower T1101A still, deliver to the first working fluid water cooler E1101A by the first hydride recycle pump P1, after the first working fluid water cooler E1101A controls certain temperature, enter hydrogenation tower from the working fluid import of the first tower T1001A tower top; Hydrogen enters hydrogenation tower tower reactor top after hydrogen filter is removed the mechanical impurity that may carry secretly.
The horizontal series that whole hydrogenation system is filled by palladium catalyst or two in parallel reaction towers form, and adopt under normal circumstances two tower string use, also can use and another tower carries out the regeneration of catalyst or in for subsequent use at the next tower of light load.Spray and lower time through bed top sparger at working fluid and circulation hydride simultaneously, 2-ethyl-anthraquinone wherein and carry out hydrogenation with the hydrogen of reverse rising under palladium catalysis, generate corresponding 2-ethyl hydrogen anthraquinone and a small amount of tetrahydrochysene 2-ethyl-anthraquinone, the working fluid after catalyst shortening is called hydride.Enter after tower reactor by controlling needs, partly return to tower top by circulation hydrogenation liquid pump.Return in tower and utilize after regeneration vapour cooler makes wherein most of aromatic hydrocarbons condensation from the isolated hydrogenation tail gas of tower top (mainly carrying partial solvent aromatic hydrocarbons secretly).A hydride part for hydrogenation tower reactor is sent hydrogenation tower back to through hydride recycle pump, and another part hydride is pressed into hydride strainer by tower bottom pressure, catalyst and the carrier a small amount of powder of elimination from washing away out in hydrogenation tower.Hydride after filtering enters hydride storage tank, relends and helps draw-off pump that hydride is sent into oxidizing tower.
The present invention has following effect:
(1) the present invention has adopted the technical process that gas-liquid counter current fixed bed hydrogenation technology and efficient ball palladium catalyst combine;
(2) mainly hydrogenation tower external circulation hydrogenation water cooler, constitute the complete hydroprocessing Controlling System that contains large flow circulation hydride, thereby realized the real-time optimization adjusting of hydrogenation conditions (temperature, pressure, the actual flow that enters catalyst layer of working fluid) multiparameter is controlled, thereby tower structure and catalyzer service efficiency are effectively improved;
(3) the cooling automatic control of systemic circulation flow hydrogenation mixed solution, realizes the accurate control to catalyst sensitive temperature, thereby effectively selects the best use temperature of palladium catalyst;
(4) in working fluid, effective anthraquinone hydrogenation reaction is carried out under more effective air-flow counter current contact, is more conducive to overcome the generation of side reaction;
(5) the ingenious combination of the parallel series connection of realization two towers, selects the operation scheme of more rational serial or parallel connection, thereby increase turndown ratio at the different use active phase of catalyst and different market loads;
(6), in external circulating cooling hydrogenation scheme, by working fluid and circulation hydride process centrifugal pumping process, automatically realize highly and mixing dexterously;
(7), in catalyst layer, as the upstream of raw hydrogen, by effectively controlling in real time of hydrogen emptying and circulating flow rate, overcome traditional gas-liquid following current hydrogenation fixed bed and upgraded the initial stage and use the discomfort often occurring late period at catalyst.
Hydrogenation system for hydrogen peroxide manufacture of the present invention, really has now most complete anthraquinone hydrogenation reaction flow process in the world; On the same device of actual motion, successfully reach hydrogenation high-level efficiency and simple to operate stable, every consumption indicators has remarkable reduction.
Claims (3)
1. for a hydrogenation system for hydrogen peroxide manufacture, comprise the first working fluid water cooler (E1101A), the second working fluid water cooler (E1101B), hydrogenation tower, hydride strainer (X1103) and hydride storage tank (V1104); it is characterized in that: described hydrogenation tower is divided into the first tower (T1101A) and the second tower (T1101B), described the first tower (T1101A) and the second tower (T1101B) horizontal series or be arranged in parallel, the working fluid import of the first tower (T1101A) tower top connects the outlet of the first working fluid water cooler (E1101A), the hydrogen inlet on hydrogenation tower tower reactor top all connects the sources of hydrogen from hydrogen filter, at the bottom of the first tower (T1101A) still first outlet connects the import of the first working fluid water cooler (E1101A) through hydride recycle pump (P1), the import of the first working fluid water cooler (E1101A) also connects working fluid source through the first hydride recycle pump (P1), at the bottom of the first tower (T1101A) still second outlet connects the import of the second working fluid water cooler (E1101B) through the second hydride recycle pump (P2), the outlet of the second working fluid water cooler (E1101B) connects the hydride import of the second tower (T1101B) tower top, outlet at the bottom of the second tower (T1101B) still connects the import of the second working fluid water cooler (E1101B) through the second hydride recycle pump (P2), at the bottom of the second tower (T1101B) still, another outlet connects the import of hydride strainer (X1103), the outlet of hydride strainer (X1103) connects the import of hydride storage tank (V1104), the outlet of hydride storage tank (V1104) connects the import of hydride water cooler (E1102) through hydrogenation liquid pump (P3), the outlet of hydride water cooler (E1102) connects oxidizing tower.
2. the hydrogenation system for hydrogen peroxide manufacture as claimed in claim 1, is characterized in that: the hydrogenation tail gas outlet of described hydrogenation column overhead connects respectively the first hydrogenation tail gas condenser (E1103A) and the second hydrogenation tail gas condenser (E1103B).
3. the hydrogenation system for hydrogen peroxide manufacture as claimed in claim 1, is characterized in that: described the first tower (T1101A) and the second tower (T1101B) are horizontally disposed with or are setting up and down.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410191991.6A CN103964394B (en) | 2014-05-07 | 2014-05-07 | For the hydrogenation system of hydrogen peroxide manufacture |
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| CN201410191991.6A CN103964394B (en) | 2014-05-07 | 2014-05-07 | For the hydrogenation system of hydrogen peroxide manufacture |
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| CN103964394B CN103964394B (en) | 2015-11-04 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105540551A (en) * | 2014-11-03 | 2016-05-04 | 中国石油化工股份有限公司 | Efficient hydrogenation process in hydrogen peroxide production |
| CN107032305A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | The production system and production method of a kind of hydrogen peroxide |
| CN107032306A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | Fluid bed produces the system and method for hydrogen peroxide |
| CN107098317A (en) * | 2017-06-15 | 2017-08-29 | 扬州惠通化工科技股份有限公司 | The system and method for process for prepairng hydrogen peroxide by anthraquinone |
| CN109809367A (en) * | 2019-04-03 | 2019-05-28 | 江山市双氧水有限公司 | One kind is for hydrogenation tower process devices double in Hydrogen Peroxide Production system |
| 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 |
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| CN101066751A (en) * | 2006-05-01 | 2007-11-07 | 三菱瓦斯化学株式会社 | Method for activating hydrogenation catalyst and method for producing hydrogen peroxide including same |
| CN101837957A (en) * | 2010-04-29 | 2010-09-22 | 扬州惠通化工技术有限公司 | Hydrogenation system for producing hydrogen peroxide |
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2014
- 2014-05-07 CN CN201410191991.6A patent/CN103964394B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066751A (en) * | 2006-05-01 | 2007-11-07 | 三菱瓦斯化学株式会社 | Method for activating hydrogenation catalyst and method for producing hydrogen peroxide including same |
| CN101837957A (en) * | 2010-04-29 | 2010-09-22 | 扬州惠通化工技术有限公司 | Hydrogenation system for producing hydrogen peroxide |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105540551A (en) * | 2014-11-03 | 2016-05-04 | 中国石油化工股份有限公司 | Efficient hydrogenation process in hydrogen peroxide production |
| CN105540551B (en) * | 2014-11-03 | 2017-07-28 | 中国石油化工股份有限公司 | A kind of efficient hydrogenation process in Hydrogen Peroxide Production |
| CN107032305A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | The production system and production method of a kind of hydrogen peroxide |
| CN107032306A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | Fluid bed produces the system and method for hydrogen peroxide |
| CN107098317A (en) * | 2017-06-15 | 2017-08-29 | 扬州惠通化工科技股份有限公司 | The system and method for process for prepairng hydrogen peroxide by anthraquinone |
| CN107098317B (en) * | 2017-06-15 | 2023-06-27 | 扬州惠通科技股份有限公司 | System and method for producing hydrogen peroxide by anthraquinone process |
| CN107032306B (en) * | 2017-06-15 | 2023-07-14 | 扬州惠通科技股份有限公司 | System and method for producing hydrogen peroxide by fluidized bed |
| CN107032305B (en) * | 2017-06-15 | 2023-07-14 | 扬州惠通科技股份有限公司 | Hydrogen peroxide production system and production method |
| CN109809367A (en) * | 2019-04-03 | 2019-05-28 | 江山市双氧水有限公司 | One kind is for hydrogenation tower process devices double in Hydrogen Peroxide Production system |
| 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 |
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| CN103964394B (en) | 2015-11-04 |
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Effective date of registration: 20170503 Address after: 225003, Jiangsu, Yangzhou economic and Technological Development Zone, 186 middle Yangtze River Road, block B, 5 floor Patentee after: Polytex Chemical Engineering Co., Ltd. Address before: Huishan District Luo Luonan Avenue she Zhen Fu Shan Cun 214187 Jiangsu city of Wuxi Province Patentee before: Complete chemical engineering Science and Technology Ltd. without Sion |