CN103964394B - For the hydrogenation system of hydrogen peroxide manufacture - Google Patents
For the hydrogenation system of hydrogen peroxide manufacture Download PDFInfo
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- CN103964394B CN103964394B CN201410191991.6A CN201410191991A CN103964394B CN 103964394 B CN103964394 B CN 103964394B CN 201410191991 A CN201410191991 A CN 201410191991A CN 103964394 B CN103964394 B CN 103964394B
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Abstract
The present invention relates to a kind of hydrogenation system for hydrogen peroxide manufacture, comprise hydrogenation tower; Feature is: described hydrogenation tower is two towers of band tower reactor, first column overhead import connects the outlet of the first working fluid water cooler, the hydrogen inlet on tower reactor top connects sources of hydrogen, the import of an outlet connection first working fluid water cooler at the bottom of first tower reactor, the import of the first working fluid water cooler connects cycle working fluid source; The import of another outlet connection second working fluid water cooler at the bottom of still, the outlet of the second working fluid water cooler connects the hydride import of the second column overhead, outlet at the bottom of second tower reactor connects the import of the second working fluid water cooler through the second hydride recycle pump, another outlet of tower reactor connects hydride strainer, hydride strainer connects hydride storage tank, hydride storage tank connects hydride water cooler, and hydride water cooler connects oxidizing tower.The invention solves gas-liquid to flow in fixed bed inequality, the bias current of partial duty liquid, be detained and cause anthraquinone excessive hydrogenation and the problem of degrading.
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, the typically three tower cascade connected technique in upper, middle and lower of Liming chemical Inst's exploitation, and Chinese invention patent: the two tower tandem process up and down of the band side cooler described by ZL201010160053.1.All entered by tower top as the hydrogen of raw material and working fluid, gas-liquid two-phase and flow through catalyst layer and under.Owing to being filled with solid catalyst (i.e. fixed bed) hydrogenation tower is in-built, gas, liquid flow concurrent biochemical reaction between catalyst grains, and thus the filling situation of catalyst and temperature of reaction control, most important on the impact of hydrogenation.Existing processing condition limit hydrogenation efficiency, and chemical cost is high relative 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, solving gas-liquid to flow in fixed bed inequality, because of bias current, delay and cause anthraquinone excessive hydrogenation, there is the phenomenon of side reaction in partial duty liquid; 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 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, the first outlet at the bottom of first tower reactor 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, the second outlet at the bottom of first tower reactor 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 second tower reactor connects the import of the second working fluid water cooler through the second hydride recycle pump, another outlet at the bottom of second tower reactor 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 hydrogenated tail gas outlet of described hydrogenation column overhead connects the first hydrogenated tail gas condenser and the second hydrogenated tail gas condenser respectively.
Described first tower and the second tower are horizontally disposed with or setting up and down.
The present invention has the following advantages: (1) the present invention more thoroughly overcomes gas-liquid and to flow in fixed bed inequality, and partial duty liquid, because of bias current, delay and cause anthraquinone excessive hydrogenation, the phenomenon that side reaction causes anthraquinone to degrade occurs; (2) hydrogenation efficiency of catalyst service efficiency and working fluid at identical conditions, improves about 50%.
Accompanying drawing explanation
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 hydrogenated tail gas condenser E1103A, the second hydrogenated 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 the first tower T1101A of in parallel or series connection and the second tower T1101B, 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, the first outlet at the bottom of first tower T1101A tower reactor 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, the second outlet at the bottom of first tower T1101A still 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 second tower T1101B still connects the import of the second working fluid water cooler E1101B through the second hydride recycle pump P2, the import of hydride strainer X1103 is connected at the bottom of second tower T1101B still, 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,
Described first tower T1101A is connected the first hydrogenated tail gas condenser E1103A and the second hydrogenated tail gas condenser E1103B respectively with the hydrogenated tail gas outlet of the second tower T1101B top of tower;
Import and the outlet of described 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 hydrogenated tail gas condenser E1103A and the second hydrogenated tail gas condenser E1103B 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 of exporting mixes at the bottom of the cycle working fluid 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, control to enter hydrogenation tower from the working fluid import of the first tower T1001A tower top after certain temperature through the first working fluid water cooler E1101A; Hydrogen removes after the mechanical impurity that may carry secretly through hydrogen filter and enters hydrogenation tower tower reactor top.
Two reaction towers of the horizontal series that whole hydrogenation system is filled by palladium catalyst or parallel connection form, and adopt two tower string use under normal circumstances, also can use at the next tower of light load and another tower carries out the regeneration of catalyst or is in for subsequent use.Time under working fluid and circulation hydride are simultaneously through bed top sparger spray, 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, namely the working fluid after catalyst shortening is called hydride.By controlling needs after entering tower reactor, part returns tower top by circulation hydrogenation liquid pump.Return in tower after regeneration vapour cooler makes wherein most of aromatic hydrocarbons condensation from the isolated hydrogenated tail gas of tower top (main entrainment portions solvent aromatic hydrocarbons) and utilize.A hydride part for hydrogenation tower reactor sends hydrogenation tower back to through hydride recycle pump, and another part hydride is by tower bottom pressure press-in hydride strainer, the catalyst that elimination washes away out in hydrogenation tower and a small amount of powder of carrier.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) present invention employs the technical process that gas-liquid counter current fixed bed hydrogenation technology and efficient ball palladium catalyst combine;
(2) mainly at the external circulation hydrogenation water cooler of hydrogenation tower, combination forms the complete hydroprocessing Controlling System containing large discharge circulation hydride, thus achieve the real-time optimization regulable control to hydrogenation conditions (the actual flow entering catalyst layer of temperature, pressure, working fluid) multiparameter, thus effectively improve tower structure and catalyzer service efficiency;
(3) the cooling automatic control of systemic circulation flow hydrogenation mixed solution, realizes the accurate control to catalyst sensitive temperature, thus the effective best use temperature selecting palladium catalyst;
(4) in working fluid, effective anthraquinone hydrogenation reaction is carried out under more effective gas flow counterflow contact, is more conducive to the generation overcoming side reaction;
(5) realize the ingenious combination of parallel series connection two tower, select at the different use active phase of catalyst and different market loads, the more reasonably operation scheme of serial or parallel connection, thus increase turndown ratio;
(6) in external circulating cooling hydrogenation scheme, dexterously by working fluid and circulation hydride in centrifugal pumping process, automatically realize highly mixing;
(7) in catalyst layer, as the upstream of raw hydrogen, controlled by hydrogen gas automatic blow down and the effective in real time of circulating flow rate, overcome traditional gas-liquid following current hydrogenation fixed bed and upgrade the initial stage at catalyst and use the discomfort often occurred late period.
Hydrogenation system for hydrogen peroxide manufacture of the present invention, really has current 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 (2)
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 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, the first outlet at the bottom of first tower (T1101A) still 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), the second outlet at the bottom of first tower (T1101A) still 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 second tower (T1101B) still connects the import of the second working fluid water cooler (E1101B) through the second hydride recycle pump (P2), another outlet at the bottom of second tower (T1101B) still 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. as claimed in claim 1 for the hydrogenation system of hydrogen peroxide manufacture, it is characterized in that: the hydrogenated tail gas outlet of described hydrogenation column overhead connects the first hydrogenated tail gas condenser (E1103A) and the second hydrogenated tail gas condenser (E1103B) respectively.
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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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| CN103964394A CN103964394A (en) | 2014-08-06 |
| CN103964394B true CN103964394B (en) | 2015-11-04 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
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 |
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- 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 |
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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 |
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