CN111573628B - Anthraquinone process hydrogen peroxide solution production catalyst regeneration circulating filtration system - Google Patents
Anthraquinone process hydrogen peroxide solution production catalyst regeneration circulating filtration system Download PDFInfo
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- CN111573628B CN111573628B CN202010250916.8A CN202010250916A CN111573628B CN 111573628 B CN111573628 B CN 111573628B CN 202010250916 A CN202010250916 A CN 202010250916A CN 111573628 B CN111573628 B CN 111573628B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/022—Preparation from organic compounds
- C01B15/023—Preparation from organic compounds by the alkyl-anthraquinone process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/20—Regeneration or reactivation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/50—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using organic liquids
- B01J38/56—Hydrocarbons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/72—Regeneration or reactivation of catalysts, in general including segregation of diverse particles
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The invention belongs to the technical field of chemical production, and particularly relates to a regeneration circulating filtration system for an anthraquinone method hydrogen peroxide production catalyst, which comprises a regeneration cooler, wherein a liquid inlet of the regeneration cooler is communicated to a hydrogenation tower through a pipeline; the liquid outlet of the regeneration cooler is connected to a regeneration metering tank, the outlet of the regeneration metering tank is divided into two paths, one path is communicated to the preparation kettle, the other path is communicated to the liquid inlet of the regeneration circulating pump, and the liquid outlet of the regeneration circulating pump is divided into three paths: one path is communicated to the preparation kettle, the other path is communicated to the regeneration filter, and the other path is communicated to the hydrogenation tower after being converged with a liquid outlet pipeline of the regeneration filter through a pipeline; the invention forms a circulating system by adding a regenerative cooler, a regenerative metering tank, a regenerative circulating pump and a regenerative filter, circularly soaks the catalyst, effectively removes solid impurities such as alumina powder, broken catalyst powder, ceramic balls and the like by matching with the regenerative filter, and reduces the damage of the catalyst; the activity of the regenerated catalyst is improved, and the service life of the catalyst is prolonged.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a catalyst regeneration circulating filtration system for hydrogen peroxide production by an anthraquinone process.
Background
The anthraquinone process of producing hydrogen peroxide solution with 2-ethyl anthraquinone and tetrahydro 2-ethyl anthraquinone as carrier and trioctyl phosphate and heavy arene as solvent includes the steps of hydrogenation, oxidation, extraction, post-treatment and preparation. The hydrogenation process mainly comprises that working solution and hydrogen flow downwards in a hydrogenation tower provided with a catalyst bed layer to carry out hydrogenation reaction, and after the catalyst bed layer of the hydrogenation tower runs for a period of time, the activity is reduced or inactivated, and regeneration treatment is needed. The commonly used regeneration method is a steam method, i.e. organic impurities and inorganic impurities adsorbed on the catalyst are washed clean by steam, so that the catalyst is recovered to activity. The steam method regeneration has the following problems: only steam is used for blowing, alkali liquor, anthraquinone and anthraquinone degradation products adsorbed in catalyst micropores cannot be effectively dissolved and separated, so that the catalyst micropores are blocked, and the regeneration effect is poor; alumina powder on the surface of the catalyst, catalyst powder in the bed layer and damaged ceramic balls can not be effectively removed, so that the pressure difference of the catalyst bed layer is increased, and the activity of the catalyst is reduced.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a catalyst regeneration circulating and filtering system for producing hydrogen peroxide by an anthraquinone process, which improves the regeneration effect of the catalyst, reduces the damage to the catalyst and prolongs the service life of the catalyst.
In order to achieve the purpose, the invention adopts the following technical scheme:
a catalyst regeneration circulating filtration system for anthraquinone process hydrogen peroxide production is used for the regeneration of a catalyst in a hydrogenation tower, and comprises a regeneration cooler, wherein a liquid inlet of the regeneration cooler is communicated to the hydrogenation tower through a pipeline with a control valve; the liquid outlet of the regeneration cooler is connected to a regeneration metering tank, the outlet of the regeneration metering tank is divided into two paths, one path is communicated to the preparation kettle through a material pumping pipeline with a control valve, the other path is communicated to the liquid inlet of the regeneration circulating pump through a pipeline with a control valve, and the liquid outlet of the regeneration circulating pump is divided into three paths: one path is communicated to the preparation kettle through a material returning pipeline with a control valve, one path is communicated to the regeneration filter through a pipeline with a control valve, and the other path is communicated to the hydrogenation tower after being converged with a liquid outlet pipeline of the regeneration filter through a pipeline with a control valve;
wherein, the hydrogenation tower is provided with a working solution inlet pipe and a feeding pipeline;
a first steam access pipe and a cooling water access pipe are arranged on the side wall of the regenerative cooler;
a first nitrogen gas access pipe is arranged on the regeneration metering tank;
the top of regeneration filter is equipped with a demineralized water and inserts pipe, a second steam and inserts pipe and a second nitrogen and insert the pipe, and is equipped with a blow-off pipe in its bottom, regeneration filter's internally mounted has stainless steel metal filter.
Compared with the prior art, the invention has the following technical effects:
according to the catalyst regeneration circulating and filtering system for the production of hydrogen peroxide by the anthraquinone process, the regeneration cooler, the regeneration metering tank, the regeneration circulating pump and the regeneration filter are additionally arranged to form a circulating system, the catalyst is respectively subjected to circulating soaking by adopting hot aromatic hydrocarbon, and anthraquinone degradation products adsorbed in the catalyst are effectively dissolved and separated; the catalyst is circularly soaked by hot desalted water, alkali liquor adsorbed in the catalyst is dissolved and separated, and solid impurities such as alumina powder, crushed catalyst powder, ceramic balls and the like are effectively removed by matching with a regenerative filter, so that the catalyst damage is reduced; the activity of the regenerated catalyst is improved, and the service life of the catalyst is prolonged.
Drawings
FIG. 1 is a schematic view of a catalyst regeneration circulating filtration system for the production of hydrogen peroxide by anthraquinone process according to the present invention;
the reference numbers in the figures illustrate: 1-a hydrogenation tower, 11-a working solution access pipe, 12-a feeding pipeline, 2-a regenerative cooler, 21-a first steam access pipe, 22-a cooling water access pipe, 3-a regenerative metering tank, 31-a material pumping pipeline, 32-a first nitrogen access pipe, 4-a regenerative circulating pump, 41-a material returning pipeline, 5-a regenerative filter, 51-a liquid outlet pipeline, 52-a desalted water access pipe, 53-a second steam access pipe, 54-a second nitrogen access pipe, 55-a sewage discharge pipe and 56-a stainless steel metal filter element.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
As shown in figure 1, the invention provides a catalyst regeneration circulating and filtering system for hydrogen peroxide production by an anthraquinone process, which is used for regenerating a catalyst in a hydrogenation tower 1, wherein the regeneration circulating and filtering system comprises a regeneration cooler 2, and a liquid inlet of the regeneration cooler 2 is communicated to the hydrogenation tower 1 through a pipeline with a control valve; the liquid outlet of the regenerative cooler 2 is connected to a regenerative metering tank 3, the outlet of the regenerative metering tank 3 is divided into two paths, one path is communicated to the preparation kettle through a material pumping pipeline 31 with a control valve, the other path is communicated to the liquid inlet of a regenerative circulating pump 4 through a pipeline with a control valve, and the liquid outlet of the regenerative circulating pump 4 is divided into three paths: one path is communicated to the preparation kettle through a material returning pipeline 41 with a control valve, the other path is communicated to a regeneration filter 5 through a pipeline with a control valve, and the other path is communicated to the hydrogenation tower 1 after being converged with a liquid outlet pipeline 51 of the regeneration filter 5 through a pipeline with a control valve;
wherein, the hydrogenation tower 1 is provided with a working solution inlet pipe 11 and a feeding pipeline 12;
a first steam access pipe 21 and a cooling water access pipe 22 are arranged on the side wall of the regenerative cooler 2;
a first nitrogen gas access pipe 32 is arranged on the regeneration metering tank 3;
the top of the regeneration filter 5 is provided with a desalted water inlet pipe 52, a second steam inlet pipe 53 and a second nitrogen inlet pipe 54, and the bottom of the regeneration filter 5 is provided with a drain pipe 55, and the regeneration filter 5 is internally provided with a stainless steel metal filter element 56.
In the invention, a palladium catalyst and inert alumina ceramic balls are filled in the hydrogenation tower 1 and are used for the hydrogenation process in the production of hydrogen peroxide by an anthraquinone method. The regenerative cooler 2 can heat or cool the circulating liquid passing through the regenerative cooler 2 through the first steam inlet pipe 21 and the cooling water inlet pipe 22, so as to control the temperature of the circulating liquid.
The regeneration circulating pump 4 provides circulating power of circulating liquid.
The regeneration filter 5 filters solid impurities in the circulating liquid, such as alumina powder, anthraquinone particles, broken catalyst powder and ceramic balls. In addition, in the present invention, the regeneration filter 5 may be backwashed with steam or desalted water, and nitrogen gas may be purged to remove the filtrate. In order to facilitate cleaning, the stainless steel filter element 56 in the regeneration filter 5 is detachable, that is, when the backwashing with steam or desalted water is not satisfactory, the stainless steel filter element 56 can be detached and cleaned to remove solid impurities accumulated on the stainless steel filter element 56.
The invention provides a regeneration circulating filtration system for a catalyst produced by hydrogen peroxide through an anthraquinone process, which has the working principle that:
an organic solvent, such as aromatic hydrocarbon, is added through a feeding pipeline 12 on the hydrogenation tower 1, the aromatic hydrocarbon passes through the hydrogenation tower 1 where the catalyst is located, and then sequentially enters a regenerative cooler 2, a regenerative metering tank 3, a regenerative circulating pump 4 and a regenerative filter 5, and then returns to the hydrogenation tower 1, so that circulation is formed. Wherein, the regenerative cooler 2 heats the circulated aromatic hydrocarbon, specifically, the aromatic hydrocarbon is heated to 40-45 ℃; a first nitrogen inlet pipe 32 on the regeneration metering tank 3 is filled with nitrogen to ensure the safety of the aromatic hydrocarbon in the circulation process; the regeneration circulating pump 4 provides circulating power, the aromatic hydrocarbon soaks and washes the catalyst in the process of continuous circulation, anthraquinone and its degradation product absorbed in the catalyst are fully dissolved out, in order to improve the activity of regenerated catalyst; the regenerative filter 5 realizes the filtering function, and the aromatic hydrocarbon can be indirectly supplemented from the feeding pipeline 12 and put into the preparation kettle for cleaning through the material extracting pipeline 31 or the material returning pipeline 41 for recycling.
In the invention, in order to achieve a better soaking and washing effect on the catalyst, a mixed solution of aromatic hydrocarbon and trioctyl phosphate can be added into a hydrogenation tower 1 through a feeding pipeline 12, specifically, the aromatic hydrocarbon and trioctyl phosphate are mixed according to a volume ratio of 1: 3-4, mixing; the arene is dissolved 2-ethyl anthraquinone and degradation products thereof, and the trioctyl phosphate is dissolved hydrogen anthraquinone.
In addition, the regeneration circulating filtration system provided by the invention can also add desalted water into the circulating system through a desalted water access pipe 52 on the regeneration filter 5, the desalted water is heated in the regeneration cooler 2, and the regeneration filter 5 dissolves and separates out the alkali liquor adsorbed by the catalyst in the continuous filtration process; the desalted water can be fed intermittently or continuously through the desalted water feeding pipe 52, and the circulating system is discharged from the material returning pipe 41, wherein the desalted water is fed and circulated until the desalted water discharged from the material returning pipe 41 is clear and transparent. Through the circulating soaking and washing of the desalted water and the filtration of the regeneration filter 5, alumina powder, damaged catalyst powder and ceramic balls are effectively removed, the damage of the catalyst is reduced, the activity of the regenerated catalyst is improved, and the service life of the catalyst is prolonged.
In the invention, the desalted water is colorless and transparent, has no suspended matter, contains no calcium, magnesium, chlorine and heavy metal ions, has the conductivity of less than or equal to 1 mu S/cm and has the pH value of 6-7; the nitrogen contains no oil, rust and other impurities, the purity is more than or equal to 99 percent, and the oxygen content is less than or equal to 0.2 percent; the aromatic hydrocarbon is C9 and C10 fractions, the aromatic hydrocarbon content is more than or equal to 96 percent (measured by a sulfonation method), and the total sulfur content is less than or equal to 5 ppm.
The preferred embodiments of the present invention have been described in detail with reference to the accompanying drawings, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (1)
1. A catalyst regeneration circulating and filtering system for production of hydrogen peroxide by an anthraquinone process is used for regeneration of a catalyst in a hydrogenation tower (1), and is characterized in that the regeneration circulating and filtering system comprises a regeneration cooler (2), and a liquid inlet of the regeneration cooler (2) is communicated to the hydrogenation tower (1) through a pipeline with a control valve; the liquid outlet of the regenerative cooler (2) is connected to a regenerative metering tank (3), the outlet of the regenerative metering tank (3) is divided into two paths, one path is communicated to the preparation kettle through a material pumping pipeline (31) with a control valve, the other path is communicated to the liquid inlet of a regenerative circulating pump (4) through a pipeline with a control valve, and the liquid outlet of the regenerative circulating pump (4) is divided into three paths: one path is communicated to the preparation kettle through a material returning pipeline (41) with a control valve, the other path is communicated to the regeneration filter (5) through a pipeline with a control valve, and the other path is communicated to the hydrogenation tower (1) after being converged with a liquid outlet pipeline (51) of the regeneration filter (5) through a pipeline with a control valve;
wherein, the hydrogenation tower (1) is provided with a working solution access pipe (11) and a feeding pipeline (12); a first steam access pipe (21) and a cooling water access pipe (22) are arranged on the side wall of the regenerative cooler (2);
a first nitrogen gas access pipe (32) is arranged on the regeneration metering tank (3);
the top of the regeneration filter (5) is provided with a desalted water inlet pipe (52), a second steam inlet pipe (53) and a second nitrogen inlet pipe (54), the bottom of the regeneration filter is provided with a drain pipe (55), and a stainless steel metal filter element (56) is arranged in the regeneration filter (5);
adding an organic solvent through a feeding pipeline (12) on the hydrogenation tower (1), wherein the organic solvent sequentially enters a regenerative cooler (2), a regenerative metering tank (3), a regenerative circulating pump (4) and a regenerative filter (5) after passing through the hydrogenation tower (1) where the catalyst is located, and then returns to the hydrogenation tower (1); the regenerative cooler (2) heats the circulating organic solvent, the regenerative filter (5) realizes filtration, the organic solvent is indirectly supplemented from the feeding pipeline (12), and the organic solvent is placed into a preparation kettle through the material pumping pipeline (31) or the material returning pipeline (41) for cleaning and recycling;
the regeneration circulating filtration system also adds desalted water into the circulating system through a desalted water inlet pipe (52) on the regeneration filter (5), the desalted water is heated in the regeneration cooler (2), the regeneration filter (5) dissolves and separates out alkali liquor adsorbed by the catalyst in the continuous filtration process, the desalted water realizes the discontinuous or continuous feeding through the desalted water inlet pipe (52), and the desalted water is discharged out of the circulating system from the material returning pipeline (41).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010250916.8A CN111573628B (en) | 2020-04-01 | 2020-04-01 | Anthraquinone process hydrogen peroxide solution production catalyst regeneration circulating filtration system |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010250916.8A CN111573628B (en) | 2020-04-01 | 2020-04-01 | Anthraquinone process hydrogen peroxide solution production catalyst regeneration circulating filtration system |
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| CN111573628A CN111573628A (en) | 2020-08-25 |
| CN111573628B true CN111573628B (en) | 2022-05-13 |
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| CN112919425A (en) * | 2021-02-03 | 2021-06-08 | 安徽金禾实业股份有限公司 | Method for circulating filtration in hydrogen peroxide production |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1348071A (en) * | 1970-08-27 | 1974-03-13 | Degussa | Hydrogen peroxide synthesis |
| 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 |
| CN104511315A (en) * | 2013-09-28 | 2015-04-15 | 中国石油化工股份有限公司 | Regeneration method of palladium catalyst for hydrogenation reaction |
| CN204356082U (en) * | 2015-01-05 | 2015-05-27 | 湖南中成化工有限公司 | The hydrogen peroxide hydrogenation system of catalyst regneration can be carried out online |
| CN106853957A (en) * | 2017-02-24 | 2017-06-16 | 华强化工集团股份有限公司 | Using the anthraquinone producing hydrogen peroxide technique of palladium catalyst fixed bed and its alkali lye separator |
-
2020
- 2020-04-01 CN CN202010250916.8A patent/CN111573628B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1348071A (en) * | 1970-08-27 | 1974-03-13 | Degussa | Hydrogen peroxide synthesis |
| 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 |
| CN104511315A (en) * | 2013-09-28 | 2015-04-15 | 中国石油化工股份有限公司 | Regeneration method of palladium catalyst for hydrogenation reaction |
| CN204356082U (en) * | 2015-01-05 | 2015-05-27 | 湖南中成化工有限公司 | The hydrogen peroxide hydrogenation system of catalyst regneration can be carried out online |
| CN106853957A (en) * | 2017-02-24 | 2017-06-16 | 华强化工集团股份有限公司 | Using the anthraquinone producing hydrogen peroxide technique of palladium catalyst fixed bed and its alkali lye separator |
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