CN115501680A - Working solution regeneration device for preparing hydrogen peroxide by anthraquinone process - Google Patents
Working solution regeneration device for preparing hydrogen peroxide by anthraquinone process Download PDFInfo
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- CN115501680A CN115501680A CN202110696020.7A CN202110696020A CN115501680A CN 115501680 A CN115501680 A CN 115501680A CN 202110696020 A CN202110696020 A CN 202110696020A CN 115501680 A CN115501680 A CN 115501680A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/02—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor with moving adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/203—Equilibration or regeneration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction, e.g. ion-exchange, ion-pair, ion-suppression or ion-exclusion
- B01D15/361—Ion-exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/003—Filters in combination with devices for the removal of liquids
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- C—CHEMISTRY; METALLURGY
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- 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
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- C01B15/023—Preparation from organic compounds by the alkyl-anthraquinone process
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Abstract
The invention relates to the field of hydrogen peroxide preparation, and discloses a working solution regeneration device for preparing hydrogen peroxide by an anthraquinone method. The device includes: adsorption tower (1), filter unit (2) and adsorbent regeneration unit (4), adsorption tower (1) includes: a liquid inlet at the bottom; the tower body (10) is filled with an adsorbent, and the lower part of the side surface of the tower body is provided with an adsorbent backflow inlet; the diameter expanding part (11) is positioned at the top end of the adsorption tower (1), the diameter of the diameter expanding part is larger than that of the tower body (10), the upper part of the side surface of the diameter expanding part is provided with an overflow port, and the lower part of the side surface of the diameter expanding part is provided with an adsorbent backflow outlet; a liquid distributor (13) connected with the liquid inlet; and a sleeve (12) connected to the liquid distributor (13) and having a tip end located in the enlarged diameter portion (11). The device can remove metal ions in the working solution, and improve the safety and stability of hydrogen peroxide preparation.
Description
Technical Field
The invention relates to the field of hydrogen peroxide preparation, in particular to a working solution regeneration device for preparing hydrogen peroxide by an anthraquinone process.
Background
The hydrogen peroxide is a green chemical product, and the production and use processes of the hydrogen peroxide hardly cause pollution, so the hydrogen peroxide is called as a 'clean' chemical product, is used as an oxidant, a bleaching agent, a disinfectant, a deoxidizer, a polymer initiator and a crosslinking agent, and is widely applied to the industries of chemical industry, papermaking, environmental protection, electronics, food, medicine, textile, mining industry, agricultural waste processing and the like.
At present, the production methods of hydrogen peroxide mainly comprise an electrolysis method, an isopropanol method, an oxygen cathode reduction method, a hydrogen-oxygen direct oxidation method, a vacuum enrichment method, an anthraquinone method and the like. Among them, the anthraquinone process is the mainstream of industrial hydrogen peroxide production, and industrial hydrogen peroxide is produced by the anthraquinone process in an amount of 99% or more in terms of production amount worldwide. The anthraquinone process includes hydrogenation, oxidation, extraction, post-treatment of circular work liquid and other technological steps. The working compound, typically an anthraquinone-based material, in the working fluid is first hydrogenated, and this step is usually carried out by reacting the working compound with hydrogen in the presence of a catalyst. Then, in the reoxidation unit, the hydrogenated working compound and an oxidant undergo an auto-oxidation reaction, oxygen can be air, oxygen or gas rich in oxygen, hydrogen peroxide is generated after the oxidation reaction, and the generated hydrogen peroxide is dissolved in the working solution and exists in a thinner concentration. Then hydrogen peroxide is enriched into water through extraction to obtain a hydrogen peroxide crude product, and the hydrogen peroxide crude product is purified through purification and other processes. The working compound is subjected to alkaline washing or vacuum drying to remove water and raffinate hydrogen peroxide, and then is circulated back to the hydrogenation unit for hydrogenation reaction, so that the circulation of the whole process is realized.
Due to the scouring and corrosion of the equipment, and the introduction of metal ion impurities into the air for oxidation and the pure water for extraction, a small amount of metal ion impurities will be present in the working solution. Hydrogen peroxide is particularly sensitive to metal ion impurities, which at ppb levels can lead to decomposition of hydrogen peroxide, thereby reducing production efficiency and reducing safety of production.
At present, the method for solving the problem of hydrogen peroxide instability in the production process is to add phosphoric acid into a system as a stabilizer, add phosphoric acid before oxidation and in pure water for extraction, complex metal ion impurities and improve the stability of hydrogen peroxide. However, excessive addition of phosphoric acid causes pollution discharge and also causes problems such as equipment blockage.
Disclosure of Invention
The invention aims to overcome the problem of accumulation of metal ions in working solution prepared from hydrogen peroxide in the prior art, and provides a working solution regeneration device for preparing hydrogen peroxide by an anthraquinone method.
In order to achieve the above object, one aspect of the present invention provides an apparatus for regenerating a hydrogen peroxide working solution by an anthraquinone process, the apparatus comprising:
adsorption tower, filter unit and adsorbent regeneration unit, the adsorption tower includes:
a liquid inlet at the bottom;
the tower body is filled with an adsorbent, and the lower part of the side surface of the tower body is provided with an adsorbent backflow inlet;
the diameter of the diameter expanding part is larger than that of the tower body, the upper part of the side surface of the diameter expanding part is provided with an overflow port, and the lower part of the side surface of the diameter expanding part is provided with an adsorbent backflow outlet;
the liquid distributor is connected with the liquid inlet; and
a sleeve connected to the liquid distributor and having a distal end located in the enlarged diameter portion,
wherein the overflow port is connected with the filtering unit; the adsorbent regeneration unit is respectively connected with the adsorbent backflow outlet and the adsorbent backflow inlet.
Preferably, the ratio of the maximum diameter of the enlarged diameter portion to the diameter of the tower body is 1.1-2:1.
preferably, the tower body and the diameter-expanding part are integrally formed.
Preferably, the ratio of the diameter of the sleeve to the diameter of the tower is from 0.3 to 0.8:1.
preferably, there is a gap between the sleeve and the liquid distributor.
Preferably, the height of the voids is 400-600mm.
Preferably, the adsorbent regeneration unit is a stirred tank.
Preferably, the number of the filter units is more than 1, preferably more than one, and more preferably 2-3.
Preferably, the filter unit is a filter, and the filter medium is one or more of a cloth bag filter element, a chemical fiber filter element, a metal mesh filter element, a metal powder sintered filter element, a PP filter element, a line gap filter element and an activated carbon filter element.
Preferably, the pore size of the filter medium is 0.1 to 100 μm.
Preferably, when the number of the filter units is plural, the pore size of the filter medium of the filter unit located at the rear is smaller than that of the filter medium of the filter unit located at the front.
Preferably, the top and the bottom of the adsorption tower are provided with rupture discs, and the rupture discs are used for pressure relief when the pressure in the tank is greater than the specified pressure.
Preferably, the apparatus further comprises a conveying unit disposed on a pipeline between the adsorbent regeneration unit and the adsorbent inlet, for conveying the adsorbent into the adsorption tower.
Preferably, the adsorbent is one or more of macroporous resin, molecular sieve, activated carbon, MOF material, hydrotalcite, diatomaceous earth, alumina microspheres, cation exchange resin and anion exchange resin with the capability of adsorbing metal ions.
The second aspect of the invention provides a regeneration method of working solution for preparing hydrogen peroxide by an anthraquinone process, which comprises the step of introducing the working solution into the device for regeneration when the content of metal ions in the working solution is more than 10ppm.
Through the technical scheme, the device disclosed by the invention can efficiently remove metal ions in the hydrogen peroxide working solution prepared by the anthraquinone method, and the safety and stability of hydrogen peroxide preparation are improved.
Drawings
FIG. 1 is a schematic structural diagram of a working solution regeneration device for preparing hydrogen peroxide by an anthraquinone process.
Description of the reference numerals
1. An adsorption tower; 2 a first filtering unit;
3. a second filter unit; 4 an adsorbent regeneration unit;
10. a tower body; 11 an expanding part;
12. a sleeve; 13 a liquid distributor;
a, working solution; and B, adsorbing agent.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and these ranges or values should be understood to encompass values close to these ranges or values. For numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
In the present invention, the use of directional terms such as "upper, lower, left, right" generally means upper, lower, left, right with reference to the accompanying drawings, unless otherwise specified. "inner and outer" refer to the inner and outer relative to the contour of the component itself. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, the metal ion content ppm means mass ppm.
The invention provides a regeneration device of hydrogen peroxide working solution by anthraquinone process, as shown in figure 1, the device comprises:
adsorption tower 1, filter unit 2 and adsorbent regeneration unit 4, adsorption tower 1 includes:
a liquid inlet at the bottom;
the tower body 10 is used for being filled with an adsorbent, and the lower part of the side surface of the tower body is provided with an adsorbent backflow inlet;
the diameter-expanding part 11 is positioned at the top end of the adsorption tower 1, the diameter of the diameter-expanding part is larger than that of the tower body 10, the upper part of the side surface of the diameter-expanding part is provided with an overflow port, and the lower part of the side surface of the diameter-expanding part is provided with an adsorbent backflow outlet;
a liquid distributor 13 connected with the liquid inlet; and
a sleeve 12 connected to the liquid distributor 13 and having a tip end located in the enlarged diameter portion 11,
wherein the overflow port is connected with the filtering unit 2; the adsorbent regeneration unit 4 is connected with the adsorbent backflow outlet and the adsorbent backflow inlet respectively.
According to the present invention, in the adsorption column 1 of the present invention, the sleeve 12 is connected to the liquid distributor 13 and has a distal end located in the enlarged diameter portion 11, so that the working fluid enters from the fluid inlet, passes through the liquid distributor 13, and then moves upward in the sleeve 12 together with the adsorbent into the enlarged diameter portion 11, and then, due to a reduction in the flow velocity, the adsorbent falls by gravity, whereby a supernatant is obtained at an upper portion of the enlarged diameter portion, and the supernatant overflows and is discharged from an overflow port of the enlarged diameter portion 11, and the falling adsorbent and a part of the working fluid return to the bottom of the adsorption column 1. Since the supernatant liquid still contains a small amount of solid components, the overflow port is connected to the filtering unit 2, so that the working fluid is discharged from the adsorption tower 1 and then filtered by the filtering unit 2.
In order to realize the on-line regeneration of the adsorbent, the device of the invention is provided with an adsorbent regeneration unit 4, and the adsorbent regeneration unit 4 is respectively connected with the adsorbent backflow outlet and the adsorbent backflow inlet, so that the adsorbent enters the adsorbent regeneration unit 4 through the adsorbent backflow outlet for regeneration when the adsorbent needs to be regenerated, and then returns to the adsorption tower 1 from the adsorbent backflow inlet.
According to the invention, in order to facilitate the adsorbent returning to the bottom of the column to re-enter the casing 12, it is preferred that there is a gap between said casing 12 and said liquid distributor 13; in order to make the working fluid passing through the liquid distributor 13 enter the sleeve 12 as much as possible while the adsorbent returning to the bottom of the column can enter the sleeve again, the height of the gap is preferably 400 to 600mm, more preferably 450 to 550mm.
According to the present invention, in order to make the liquid flow rate of the enlarged diameter part 11 in a suitable range for settling of the adsorbent, it is preferable that the ratio of the maximum diameter of the enlarged diameter part 11 to the diameter of the tower body 10 is 1.1 to 2:1; more preferably, the ratio of the maximum diameter of the enlarged diameter portion 11 to the diameter of the tower 10 is 1.2-1.8:1.
in order to facilitate the settling of the adsorbent, the top end of the sleeve 12 is preferably located at a level below the overflow.
The connection mode of the tower body 10 and the diameter-expanded part 11 is not particularly limited, and the tower body and the diameter-expanded part may be integrally formed or may be connected by welding, bolting, riveting or the like; preferably, the tower body 10 and the enlarged diameter part 11 are integrally formed.
According to the present invention, in order to improve the adsorption efficiency by allowing the adsorbent to be sufficiently contacted with the liquid, it is preferable that the ratio of the diameter of the sleeve 12 to the diameter of the tower body 10 is 0.3 to 0.8:1; more preferably, the ratio of the diameter of the sleeve 12 to the diameter of the tower 10 is 0.4-0.7:1.
according to the present invention, preferably, the adsorbent regeneration unit 4 is a stirred tank.
According to the present invention, in order to make the filtration more sufficient and reduce the influence on the production of hydrogen peroxide, it is preferable that the number of the filter units 2 is 1 or more, preferably more, and more preferably 2 to 3.
According to the present invention, in order to reduce maintenance time and improve filtration efficiency, it is preferable that the filtration unit is a backwash filter.
The filter medium of the filter unit is not particularly limited, and may be, for example, one or more of a bag filter element, a chemical fiber filter element, a metal mesh filter element, a metal powder sintered filter element, a PP filter element, a wire gap filter element, and an activated carbon filter element; preferably, the filter medium of the filter unit is one or more of a chemical fiber filter element, a metal mesh filter element and a metal powder sintered filter element.
According to the invention, the pore size of the filter medium can be adjusted arbitrarily according to the needs, and the pore size of the filter medium can be 0.1-100 μm, for example; preferably, the pore size of the filter medium is 0.1 to 50 μm, more preferably, the pore size of the filter medium is 0.1 to 20 μm.
According to the present invention, when the filter unit is plural, it is preferable that the pore size of the filter medium of the filter unit located at the rear is smaller than that of the filter medium of the filter unit located at the front in order to improve the filtering efficiency.
According to the present invention, in order to improve the safety of the apparatus, it is preferable that the top and bottom of the adsorption tower 1 are provided with rupture discs for releasing pressure when the pressure in the tank is higher than a predetermined pressure, which can be selected by those skilled in the art according to the actual situation, for example, 0.6Mpa.
According to the present invention, it is preferable that the apparatus further comprises a transfer unit 5, the transfer unit 5 being provided on a pipeline between the adsorbent regeneration unit 4 and the adsorbent inlet for transferring the adsorbent into the adsorption tower 1. Preferably, the delivery unit is a centrifugal pump.
According to the present invention, the adsorbent filled in the adsorption tower 1 may be one or more of macroporous resin, molecular sieve, activated carbon, MOF material, hydrotalcite, diatomaceous earth, alumina microspheres, cation exchange resin, and anion exchange resin; more preferably, the adsorbent is one or more of a molecular sieve, activated carbon, MOF material, cation exchange resin and anion exchange resin.
The second aspect of the invention provides a regeneration method of working solution for preparing hydrogen peroxide by an anthraquinone process, which comprises the step of introducing the working solution into the regeneration device of the invention for regeneration when the content of metal ions in the working solution is more than 10ppm.
The method of using the apparatus for regenerating a hydrogen peroxide working fluid by an anthraquinone process according to the present invention will be described below.
As shown in fig. 1, the apparatus for regenerating the hydrogen peroxide working fluid by the anthraquinone process provided by the invention comprises: adsorption tower 1, first filter unit 2, second filter unit 3, adsorbent regeneration unit 4 and conveying unit 5, adsorption tower 1 includes: a liquid inlet at the bottom; a tower body 10 filled with an adsorbent and having an adsorbent return inlet at a lower portion of a side surface thereof; an overflow port is arranged at the upper part of the side surface of the diameter expanding part 11 positioned at the top end of the adsorption tower 1, and an adsorbent backflow outlet is arranged at the lower part of the side surface; a liquid distributor 13 connected with the liquid inlet, and a sleeve 12 connected with the liquid distributor 13 in a spaced way, wherein the end of the sleeve 12 is positioned in the diameter-expanding part 11. The overflow port is connected with the first filtering unit 2, and the first filtering unit 2 is connected with the second filtering unit 3; and the adsorbent regeneration unit 4 is respectively connected with the adsorbent backflow outlet and the adsorbent backflow inlet.
The working liquid enters the adsorption tower 1 from the liquid inlet, then enters the sleeve 12 after passing through the liquid distributor 13, drives the adsorbent to move upwards in the sleeve 12 to the tail end of the sleeve 12, then enters the diameter expanding part 11, the liquid flow rate is reduced in the diameter expanding part 11, the adsorbent and part of the liquid fall back to the tower body 10 under the action of gravity, the supernatant overflows through the overflow port, enters the first filtering unit 2, is filtered, then enters the second filtering unit 3, and is introduced into the anthraquinone method hydrogen peroxide preparation device.
When the adsorbent needs to be regenerated, the adsorbent backflow outlet is opened, the adsorbent is introduced into the adsorbent regeneration unit 4 for regeneration, then the adsorbent backflow inlet is opened, and the regenerated adsorbent is introduced into the adsorption tower 1.
In the following examples, the adsorbent diatomaceous earth was purchased from Huali diatomaceous earth products Ltd, in Shengzhou, under the designation CDX-5.
Example 1
The device shown in FIG. 1 is used for regenerating the hydrogen peroxide working solution of anthraquinone process of Balingdivision, china petrochemical industry, inc., wherein the total concentration of anthraquinone compounds in the working solution is 135g/L, and the content of metal ions is 10ppm.
The working solution enters the adsorption tower 1 from the liquid inlet (the tower body is 10mm in diameter and 10000mm in height, and is filled with diatomite with the diameter of 10mm, and the filling amount is 30m 3 ) Then the supernatant passes through a liquid distributor 13 (a metal sintered plate with the aperture of 100 mu m), enters a sleeve 12 (the diameter is 1800mm, a gap of 500mm is arranged between the sleeve 12 and the liquid distributor 13), drives the adsorbent to move upwards in the sleeve 12 to the tail end of the sleeve 12, then enters an expanding part 11 (the maximum diameter is 2750mm and the height is 6200 mm), the liquid flow rate is reduced in the expanding part 11, the adsorbent and part of the liquid fall back to the tower body 10 under the action of gravity, the supernatant overflows through an overflow port, enters a first filtering unit 2 (a back-flushing type filter, the filtering medium is a cloth bag, the aperture is 5 mu m), is filtered, and then enters a second filtering unitAnd a second filtering unit 3 (a back-flushing filter, wherein a filtering medium is a metal sintered pipe, and the aperture is 1 mu m) filters the mixture, and then the mixture is introduced into a hydrogen peroxide preparation device by an anthraquinone method. The metal ion content of the regenerated working solution is shown in table 1.
In addition, when the adsorbent needs to be regenerated, the adsorbent reflux outlet is opened, the adsorbent is introduced into the adsorbent regeneration unit 4 (stirred tank), 2 mass% dilute hydrochloric acid with the volume 10 times that of the adsorbent is introduced into the adsorbent regeneration unit 4, the adsorbent is sufficiently stirred to regenerate the adsorbent, then the adsorbent reflux inlet is opened, and the regenerated adsorbent is introduced into the adsorption tower 1.
Example 2
The same apparatus as in example 1 was used to regenerate the hydrogen peroxide working solution of anthraquinone process from the company of Balinghouse, inc. of petrochemical engineering Ltd, except that the maximum diameter of the diameter-enlarged part 11 was 3000mm, the total concentration of anthraquinone compounds in the working solution was 135g/L, and the metal ion content was 10ppm. The metal ion content of the regenerated working solution is shown in table 1.
Example 3
The same apparatus as in example 1 was used to regenerate the hydrogen peroxide working fluid by anthraquinone process, produced by Balingdivision, inc., of petrochemical corporation, china, except that the maximum diameter of the diameter-enlarged part 11 was 4500mm, the total concentration of anthraquinone compounds in the working fluid was 135g/L, and the metal ion content was 10ppm. The metal ion content of the regenerated working solution is shown in table 1.
Example 4
The same apparatus as in example 1 was used to regenerate hydrogen peroxide working fluid by anthraquinone method from holy division, a company of petrochemical industries, ltd, china, except that the maximum diameter of the diameter-enlarged part 11 was 5000mm, the total concentration of anthraquinone compounds in the working fluid was 135g/L, and the metal ion content was 10ppm. The metal ion content of the regenerated working solution is shown in table 1.
The impurity removal rate in the following table 1 was calculated by the following formula:
removal rate (%) = (organic phase metal ion content before regeneration-organic phase metal ion content after regeneration)/organic phase metal ion content before regeneration 100%
The stability of the obtained hydrogen peroxide product is tested by adopting the stability test method specified in the industrial hydrogen peroxide of GB1616-2014, and the stability of the hydrogen peroxide product is high, so that the stability of the hydrogen peroxide in the oxidation process and the extraction process is also high. The method is to add a hydrogen peroxide product into a boiling water bath for 5 hours, and the calculation formula of the hydrogen peroxide stability is as follows:
hydrogen peroxide stability (%) = (hydrogen peroxide mass concentration before boiling water bath (%) -hydrogen peroxide mass concentration after boiling water bath (%)/hydrogen peroxide mass concentration before boiling water bath (%)
TABLE 1
The results show that the regeneration device for the hydrogen peroxide working solution prepared by the anthraquinone process can efficiently remove metal ions in the hydrogen peroxide working solution prepared by the anthraquinone process, and improve the safety and stability of hydrogen peroxide preparation.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. An anthraquinone process hydrogen peroxide working solution regenerating unit, characterized by that, the apparatus includes:
adsorption tower (1), filter unit (2) and adsorbent regeneration unit (4), adsorption tower (1) includes:
a liquid inlet at the bottom;
the tower body (10) is filled with an adsorbent, and the lower part of the side surface of the tower body is provided with an adsorbent backflow inlet;
the diameter expanding part (11) is positioned at the top end of the adsorption tower (1), the diameter of the diameter expanding part is larger than that of the tower body (10), the upper part of the side surface of the diameter expanding part is provided with an overflow port, and the lower part of the side surface of the diameter expanding part is provided with an adsorbent backflow outlet;
a liquid distributor (13) connected with the liquid inlet; and
a sleeve (12) connected to the liquid distributor (13) and ending in the enlarged diameter section (11),
wherein the overflow port is connected with the filtering unit (2); and the adsorbent regeneration unit (4) is respectively connected with the adsorbent backflow outlet and the adsorbent backflow inlet.
2. A device according to claim 1, wherein the ratio of the maximum diameter of the enlarged diameter part (11) to the diameter of the tower (10) is 1.1-2:1;
preferably, the tower body (10) and the diameter expanding part (11) are integrally formed.
3. The device according to claim 1, wherein the ratio of the diameter of the casing (12) to the diameter of the tower (10) is 0.3-0.8:1;
preferably, there is a gap between the sleeve (12) and the liquid distributor (13);
preferably, the height of the voids is 400-600mm.
4. The apparatus according to claim 1, wherein the adsorbent regeneration unit (4) is a stirred tank.
5. The device according to claim 1, wherein the number of filter units (2) is 1 or more, preferably more, more preferably 2-3;
preferably, the filter unit is a filter, and the filter medium is one or more of a cloth bag filter element, a chemical fiber filter element, a metal mesh filter element, a metal powder sintered filter element, a PP filter element, a line gap filter element and an activated carbon filter element;
preferably, the pore size of the filter medium is 0.1 to 100 μm.
6. Device according to claim 5, wherein, when the filtering units (2) are plural, the pore size of the filtering medium of the filtering unit located at the back is smaller than that of the filtering medium of the filtering unit located at the front.
7. The apparatus according to claim 1, wherein the top and bottom of the adsorption tower (1) are provided with rupture discs for pressure relief when the pressure in the tank is greater than a prescribed pressure.
8. The apparatus according to claim 1, wherein the apparatus further comprises a transfer unit (5), the transfer unit (5) being arranged on a line between the adsorbent regeneration unit (4) and the adsorbent inlet for transferring the adsorbent into the adsorption column (1).
9. The device of claim 1, wherein the adsorbent is one or more of a macroporous resin, a molecular sieve, activated carbon, a MOF material, hydrotalcite, diatomaceous earth, alumina microspheres, a cation exchange resin, and an anion exchange resin.
10. A regeneration method of working solution for preparing hydrogen peroxide by an anthraquinone process is characterized by comprising the step of introducing the working solution into the device of any one of claims 1 to 9 for regeneration when the content of metal ions in the working solution is more than 10ppm.
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