CN114522444B - Extraction equipment for anthraquinone process hydrogen peroxide - Google Patents
Extraction equipment for anthraquinone process hydrogen peroxide Download PDFInfo
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- CN114522444B CN114522444B CN202111605573.3A CN202111605573A CN114522444B CN 114522444 B CN114522444 B CN 114522444B CN 202111605573 A CN202111605573 A CN 202111605573A CN 114522444 B CN114522444 B CN 114522444B
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000000605 extraction Methods 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 31
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 150000004056 anthraquinones Chemical class 0.000 title claims abstract description 22
- 230000008569 process Effects 0.000 title claims abstract description 19
- 239000000945 filler Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000004062 sedimentation Methods 0.000 claims abstract description 20
- 238000005352 clarification Methods 0.000 claims abstract description 19
- 239000011324 bead Substances 0.000 claims abstract description 18
- 230000001590 oxidative effect Effects 0.000 claims abstract description 16
- 239000000919 ceramic Substances 0.000 claims abstract description 13
- 239000004744 fabric Substances 0.000 claims description 14
- 239000003365 glass fiber Substances 0.000 claims description 13
- 238000012856 packing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 238000004220 aggregation Methods 0.000 claims description 7
- 230000002776 aggregation Effects 0.000 claims description 7
- 230000002265 prevention Effects 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 230000007423 decrease Effects 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 claims 1
- 230000005055 memory storage Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000012546 transfer Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000000926 separation method Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000012224 working solution Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- -1 alkyl anthraquinone Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0446—Juxtaposition of mixers-settlers
- B01D11/0449—Juxtaposition of mixers-settlers with stationary contacting elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
-
- 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
-
- 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
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses extraction equipment of anthraquinone process hydrogen peroxide, which comprises a closed tower body, wherein the closed tower body is divided into a clarification section, an extraction section and a sedimentation section from top to bottom, the clarification section and the sedimentation section are of an external expansion cavity structure, are fixedly arranged on two sides of the end surface of the extraction section, are filled with anti-back mixing fillers, and are provided with a pure water inlet, a disperse phase outlet, an oxidizing liquid inlet and a continuous phase outlet in a decibel manner; the extraction section is internally provided with a plurality of hollow bundling pipes which are arranged in parallel and serve as parallel flow channels of a disperse phase and a continuous phase, the hollow bundling pipes are provided with a plurality of expansion joints, the section of the inner cavity of each expansion joint is trapezoid, inert ceramic beads are filled in the inner cavity of each expansion joint, and the side wall of each expansion joint is provided with a diversion hole which faces to the disperse phase converging and filling layer. The intelligent temperature control system has high temperature control precision, intelligent control, real-time effectiveness, memory storage function, stable performance and reduced frequent cost.
Description
Technical Field
The invention relates to a hydrogen peroxide preparation technology in the technical field of chemical industry, in particular to hydrogen peroxide extraction equipment used in a process for preparing hydrogen peroxide by an anthraquinone method.
Background
Hydrogen peroxide is used as an important green chemical product and is often used as an oxidant in chemical production, water is generated when chemical reaction occurs in the using process due to the unique performance, and toxic and harmful products are not generated, so that the hydrogen peroxide is widely applied to various fields of chemical synthesis, food, textile, metallurgy, electronics, agriculture, medicine, papermaking, national defense, environmental protection and the like, and particularly the emerging green chemical technology. With the increase of hydrogen peroxide demand in domestic market, hydrogen peroxide production capacity is also increasing year by year, which promotes people to pay more attention to the research of hydrogen peroxide production technology
The main production methods of hydrogen peroxide mainly comprise a sulfate electrolysis method, an isopropanol oxidation method, an oxyhydrogen synthesis method, an anthraquinone method and the like, wherein the sulfate electrolysis method generates hydrogen peroxide by electrolyzing sulfate or bisulfate, but the energy consumption is high, and the equipment production capacity is low; in the isopropanol method, isopropanol is oxidized by air or oxygen in the presence of hydrogen peroxide or other peroxides to obtain a hydrogen peroxide product, but the production conditions are severe, the production cost is high, and the consumption of the medicament is large; the oxyhydrogen synthesis method is the most environment-friendly production process, hydrogen and oxygen are directly synthesized to generate hydrogen peroxide under the action of high pressure and a catalyst, but the potential safety hazard is large, and the requirement on flow management is high; for the above reasons, the actual application ratio of the above three methods is not high.
At present, the main production method of hydrogen peroxide is an anthraquinone method, which uses alkylanthraquinone as a working carrier, uses various organic matters with high solubility to anthraquinone as solvents to prepare working solution, and carries out hydrogenation reaction with hydrogen under certain pressure and temperature conditions and in the presence of palladium catalyst to obtain corresponding hydrogenation solution of alkylanthraquinone. And oxidizing the hydrogenated liquid with oxygen in air at a certain temperature and pressure to obtain oxidized liquid, wherein alkyl hydroanthraquinone is oxidized and reduced to alkyl anthraquinone and hydrogen peroxide is generated. Hydrogen peroxide is extracted, purified and concentrated to obtain hydrogen peroxide products with different concentrations, and meanwhile, the working solution is dehydrated and regenerated by clay and then returned to the hydrogenation process for recycling.
However, in the existing method for preparing hydrogen peroxide by the anthraquinone method, the oxidation liquid sent by the oxidation process is extracted in an extraction tower in the extraction and purification process to obtain a crude hydrogen peroxide solution. The crude hydrogen peroxide solution is treated by a purifying tower to obtain dilute hydrogen peroxide, and then a concentration procedure is carried out to obtain a hydrogen peroxide product with the concentration of 50%. The operation of the extraction column is directly related to the productivity, the product quality and the safe operation of the device. In the prior art, the design of hydrogen peroxide extraction and purification equipment such as a sieve plate extraction tower and a filler extraction tower has defects, and the residence time of a disperse phase in the equipment is shorter, so that the contact mass transfer time of two phases is shorter, and the mass transfer efficiency is lower; meanwhile, as the interfacial tension of an oxidation liquid-water system is larger, the traditional extraction equipment cannot effectively break the disperse phase into smaller liquid drops, so that the mass transfer area is smaller, the extraction efficiency is poorer, and meanwhile, the phenomenon of back mixing of feed liquid exists, so that the extraction efficiency is very low.
Patent CN 102583257A provides an extraction device for preparing hydrogen peroxide by an anthraquinone method, which can effectively solve the problems of mass transfer area, poor extraction efficiency and back mixing of feed liquid of the traditional extraction device, but has relatively complex device structure, large device volume, large filler consumption, high operation difficulty in the operation process and difficult control of operation and maintenance cost.
Disclosure of Invention
The technical problem solved by the invention is to provide extraction equipment for anthraquinone process hydrogen peroxide so as to solve the defects in the background technology.
The technical problems solved by the invention are realized by adopting the following technical scheme:
the extraction equipment of anthraquinone process hydrogen peroxide is characterized in that the main body of the equipment is of a closed tower structure, the tower is divided into a clarification section, an extraction section and a sedimentation section from top to bottom, a disperse phase outlet and a pure water inlet are arranged on the clarification section, and a continuous phase outlet and an oxidizing liquid inlet are arranged on the sedimentation section;
the clarifying section and the settling section are both of external expansion cavity structures and are fixedly arranged on two sides of the end face of the extracting section, the interior of the expansion joint is a volume cavity, back mixing prevention fillers for placing continuous phase and disperse phase back mixing are respectively filled in the solvent cavity, the back mixing prevention fillers are packaged in a filler bracket, and the end face of the back mixing prevention fillers is packaged at the inner side of the filler bracket through glass fiber fabrics; the clarification section and the sedimentation section are respectively provided with a disperse phase outlet and a continuous phase outlet at the outer sides of the filler brackets, and meanwhile, the inner sides of the clarification section and the sedimentation section, which correspond to the filler brackets, are respectively provided with a tubular distributor facing the extraction section, and the feeding ends of the tubular distributors are respectively connected with a pure water inlet and an oxidizing liquid inlet;
the extraction section comprises an outer shell, wherein the outer shell is a hollow cylindrical shell, two ends of the outer shell are open and are respectively communicated with the clarification section and the sedimentation section, a plurality of hollow bundling pipes which are arranged in parallel are arranged in the outer shell and serve as parallel flow channels of a disperse phase and a continuous phase, the inner diameter of a single pipe of each hollow bundling pipe is 100-120 mm, a plurality of expansion joints are arranged on the pipe body, the cross section of an inner cavity of each expansion joint is trapezoid, the upper bottom of the trapezoid cross section is 1.2-1.5 times of the inner diameter of each bundling pipe, the lower bottom of the trapezoid cross section is 1.5-2.5 times of the inner diameter of each bundling pipe, the height of each expansion joint is 70-90 mm, inert ceramic beads are filled in each expansion joint, the particle size of each inert material bead is 3-15 mm, the particle size of each expansion joint is continuously reduced from bottom to top in the height direction of each expansion joint, the upper surface and the lower surface of each expansion joint are limited by glass fiber cloth, a separation sieve plate is further arranged on the glass fiber cloth on the upper surface to be sealed, and a layer of dispersed phase crushing layer is formed on the separation sieve plate; meanwhile, a flow guide hole is formed in the side wall of the expansion joint, a disperse phase aggregation packing layer for sealing the outer surface of the expansion joint is arranged in the outer shell of the expansion joint, and the flow guide hole faces the disperse phase aggregation packing layer.
And as a further limitation, the outer shell of the extraction section is an integrally formed metal cylinder, end flanges are respectively arranged on the end surfaces of two sides of the outer shell, and the end surfaces of the outer shell are detachably connected with the clarification section and the sedimentation section through the end flanges so as to facilitate maintenance of equipment.
By way of further limitation, the sum of the cross-sectional areas of the hollow cluster tubes is 30-45% of the cross-sectional area of the volumetric portion of the outer shell.
As a further limitation, the number of expansion joints on the same hollow bundling tube is 3-6.
By way of further limitation, expansion joints on the same hollow cluster tube are equally spaced.
By way of further limitation, the pitch between adjacent expansion joints on the same hollow cluster tube increases continuously from bottom to top.
As further limitation, expansion joints on different hollow bundling pipes are arranged in a staggered mode so as to ensure the arrangement density of the hollow bundling pipes between the outer shell bodies and ensure the compactness of an extraction structure in the extraction section.
The guide holes are arranged obliquely, form an elevation angle of 45-60 degrees with the horizontal plane, and disperse, gather and fill outwards.
By way of further limitation, the inert ceramic beads are formed from an inert alumina ceramic.
The beneficial effects are that: the extraction equipment of the anthraquinone process hydrogen peroxide has compact structure, avoids the defect of overlarge and complicated extraction separator, can effectively improve the separation precision of an extraction tower, reduces the load of a subsequent process, simultaneously utilizes a plurality of bundling tube single tubes as parallel flow channels of a disperse phase and a continuous phase in the extraction process, utilizes an expansion joint structure to enable the anthraquinone derivative working solution containing hydrogen peroxide to contact with water in the parallel flow channels, utilizes inert ceramic beads with different particle diameters in the expansion joint structure to improve the contact surface area of the anthraquinone derivative working solution containing hydrogen peroxide and water at an oil-water interface, enables the hydrogen peroxide in the anthraquinone derivative working solution to be dissolved or dispersed into the water phase from an oil phase as much as possible, increases the contact time of two phases, effectively improves the extraction mass transfer efficiency, and simultaneously, the reducing inert ceramic beads can effectively prevent the disperse phase from flowing in the continuous guide flow channels, thereby reducing the back mixing of the disperse phase and further improving the extraction mass transfer efficiency to improve the extraction effect.
Drawings
Fig. 1 is a schematic structural view of a preferred embodiment of the present invention.
Fig. 2 is an enlarged detail view of the expansion joint portion of fig. 1.
Wherein: 1. a clarification section; 2. a dispersed phase outlet; 3. a continuous phase back-mix resistant filler; 4. a pure water inlet; 5. a continuous phase tubular distributor; 6. a connecting flange; 7. an extraction section; 8. a hollow cluster tube; 9. an expansion joint; 10. a dispersed phase tubular distributor; 11. an oxidizing liquid inlet; 12. a dispersed phase back-mixing preventing filler; 13. a sedimentation section; 14. a continuous phase outlet; 15. crushing filler by using a disperse phase; 16. separating the sieve plate; 17. an expansion joint housing; 18. a dispersed phase polymerization and packing layer; 19. a deflector aperture; 20. inert ceramic beads; 21 glass fiber cloth.
Detailed Description
The invention is further described in connection with the following embodiments in order to make the technical means, the creation features, the achievement of the purpose and the effect of the invention easy to understand.
In the following examples, it will be understood by those skilled in the art that all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs unless defined otherwise. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Referring to fig. 1 and 2, in the embodiment, the extraction device is a tower structure, and the tower structure includes an independently formed clarification section 1, an extraction section 7 and a sedimentation section 13, wherein the outer casing of the extraction section 7 is a cylindrical casing with two open ends, the two end faces of the cylindrical casing are open and are provided with connecting flanges 6 at the open positions, the clarification section 1 and the sedimentation section 13 are connected with the extraction section 7 at the positions of the connecting flanges 6 through bolts and sealing elements, and the structure can conveniently separate the three-section structure of the extraction device, thereby being beneficial to later maintenance and replacement of loss elements and consumable materials.
In this embodiment, the clarifying section 1 is an external expansion cavity structure, the diameter of the cavity is 1.5 times of the diameter of the extracting section, the cavity is filled with continuous phase back mixing preventing filler 3, the continuous phase back mixing preventing filler 3 is packaged in a filler bracket, the upper and lower surfaces of the inner side of the filler bracket are packaged by glass fiber fabrics, the upper and lower surfaces of the continuous phase back mixing preventing filler 3 are provided with dispersed phase outlets 2, the lower part of the continuous phase back mixing preventing filler 3 is provided with a continuous phase pipe type distributor 5 facing the extracting section 7, and the continuous phase pipe type distributor 5 is externally connected with a pure water inlet 4.
Two circles of hollow bundling pipes 8 are arranged in the extraction section 7 in an annular arrangement, eight hollow bundling pipes 8 are arranged in the outer circle, four hollow bundling pipes 8 are arranged in the inner circle, the twelve hollow bundling pipes 8 are arranged in parallel, and the sum of the cross-sectional areas accounts for 30% of the cross-sectional area of the volume part of the extraction section 7.
In fig. 1, for convenience of description, only the cross-sectional state of four hollow bundling pipes 8 on the same cross-section is shown, each hollow bundling pipe 8 is provided with four expansion joints 9, the four expansion joints 9 are arranged at equal intervals to facilitate equal proportion adjustment and replacement, and the expansion joints 9 on adjacent hollow bundling pipes 8 are arranged in a staggered manner, so that the arrangement of the hollow bundling pipes 8 is more compact in the extraction section 7, the internal structure is more compact, the space utilization rate of a working area is improved, and the separation extraction density in a unit space is higher. The hollow bundling tube 8 is a parallel flow channel of a disperse phase and a continuous phase, the inner diameter of a single tube is 100mm, the outer layer of the expansion joint 9 is an integrally formed cylindrical expansion joint, the hollow bundling tube 8 is directly formed, a filler frame is sleeved outside the expansion joint 9, a disperse phase aggregation and filler layer 18 is filled in the filler frame, so that the disperse phase aggregation and filler layer 18 wraps the whole expansion joint 9, a cavity communicated with the hollow bundling tube 8 from top to bottom is arranged in the expansion joint 9, the cross section of the cavity is trapezoid, the upper bottom of the trapezoid is 130mm, the lower bottom is 200mm, meanwhile, inert material beads 20 with different sizes are filled in the cavity, the inert material beads 20 are made of inert alumina ceramics, the particle size range of the inert material beads is 5-15 mm, when the inert material beads 20 are laid in the cavity layer by layer, the particle size of the inert material beads 20 are laid in the lower layer, the inert material beads 20 are continuously reduced from bottom to top in the height direction of the expansion joint 9, the upper surface of the expansion joint 9, the glass fiber cloth 21 is arranged on the glass fiber cloth, and the glass fiber cloth is further broken, and the glass fiber cloth is arranged on the upper surface of the glass filler layer 16 is separated by the glass fiber cloth, and the glass filler layer is arranged on the surface of the glass cloth 16. In addition, a plurality of diversion holes 19 are uniformly formed on the side wall corresponding to the expansion joint shell 17 of the expansion joint 9, and the diversion holes 19 are obliquely arranged, form an elevation angle of 50 degrees with the horizontal plane, and are gathered with a filler layer 18 towards the outside in a dispersed phase.
And an external expansion cavity is arranged at the lower part of the extraction section 7 to serve as a sedimentation end 13, a filler bracket is also arranged in the sedimentation end 13, a dispersed phase back-mixing preventing filler 12 is filled in the filler bracket, a dispersed phase tubular distributor 10 facing the extraction section 7 is correspondingly arranged at the upper part of the dispersed phase back-mixing preventing filler 12, the dispersed phase tubular distributor 10 is externally connected with an oxidizing liquid inlet 11, and a continuous phase outlet 14 is arranged at the lower part of the dispersed phase back-mixing preventing filler 12.
When the equipment of the embodiment is used, pure water is adopted to extract hydrogen peroxide in the oxidation liquid, pure water is introduced into the pure water inlet 4, the pure water is injected into the tower through the continuous phase tubular distributor 5 at normal temperature and normal pressure, and when the water phase interface is positioned between the continuous phase feeding distributor 5 and the continuous phase anti-backmixing filler 3, the water injection into the tower is stopped; meanwhile, by introducing the oxidizing liquid into the oxidizing liquid inlet 11, maintaining the oxidizing liquid temperature at 40-50 ℃ and injecting the oxidizing liquid into the tower through the disperse phase tubular distributor 10, when the reflux of the disperse phase (i.e. raffinate) occurs at the top of the tower, re-injecting clear water into the tower, regulating the flow of the water phase (continuous phase) and the oil phase (the disperse phase oxidizing liquid) to the operation flow, and then regulating the flow of the continuous phase outlet 14 at the bottom of the tower, so that the oil-water interface of the clarification section 1 is positioned between the continuous phase feeding distributor 5 and the continuous phase anti-backmixing filler 3, and the stable operation of the extraction equipment is realized.
In the process, the hollow cluster tube 8 is used as a parallel flow channel of the disperse phase and the continuous phase, in the process of moving the mixed flow from the sedimentation section 13 to the clarification section 1, the mixed flow is separated once through the expansion joint 9, the disperse phase oxidation liquid is separated once through the separation sieve plate 16 after the separation, is separated into smaller particles and continuously floats to the top of the tower, the next time of passing through the expansion joint 9, the inert ceramic beads 20 are used for auxiliary contact and separation, the disperse phase is continuously transported upwards through the hollow cluster tube 8, and finally flows out of the disperse phase outlet 2, and raffinate is obtained; the continuous phase is separated from the hollow cluster tube 8 through the diversion holes 19, flows downwards after passing through the dispersed phase aggregation and packing layer 18, and finally flows out of the outlet of the continuous phase to obtain the extract.
In the device, the flow rate of the water phase is fixed to be 10L/h, the flow rate of the oxidizing liquid is controlled to be 500L/h, the height of a mass transfer unit of the device can be measured to be 0.21m, and under the condition that the flow rate of the water phase is 10L/h and the flow rate of the oxidizing liquid is 500L/h, the height of the mass transfer unit of the regular packing extraction tower with the same size is 0.38m, so that the mass transfer efficiency of the device is improved by more than 20%. Simultaneously, under the extraction conditions, the content of hydrogen peroxide in the extracting solution and the content of hydrogen peroxide in the raffinate in the structured packing extraction tower are respectively measured under the same raw materials and flow conditions, wherein the content of hydrogen peroxide in the extracting solution and the content of hydrogen peroxide in the raffinate in the structured packing extraction tower are 310.0g/L and 0.28g/L respectively; the content of hydrogen peroxide in the extract liquid and the content of hydrogen peroxide in the raffinate are 322.0g/L and 0.17g/L respectively, so that the method of the embodiment also has more excellent extraction effect.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The extraction equipment of the anthraquinone process hydrogen peroxide comprises a closed tower body, and is characterized in that the closed tower body is divided into a clarification section, an extraction section and a sedimentation section from top to bottom, a disperse phase outlet and a pure water inlet are arranged on the clarification section, and a continuous phase outlet and an oxidizing liquid inlet are arranged on the sedimentation section;
the clarifying section and the settling section are both of external expansion cavity structures and are fixedly arranged on two sides of the end face of the extracting section, the interior of the expansion joint is a volume cavity, back mixing prevention fillers for placing continuous phase and disperse phase back mixing are respectively filled in the solvent cavity, the back mixing prevention fillers are packaged in a filler bracket, and the end face of the back mixing prevention fillers is packaged at the inner side of the filler bracket through glass fiber fabrics; the clarification section and the sedimentation section are respectively provided with a disperse phase outlet and a continuous phase outlet at the outer sides of the filler brackets, and meanwhile, the inner sides of the clarification section and the sedimentation section, which correspond to the filler brackets, are respectively provided with a tubular distributor facing the extraction section, and the feeding ends of the tubular distributors are respectively connected with a pure water inlet and an oxidizing liquid inlet;
the extraction section comprises an outer shell, wherein the outer shell is a hollow cylindrical shell, two ends of the outer shell are open and are respectively communicated with the clarification section and the sedimentation section, a plurality of hollow bundling pipes which are arranged in parallel are arranged in the outer shell and serve as parallel flow channels of a dispersion phase and a continuous phase, and the sum of the cross-sectional areas of the hollow bundling pipes is 30-45% of the cross-sectional area of a volume part of the outer shell; the inner diameter of a single tube of the hollow bundling tube is 100-120 mm, a plurality of expansion joints are arranged on the tube body, the cross section of an inner cavity of each expansion joint is trapezoid, the upper bottom of the trapezoid cross section is 1.2-1.5 times of the inner diameter of the bundling tube, the lower bottom is 1.5-2.5 times of the inner diameter of the single tube of the bundling tube, the height is 70-90 mm, inert ceramic beads are filled in the expansion joints, the particle size of each inert ceramic bead is 3-15 mm, the particle size of each expansion joint continuously decreases from bottom to top in the height direction, the inert ceramic beads are limited by glass fiber cloth on the upper surface and the lower surface of each expansion joint, a separating screen plate is further arranged on the glass fiber cloth on the upper surface for surface sealing, and a layer of dispersed phase crushing filler layer is further formed on the separating screen plate; meanwhile, a flow guide hole is formed in the side wall of the expansion joint, a disperse phase aggregation packing layer for sealing the outer surface of the expansion joint is arranged in the outer shell of the expansion joint, and the flow guide hole faces the disperse phase aggregation packing layer.
2. The extraction device for anthraquinone process hydrogen peroxide according to claim 1, wherein the outer shell of the extraction section is an integrally formed metal cylinder, and end surfaces of two sides of the outer shell are respectively provided with an end surface flange, and the end surfaces of the outer shell are detachably connected with the clarification section and the sedimentation section through the end surface flanges.
3. The extraction device for anthraquinone process hydrogen peroxide according to claim 1, wherein the number of expansion joints on the same hollow bundling tube is 3-6.
4. The extraction device for anthraquinone process hydrogen peroxide according to claim 1, wherein expansion joints on the same hollow bundling tube are arranged at equal intervals.
5. The extraction apparatus for anthraquinone process hydrogen peroxide according to claim 1, wherein the pitch between adjacent expansion joints on the same hollow cluster tube increases continuously from bottom to top.
6. The extraction device for anthraquinone process hydrogen peroxide according to claim 1, wherein expansion joints on different hollow bundling pipes are arranged in a staggered manner.
7. The extraction device for anthraquinone process hydrogen peroxide according to claim 1, wherein the diversion holes are obliquely arranged and form an elevation angle of 45-60 degrees with a horizontal plane.
8. The extraction device for anthraquinone-process hydrogen peroxide according to claim 1, wherein the inert ceramic beads are formed by molding inert alumina ceramics.
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| CN213253113U (en) * | 2020-07-13 | 2021-05-25 | 中国空分工程有限公司 | Extraction device for producing hydrogen peroxide by anthraquinone process |
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| RU46677U1 (en) * | 2005-03-05 | 2005-07-27 | Российская Федерация в лице Федерального агентства по атомной энергии | DEVICE FOR EXTRACTION AND SEPARATION SEPARATION |
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