CN114522444A - Extraction equipment for hydrogen peroxide by anthraquinone process - Google Patents
Extraction equipment for hydrogen peroxide by anthraquinone process Download PDFInfo
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- CN114522444A CN114522444A CN202111605573.3A CN202111605573A CN114522444A CN 114522444 A CN114522444 A CN 114522444A CN 202111605573 A CN202111605573 A CN 202111605573A CN 114522444 A CN114522444 A CN 114522444A
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000000605 extraction Methods 0.000 title claims abstract description 74
- 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 26
- 150000004056 anthraquinones Chemical class 0.000 title claims abstract description 24
- 230000008569 process Effects 0.000 title claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000011324 bead Substances 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000005352 clarification Methods 0.000 claims abstract description 19
- 238000004062 sedimentation Methods 0.000 claims abstract description 17
- 239000000919 ceramic Substances 0.000 claims abstract description 14
- 238000004581 coalescence Methods 0.000 claims abstract description 8
- 238000012856 packing Methods 0.000 claims abstract description 8
- 230000001590 oxidative effect Effects 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 11
- 239000004744 fabric Substances 0.000 claims description 10
- 239000003365 glass fiber Substances 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000004806 packaging method and process Methods 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
- 238000000465 moulding Methods 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 230000006870 function Effects 0.000 abstract 1
- 230000005055 memory storage Effects 0.000 abstract 1
- 238000012546 transfer Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000012224 working solution Substances 0.000 description 5
- 238000011049 filling 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
- 238000005516 engineering process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001308 synthesis method Methods 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
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- -1 alkyl anthraquinone Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 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
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 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
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005272 metallurgy Methods 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
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method 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
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses extraction equipment of hydrogen peroxide by an anthraquinone process, 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 outward-expanding cavity structure and are fixedly arranged on two sides of the end surface of the extraction section, anti-back-mixing fillers are filled in the clarification section and the sedimentation section, and a pure water inlet, a dispersed phase outlet, an oxidation liquid inlet and a continuous phase outlet are respectively arranged in decibels of the clarification section and the sedimentation section; and a plurality of hollow bundling tubes which are arranged in parallel are arranged in the extraction section and are used as parallel flow channels of the dispersed phase and the continuous phase, a plurality of expansion joints are arranged on the hollow bundling tubes, the cross section of the inner cavity of each expansion joint is trapezoidal, inert ceramic beads are filled in the inner cavity of each expansion joint, and flow guide holes facing the dispersed phase coalescence packing layer are formed in the side wall of each expansion joint. The invention has high temperature control precision, intelligent control, real-time effect realization, memory storage function, stable performance and reduction of 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 hydrogen peroxide preparation process by an anthraquinone method.
Background
Hydrogen peroxide is an important green chemical, is often used as an oxidant in chemical production, generates water during chemical reaction in the using process due to unique performance, does not generate toxic and harmful products, and is widely applied to various fields of chemical synthesis, food, textile, metallurgy, electronics, agriculture, medicine, papermaking, national defense, environmental protection and the like, particularly emerging green chemical processes. Along with the increase of the demand of domestic markets for hydrogen peroxide, the production capacity of hydrogen peroxide is increased year by year, and people are prompted to pay more and more attention to research on hydrogen peroxide production technology
The main production methods of hydrogen peroxide mainly include a sulfate electrolysis method, an isopropanol oxidation method, a hydrogen-oxygen 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 condition is severe, the production cost is high, and the medicament consumption is large; the hydrogen-oxygen 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 hydrogen-oxygen synthesis method has greater potential safety hazard and higher requirements on flow management; for the above reasons, the practical application ratio of the above three methods is not high.
At present, the main production method of hydrogen peroxide is anthraquinone method, which uses alkylanthraquinone as working carrier, uses various organic substances with high solubility to anthraquinone as solvent to prepare working solution, and makes them produce hydrogenation reaction with hydrogen gas under the condition of a certain pressure and temperature and in the presence of palladium catalyst so as to obtain the correspondent hydrogenated solution of alkylanthraquinone. The hydrogenated liquid and oxygen in the air are subjected to oxidation reaction under certain temperature and pressure conditions to obtain an oxidation liquid, and the alkyl anthraquinone is oxidized and reduced into alkyl anthraquinone while hydrogen peroxide is generated. Hydrogen peroxide is extracted, purified and concentrated to obtain hydrogen peroxide products with different concentrations, and meanwhile, the working solution returns to the hydrogenation process again for recycling after dehydration and clay regeneration.
However, in the extraction and purification process in the existing method for preparing hydrogen peroxide by anthraquinone method, the oxidation liquid sent from the oxidation procedure is extracted in an extraction tower to obtain crude hydrogen peroxide solution. The crude hydrogen peroxide solution is treated by a purification tower to obtain dilute hydrogen peroxide, and then is concentrated to obtain a hydrogen peroxide product with the concentration of 50%. The quality of the extraction tower operation is directly related to the productivity, the product quality and the safe operation of the device. The design of hydrogen peroxide extraction and purification equipment in the prior art, such as a sieve plate extraction tower and a filler extraction tower, has defects, and the retention time of a dispersed phase in the equipment is short, so that the two-phase contact mass transfer time is short, and the mass transfer efficiency is low; meanwhile, because the interfacial tension of an oxidation liquid-water system is large, the traditional extraction equipment cannot effectively break the dispersed phase into small liquid drops, so that the mass transfer area is small, the extraction efficiency is poor, and the phenomenon of feed liquid back mixing exists, so that the extraction efficiency is low.
Patent CN 102583257A provides an extraction equipment of anthraquinone method preparation hydrogen peroxide solution, and this extraction equipment can effectively solve traditional extraction equipment mass transfer area, extraction efficiency poor, the problem of feed liquid backmixing, but its equipment structure is complicated relatively, and equipment is bulky, and the filler quantity is many, and the operation degree of difficulty is high in operation process, and the operation and maintenance cost is difficult to control.
Disclosure of Invention
The technical problem to be solved by the invention is to provide extraction equipment for hydrogen peroxide by an anthraquinone process, so as to solve the defects in the background technology.
The technical problem solved by the invention is realized by adopting the following technical scheme:
an extraction device of hydrogen peroxide by an anthraquinone process, the main body of the extraction device is a closed tower body structure, the tower body is divided into a clarification section, an extraction section and a sedimentation section from top to bottom, the clarification section is provided with a dispersed phase outlet and a pure water inlet, and the sedimentation section is provided with a continuous phase outlet and an oxidizing liquid inlet;
the clarification section and the sedimentation section are both of an outward-expanding cavity structure and are fixedly arranged on two sides of the end face of the extraction section, the expansion joint is internally provided with a volume cavity, and anti-back-mixing fillers for placing back mixing of a continuous phase and a disperse phase are respectively filled in the solvent cavity, the anti-back-mixing fillers are packaged in a filler support, and the anti-back-mixing fillers are subjected to end face packaging through glass fiber fabrics on the inner side of the filler support; the clarifying section and the settling section are respectively provided with a dispersed phase outlet and a continuous phase outlet at the outer side of a filler support, meanwhile, the inner sides of the clarifying section and the settling section corresponding to the filler support are respectively provided with a tubular distributor facing the extraction section, and the feed end of the tubular distributor is respectively connected with a pure water inlet and an oxidizing liquid inlet;
the extraction section comprises an outer shell, 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 tubes which are arranged in parallel are arranged in the outer shell and are used as parallel flow channels of a dispersed phase and a continuous phase, the inner diameter of a single tube of each hollow bundling tube is 100-120 mm, a plurality of expansion joints are arranged on a tube body, the cross section of an inner cavity of each expansion joint is trapezoidal, the upper bottom of the trapezoidal cross section is 1.2-1.5 times of the inner diameter of the bundling tube, the lower bottom of the trapezoidal cross section is 1.5-2.5 times of the inner diameter of the single tube of the bundling tube, 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 ceramic bead is 3-15 mm, the particle size 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 limit the inert ceramic beads through glass fiber cloth, wherein a separation sieve plate is further arranged on the glass fiber cloth on the upper surface to carry out sealing, a dispersed phase crushing filler layer is also formed on the separation sieve plate; meanwhile, the side wall of the expansion joint is also provided with a flow guide hole, a dispersed phase coalescence packing layer for sealing the outer surface of the expansion joint is arranged in the outer shell at the position of the expansion joint, and the flow guide hole faces to the dispersed phase coalescence packing layer.
As further injectd, the shell body of extraction section is integrated into one piece's metal cylinder, and its both sides terminal surface is provided with the end face flange respectively, and passes through the end face flange with clarification section and the section of subsiding carries out the terminal surface and can dismantle the connection to conveniently carry out the maintenance of equipment and maintain.
By way of further limitation, the sum of the cross-sectional areas of the hollow bundling tubes is 30-45% of the cross-sectional area of the volume part of the outer shell.
As a further limitation, the number of the expansion joints on the same hollow bundling pipe is 3-6.
As a further limitation, the expansion joints on the same hollow bundling tube are arranged at equal intervals.
As a further limitation, the pitch distance between the expansion joints adjacent to each other on the same hollow bundling pipe continuously increases from bottom to top.
As further restriction, the expansion joints on different hollow cluster pipes are arranged in a staggered mode so as to ensure the arrangement density of the hollow cluster pipes between the outer shells and the compactness of an extraction structure in the extraction section.
As a further limitation, the flow guide holes are obliquely arranged, form an elevation angle of 45-60 degrees with the horizontal plane, and disperse, gather and fill towards the outer side.
By way of further limitation, the inert ceramic beads are formed from inert alumina ceramic.
Has the advantages that: the extraction equipment of the hydrogen peroxide solution by the anthraquinone process has a compact structure, avoids the defect of overlarge and overlarge complicated extraction separator, can effectively improve the separation precision of the extraction tower, reduces the load of the subsequent process, simultaneously utilizes a plurality of single tubes of the cluster tube as the parallel flow channel of a dispersion phase and a continuous phase in the extraction process, utilizes the expansion joint structure to ensure that the working solution of the anthraquinone derivative containing hydrogen peroxide and water are contacted in the expansion joint structure, utilizes the inert ceramic beads with different particle sizes in the expansion joint structure to improve the contact surface area of the working solution of the anthraquinone derivative containing hydrogen peroxide and water at an oil-water interface, ensures that the hydrogen peroxide in the working solution of the anthraquinone derivative is dissolved or dispersed into the water phase from an oil phase as much as possible, increases the contact time of the two phases, effectively improves the extraction mass transfer efficiency, and simultaneously, the reducing inert ceramic beads can also effectively prevent the dispersion phase from flowing into the continuous guide flow channel, thereby reducing the back mixing of the dispersed phase and further increasing the extraction mass transfer efficiency so as to improve the extraction effect.
Drawings
Fig. 1 is a schematic structural diagram 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. continuous phase anti-back mixing filler; 4. a pure water inlet; 5. a continuous phase tubular distributor; 6. a connecting flange; 7. an extraction section; 8. a hollow bundling tube; 9. an expansion joint; 10. a dispersed phase tubular distributor; 11. an oxidizing liquid inlet; 12. dispersed phase anti-back mixing filler; 13. a settling section; 14. a continuous phase outlet; 15. dispersed phase crushing filler; 16. separating the sieve plate; 17. an expansion joint housing; 18. a dispersed phase coalescence filler layer; 19. a flow guide hole; 20. inert ceramic beads; 21 glass fiber cloth.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
In the following examples, it will be understood by those skilled in the art that, unless otherwise defined, 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. 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, the extraction equipment is a tower structure, the tower structure includes a clarification section 1, an extraction section 7 and a sedimentation section 13 which are formed independently, wherein an outer shell of the extraction section 7 is a cylindrical shell with openings at two ends, the end faces of the two ends of the cylindrical shell are opened and provided with a connecting flange 6 at the opening position, and the clarification section 1 and the sedimentation section 13 are connected with the extraction section 7 through bolts and sealing elements at the connecting flange 6 position.
In this embodiment, the clarification section 1 is an external-expanding cavity structure, the diameter of the cavity is 1.5 times of the diameter of the extraction section, the cavity is filled with continuous phase anti-back-mixing filler 3, the continuous phase anti-back-mixing filler 3 is packaged in a filler support, the upper surface and the lower surface of the inner side of the filler support are subjected to end face packaging through glass fiber fabrics, the upper part of the continuous phase anti-back-mixing filler 3 is provided with a dispersed phase outlet 2, the lower part of the continuous phase anti-back-mixing filler 3 is provided with a continuous phase tubular distributor 5 facing the extraction section 7, and the continuous phase tubular distributor 5 is externally connected with a pure water inlet 4.
Two circles of hollow cluster pipes 8 which are arranged in an annular shape are arranged in the extraction section 7, eight hollow cluster pipes 8 are arranged on the outer circle, four hollow cluster pipes 8 are arranged on the inner circle, the twelve hollow cluster 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.
For convenience of description, in fig. 1, only the section states of four hollow bundling tubes 8 on the same section are shown, each hollow bundling tube 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 the adjacent hollow bundling tubes 8 are arranged in a staggered manner, so that the hollow bundling tubes 8 are arranged more closely in the extraction section 7, the internal structure is more compact, the space utilization rate of a working area is improved, and the separation and extraction density in a unit space is higher. The hollow bundling tube 8 is a parallel flow channel of a dispersed 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 and is directly formed on the hollow bundling tube 8, a filling frame is sleeved on the outer side of the expansion joint 9, a dispersed phase aggregation filling layer 18 is filled in the filling frame, so that the dispersed phase aggregation filling layer 18 wraps the whole expansion joint 9, a cavity which is communicated with the hollow bundling tube 8 up and down is arranged in the expansion joint 9, the section of the cavity is trapezoidal, the upper bottom of the trapezoidal section is 130mm, the lower bottom of the trapezoidal section is 200mm, meanwhile, inert material beads 20 with different sizes are filled in the cavity, the inert material beads 20 are formed by inert alumina ceramics, the particle size range of the inert material beads is 5-15 mm, the inert material beads are laid in the cavity layer by layer, when the inert material beads are laid, large particles 20 are laid in the lower layer, small-particle inert material beads 20 are laid on the upper layer, the particle size of the inert material beads 20 is continuously reduced from bottom to top in the height direction of the expansion joint 9, the inert material beads 20 are limited by the upper surface and the lower surface of the expansion joint 9 through glass fiber cloth 21, and a separation sieve plate 16 and dispersed phase crushing filler 15 are further arranged on the glass fiber cloth 21 on the upper surface. In addition, a plurality of flow guide holes 19 are uniformly formed in the side wall corresponding to the expansion joint shell 17 of the expansion joint 9, and the flow guide holes 19 are obliquely arranged, form an elevation angle of 50 degrees with the horizontal plane and are directed towards the outside dispersed phase coalescence filler layer 18.
An external expanding cavity is arranged at the lower part of the extraction section 7 and is used as a sedimentation end 13, a filler support is also arranged in the sedimentation end 13, a disperse phase anti-back mixing filler 12 is filled in the filler support, a disperse phase tubular distributor 10 facing the extraction section 7 is correspondingly arranged at the upper part of the disperse phase anti-back mixing filler 12, the disperse phase tubular distributor 10 is externally connected with an oxidation liquid inlet 11, and a continuous phase outlet 14 is arranged at the lower part of the disperse phase anti-back mixing filler 12.
When the equipment of the embodiment is used, pure water is adopted to extract hydrogen peroxide in the oxidizing solution, the 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-back mixing filler 3, the water injection into the tower is stopped; meanwhile, the oxidizing solution is introduced into the oxidizing solution inlet 11, the temperature of the oxidizing solution is kept to be 40-50 ℃ and then injected into the tower through the dispersed phase tubular distributor 10, when the reflux of the dispersed phase (namely raffinate) appears at the top of the tower, clear water is injected into the tower again, the flow rates of the water phase (continuous phase) and the oil phase (dispersed phase oxidizing solution) are adjusted to the operation flow rate, and then the flow rate of the continuous phase outlet 14 at the bottom of the tower is adjusted to enable the oil-water interface of the clarification section 1 to be positioned between the continuous phase feeding distributor 5 and the continuous phase anti-back mixing filler 3 and keep stable, so that the stable and continuous operation of the extraction equipment is realized.
In the process, the hollow bundling tube 8 is used as a parallel flow channel of a dispersed phase and a continuous phase, in the process that the mixed flow moves from the settling section 13 to the clarifying section 1, separation is carried out once every time the mixed flow passes through the expansion joint 9, the dispersed phase oxidation liquid is separated once through the separation sieve plate 16 after separation, the mixed flow is separated into smaller particles and continuously floats to the top of the tower, and the smaller particles pass through the expansion joint 9 next time and are subjected to auxiliary contact and separation through the inert ceramic beads 20, the dispersed phase is continuously conveyed upwards through the hollow bundling tube 8 and finally flows out from the dispersed phase outlet 2, and raffinate is obtained; and the continuous phase is separated from the hollow bundling tube 8 through the diversion holes 19, flows downwards after passing through the dispersed phase coalescence packing layer 18 and finally flows out from the continuous phase outlet to obtain the extraction liquid.
In the above-mentioned equipment, the operation water phase flow rate is fixed at 10L/h, and the control oxidizing liquid flow rate is 500L/h, and its mass transfer unit height can be measured to be 0.21m, and under the condition of water phase flow rate of 10L/h and oxidizing liquid flow rate of 500L/h, the height of its mass transfer unit is 0.38m, so that its mass transfer efficiency can be raised by above 20%. Simultaneously, measuring the content of hydrogen peroxide in the extraction liquid and the content of hydrogen peroxide in the raffinate of the regular packing extraction tower under the same raw material and flow conditions under the extraction conditions, wherein the content of hydrogen peroxide in the extraction liquid and the content of hydrogen peroxide in the raffinate in the regular 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 liquid in the embodiment are 322.0g/L and 0.17g/L respectively, so the method of the embodiment also has more excellent extraction effect.
The foregoing shows and describes the general principles, essential 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, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. An extraction device of hydrogen peroxide by an anthraquinone process 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, the clarification section is provided with a dispersed phase outlet and a pure water inlet, and the sedimentation section is provided with a continuous phase outlet and an oxidizing liquid inlet;
the clarification section and the sedimentation section are both of an outward-expanding cavity structure and are fixedly arranged on two sides of the end face of the extraction section, the expansion joint is internally provided with a volume cavity, and anti-back-mixing fillers for placing back mixing of a continuous phase and a disperse phase are respectively filled in the solvent cavity, the anti-back-mixing fillers are packaged in a filler support, and the anti-back-mixing fillers are subjected to end face packaging through glass fiber fabrics on the inner side of the filler support; the clarifying section and the settling section are respectively provided with a dispersed phase outlet and a continuous phase outlet at the outer side of a filler support, meanwhile, the inner sides of the clarifying section and the settling section corresponding to the filler support are respectively provided with a tubular distributor facing the extraction section, and the feed end of the tubular distributor is respectively connected with a pure water inlet and an oxidizing liquid inlet;
the extraction section comprises an outer shell, 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 tubes which are arranged in parallel are arranged in the outer shell and are used as parallel flow channels of a dispersed phase and a continuous phase, the inner diameter of a single tube of each hollow bundling tube is 100-120 mm, a plurality of expansion joints are arranged on a tube body, the cross section of an inner cavity of each expansion joint is trapezoidal, the upper bottom of the trapezoidal cross section is 1.2-1.5 times of the inner diameter of the bundling tube, the lower bottom of the trapezoidal cross section is 1.5-2.5 times of the inner diameter of the single tube of the bundling tube, 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 ceramic bead is 3-15 mm, the particle size 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 limit the inert ceramic beads through glass fiber cloth, wherein a separation sieve plate is further arranged on the glass fiber cloth on the upper surface to carry out sealing, a dispersed phase crushing filler layer is also formed on the separation sieve plate; meanwhile, the side wall of the expansion joint is also provided with a flow guide hole, a dispersed phase coalescence packing layer for sealing the outer surface of the expansion joint is arranged in the outer shell at the position of the expansion joint, and the flow guide hole faces to the dispersed phase coalescence packing layer.
2. The extraction equipment for hydrogen peroxide through an anthraquinone process according to claim 1, wherein the outer shell of the extraction section is an integrally formed metal cylinder, end face flanges are respectively arranged on the end faces of the two sides of the extraction section, and the end faces of the extraction section are detachably connected with the clarification section and the sedimentation section through the end face flanges.
3. The extraction equipment for hydrogen peroxide through an anthraquinone process according to claim 1, wherein the sum of the cross-sectional areas of the hollow bundling tubes is 30-45% of the cross-sectional area of the volume part of the outer shell.
4. The extraction equipment for the hydrogen peroxide through the anthraquinone process according to claim 1, wherein the number of the expansion joints on the same hollow cluster pipe is 3-6.
5. An extraction apparatus of hydrogen peroxide by anthraquinone process according to claim 1, characterized in that expansion joints on the same hollow cluster pipe are arranged at equal intervals.
6. An extraction apparatus of hydrogen peroxide by anthraquinone process according to claim 1, characterized in that the pitch distance between adjacent expansion joints on the same hollow cluster pipe is continuously increased from bottom to top.
7. The extraction equipment for hydrogen peroxide through an anthraquinone process according to claim 1, wherein expansion joints on different hollow cluster pipes are arranged in a staggered manner.
8. The extraction equipment for hydrogen peroxide through an anthraquinone process according to claim 1, wherein the flow guide holes are obliquely arranged and form an elevation angle of 45-60 degrees with a horizontal plane.
9. The extraction equipment for hydrogen peroxide by an anthraquinone process according to claim 1, wherein said inert ceramic beads are made of inert alumina ceramic by molding.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU46677U1 (en) * | 2005-03-05 | 2005-07-27 | Российская Федерация в лице Федерального агентства по атомной энергии | DEVICE FOR EXTRACTION AND SEPARATION SEPARATION |
| CN202446855U (en) * | 2011-06-02 | 2012-09-26 | 上海睿思化工科技有限公司 | Efficient liquid-liquid extraction tower containing combined stuffing unit |
| CN102728099A (en) * | 2012-06-26 | 2012-10-17 | 中国科学院过程工程研究所 | Filler extraction tower for gradient fractionating separation of large phase ratio system, and extraction method thereof |
| CN109678119A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of hydrogen dioxide solution production by anthraquinone process system and hydrogen dioxide solution production by anthraquinone process method |
| CN109678120A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of hydrogenation reactor and method for hydrogenation of hydrogen dioxide solution production by anthraquinone process |
| 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 |
-
2021
- 2021-12-25 CN CN202111605573.3A patent/CN114522444B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU46677U1 (en) * | 2005-03-05 | 2005-07-27 | Российская Федерация в лице Федерального агентства по атомной энергии | DEVICE FOR EXTRACTION AND SEPARATION SEPARATION |
| CN202446855U (en) * | 2011-06-02 | 2012-09-26 | 上海睿思化工科技有限公司 | Efficient liquid-liquid extraction tower containing combined stuffing unit |
| CN102728099A (en) * | 2012-06-26 | 2012-10-17 | 中国科学院过程工程研究所 | Filler extraction tower for gradient fractionating separation of large phase ratio system, and extraction method thereof |
| CN109678119A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of hydrogen dioxide solution production by anthraquinone process system and hydrogen dioxide solution production by anthraquinone process method |
| CN109678120A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of hydrogenation reactor and method for hydrogenation of hydrogen dioxide solution production by anthraquinone process |
| 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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