CN114477096A - High-efficiency extraction process in hydrogen peroxide production process - Google Patents
High-efficiency extraction process in hydrogen peroxide production process Download PDFInfo
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- CN114477096A CN114477096A CN202210198524.0A CN202210198524A CN114477096A CN 114477096 A CN114477096 A CN 114477096A CN 202210198524 A CN202210198524 A CN 202210198524A CN 114477096 A CN114477096 A CN 114477096A
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 238000000605 extraction Methods 0.000 title claims abstract description 86
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 122
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000003513 alkali Substances 0.000 claims abstract description 39
- 230000001590 oxidative effect Effects 0.000 claims abstract description 21
- 238000000746 purification Methods 0.000 claims abstract description 21
- 238000003860 storage Methods 0.000 claims abstract description 21
- 230000033001 locomotion Effects 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 13
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 11
- 230000005540 biological transmission Effects 0.000 claims description 29
- 230000003647 oxidation Effects 0.000 claims description 29
- 238000007254 oxidation reaction Methods 0.000 claims description 29
- 239000012224 working solution Substances 0.000 claims description 22
- 230000008929 regeneration Effects 0.000 claims description 19
- 238000011069 regeneration method Methods 0.000 claims description 19
- 230000005484 gravity Effects 0.000 claims description 16
- 238000009826 distribution Methods 0.000 claims description 15
- 238000007667 floating Methods 0.000 claims description 14
- 239000000945 filler Substances 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- SJEBAWHUJDUKQK-UHFFFAOYSA-N 2-ethylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC=C3C(=O)C2=C1 SJEBAWHUJDUKQK-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- RJGDLRCDCYRQOQ-UHFFFAOYSA-N anthrone Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3CC2=C1 RJGDLRCDCYRQOQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011324 bead Substances 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 6
- 208000034699 Vitreous floaters Diseases 0.000 claims description 5
- 150000007513 acids Chemical class 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 239000007857 degradation product Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 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 claims description 4
- 150000004056 anthraquinones Chemical class 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 claims description 2
- 239000002689 soil Substances 0.000 claims 4
- 239000011148 porous material Substances 0.000 claims 1
- 239000004927 clay Substances 0.000 abstract description 11
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- HSKPJQYAHCKJQC-UHFFFAOYSA-N 1-ethylanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2CC HSKPJQYAHCKJQC-UHFFFAOYSA-N 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 10
- 238000002156 mixing Methods 0.000 description 9
- 239000007791 liquid phase Substances 0.000 description 5
- 230000016507 interphase Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- YEVQZPWSVWZAOB-UHFFFAOYSA-N 2-(bromomethyl)-1-iodo-4-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=C(I)C(CBr)=C1 YEVQZPWSVWZAOB-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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Classifications
-
- 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
-
- 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
- B01D36/006—Purge means
-
- 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
- B01D36/008—Means to filter or treat the separated liquid
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a high-efficiency extraction process in a hydrogen peroxide production process, relates to the technical field of hydrogen peroxide production, and aims to solve the problem that the existing hydrogen peroxide has low hydrogen peroxide extraction efficiency due to uneven overflow and dispersion and unstable interface in the extraction process to influence the content of raffinate hydrogen peroxide. Firstly, oxidizing liquid enters the lower end of an extraction cavity through an oxidizing liquid inlet pipe, and pure water is conveyed to the upper end of the extraction cavity through a water inlet pipe; step two, making the movable shaft provided with the sieve plate do reciprocating vertical and rotary motion, and after the concentration reaches a set concentration, the movable shaft enters the purification tower through the extraction liquid outlet pipe; thirdly, the extract liquid flows downwards in the purification tower, the heavy aromatic hydrocarbon enters a ceramic saddle ring through a pressure pump for countercurrent extraction, and the purified hydrogen peroxide enters a hydrogen peroxide storage tank for storage; step four to step six, separating alkali and moisture of the raffinate through an raffinate separator, a drying tower and an alkali separator; and step seven, conveying the mixture to a clay bed through a hose to regenerate the mixture into the ethyl anthraquinone.
Description
Technical Field
The invention relates to the technical field of hydrogen peroxide production, in particular to a high-efficiency extraction process in a hydrogen peroxide production process.
Background
The hydrogen peroxide is light blue viscous liquid, can be mixed and dissolved with water in any proportion, is a strong oxidant, is colorless transparent liquid, and the aqueous solution of the hydrogen peroxide is suitable for medical wound disinfection, environmental disinfection and food disinfection. The hydrogen peroxide is prepared and produced by adopting an anthraquinone method in the preparation mode, 2-ethyl anthraquinone is used as a carrier, heavy aromatic hydrocarbon and trioctyl phosphate are used as solvents to prepare working liquid, the working liquid is subjected to hydrogenation, oxidation, extraction, purification and other processes to prepare finished hydrogen peroxide, and the working liquid is recycled in a system, wherein the extraction system is used for extracting and recovering hydrogen peroxide from an oxidation liquid by using pure water to generate a hydrogen peroxide solution with a certain concentration, and the hydrogen peroxide solution is purified to generate a product.
However, in the existing production and extraction process of hydrogen peroxide, overflow and drop dispersion are not uniform, material liquid in a tower is seriously mixed back, an interface is unstable, the content of hydrogen peroxide in raffinate is high, the product yield is low, the aftertreatment load is increased, and the extraction efficiency of hydrogen peroxide is further influenced, so that the existing requirements are not met, and the efficient extraction process in the hydrogen peroxide production process is provided.
Disclosure of Invention
The invention aims to provide a high-efficiency extraction process in a hydrogen peroxide production process, which aims to solve the problem of low hydrogen peroxide extraction efficiency caused by the influence of uneven overflow dispersion and unstable interface on the content of raffinate hydrogen peroxide in the extraction process of hydrogen peroxide in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a high-efficiency extraction process in a hydrogen peroxide production process comprises the following steps:
firstly, oxidizing liquid is adjusted and controlled in flow and then enters the lower end of an extraction cavity through an oxidizing liquid inlet pipe, pure water flows out of a pure water tank, is added with phosphoric acid and is conveyed to the upper end of the extraction cavity through a pure water pump through a water inlet pipe;
secondly, under the transmission of a driving motor and a motor at the rear end of the first sector gear, a movable shaft provided with a sieve plate is driven to do reciprocating vertical and rotating motion, oxidation liquid is dispersed into fine liquid beads in the sieve plate by a floating ball bed, pure water and the oxidation liquid have different specific weights, enter the tower from the tower and are in countercurrent rapid contact with the oxidation liquid, the water liquid is mutually communicated through a first through hole and an inclined pipe in the sieve plate, the concentration of hydrogen peroxide is continuously improved from the top of the tower to the bottom of the tower, and the hydrogen peroxide enters the purification tower through an extract liquid outlet pipe after reaching a set concentration;
thirdly, a ceramic saddle ring is arranged in the purification tower, the extract liquid flows downwards in the purification tower, heavy aromatic hydrocarbon enters the ceramic saddle ring through a pressure pump and then enters the top of the purification tower, the heavy aromatic hydrocarbon enters the bottom of the purification tower through potential difference connection or discontinuity to perform countercurrent extraction with the extract liquid, anthraquinone dissolved in hydrogen peroxide is taken out, and the purified hydrogen peroxide enters a hydrogen peroxide storage tank to be stored;
step four, the raffinate above the extraction tower enters the lower part of the raffinate separator through a raffinate outlet pipe, floats to the upper layer of the tower due to specific gravity, and enters an alkali separator for treatment after the working solution comes out of the upper part of the drying tower;
spraying the working liquid through a spray head below the water distribution disc under the pressurization of a water pump, enabling the working liquid to be rapidly dispersed when the working liquid contacts the conical plate, and enabling the dispersed working liquid to contact the first filter plate and the second filter plate to separate solid impurities in the working liquid under the cooperation of the first filter plate and the second filter plate;
step six, the working solution for filtering impurities enters the separating cylinder through the guide groove, a motor at the rear end of the second sector gear is started, the separating cylinder is always in a shaking state, the potassium carbonate solution in specific gravity sinks to the bottom of the separating cylinder, the working solution with light specific gravity floats upwards, and the working solution above the separating cylinder is collected;
and seventhly, conveying the mixture to a clay bed through a hose, adsorbing an acidic compound by using activated alumina at a set temperature, dehydrogenating and regenerating the anthrone, the anthrone and other degradation products into 2-ethyl anthraquinone, collecting the 2-ethyl anthraquinone in a regeneration liquid storage tank, and injecting the regeneration liquid into an oxidation cycle again through a regeneration liquid outlet pipe.
In a further embodiment, the first step and the second step comprise extraction towers, an extraction cavity is arranged inside the extraction tower, a driving cavity is arranged above the extraction tower, a driving motor is fixedly arranged inside the driving cavity, a driving shaft is arranged on an output shaft of the driving motor, a movable shaft is arranged inside the driving shaft, the upper end of the movable shaft is limited by a limiting block, the limiting block is in sliding fit with a limiting groove in the inner wall of the driving shaft, the lower end of the movable shaft penetrates through the driving cavity and extends to the bottom of the extraction cavity, a sieve plate is fixedly arranged at one end of the movable shaft, the sieve plates are five in number, a water inlet pipe is arranged above one side of the extraction tower, a raffinate outlet pipe is arranged above the water inlet pipe, an oxidation liquid inlet pipe is arranged below one side of the extraction tower, and an extract liquid outlet pipe is arranged below the other side of the extraction tower, the upper end of the extraction cavity is provided with a water liquid anti-back-mixing filler which is positioned between the water inlet pipe and the raffinate outlet pipe, the lower end of the extraction cavity is provided with an oxidation liquid anti-back-mixing filler which is positioned between the oxidation liquid inlet pipe and the extract liquid outlet pipe, the drive shaft drives the movable shaft to rotate, the sieve plate rotates along with the movable shaft, the shearing force generated by the liquid enables the oxidation liquid to be broken into a plurality of fine liquid drops, strong vortex motion is generated in the liquid phase, and the interphase contact area and the mass transfer coefficient are increased.
In a further embodiment, a first sector gear is arranged below the driving cavity, two sets of toothed rings are symmetrically distributed outside the first sector gear, a transmission gear is arranged above the first sector gear and meshed with the toothed rings outside the first sector gear, a transmission cylinder is mounted at the upper end of the movable shaft and rotatably matched with the movable shaft through a bearing, a driving shaft is arranged on one side of the transmission cylinder, a first rack is arranged on one side of the driving shaft and meshed and connected with the transmission gear and the toothed rings outside the first sector gear respectively, so that the movable shaft drives the sieve plate to vertically reciprocate, two liquid phases flowing in a countercurrent manner in the tower are promoted to be sprayed and dispersed and mixed in sieve holes, contact mass transfer is carried out, the amplitude and frequency of reciprocating motion of the sieve plate can be adjusted, and the sieve plate has the advantages of large treatment capacity, high efficiency, The operation flexibility is large.
In further embodiment, the sieve includes pipe chute, ball-floating bed, bent cap, first through-hole, second through-hole and expand the pipe, the bent cap is the annular array and sets up in the inside below of sieve, and the pipe that expands that is located the sieve bottom is connected with the sieve, first through-hole is provided with the outside of bent cap, the second through-hole is the annular array and sets up in the inside of bent cap, and bent cap and sieve pass through the bolt fastening, ball-floating bed is located the inside of sieve, and ball-floating bed comprises a plurality of independent granule floaters, has increaseed the area of contact of oxidizing liquid with the pure water to improve the update speed on liquid pearl surface, and then improve extraction efficiency.
In a further embodiment, the fourth to sixth steps comprise an alkali separator, the upper end of the inside of the alkali separator is provided with a filter chamber, the inside of the filter chamber is provided with a first filter plate and a second filter plate from top to bottom in sequence, the first filter plate and the second filter plate are respectively matched with the inner wall of the drying tower in a sliding way through sliding chutes, the first filter plate and the second filter plate are respectively fixedly connected with the sliding chutes through second springs, the vibration motors are arranged on one side of the lower end surfaces of the first filter plate and the second filter plate, the number of filter holes of the second filter plate is larger than that of the first filter plate, the guide grooves are arranged below the second filter plate, the solid impurity to inside under the cooperation between them separates, opens vibrating motor afterwards, drives the filter through vibrating motor and takes place high frequency oscillation, further improves the filtration efficiency of filter.
In a further embodiment, a separating cylinder is arranged below the guide groove, the front side and the rear side of the separating cylinder are connected with an alkali separator through a connecting shaft, a first spring is fixedly arranged at the lower end of one side of the separating cylinder, a sliding rod is arranged at the lower end of the other side of the separating cylinder, one end of the sliding rod is close to the separating cylinder, the sliding rod is in sliding connection with the inner wall of the alkali separator, a second rack is arranged on the upper end face of the sliding rod, an installation box is fixedly arranged at one side of the alkali separator, a second sector gear is installed inside the installation box, a gear ring outside the second sector gear is in meshing connection with the second rack, the position of the separating cylinder is reset under the elastic action of the first spring, the separating cylinder is always in a shaking state along with the high-speed rotation of a motor, a potassium carbonate solution in specific gravity sinks to the bottom of the separating cylinder, and a working solution with light specific gravity floats up, and collecting the working fluid above.
In a further embodiment, the outside of alkali separator is provided with the drying tower, and the drying tower passes through pipe seal with alkali separator and is connected, and the one end of connecting pipe extends to the inside of alkali separator, the one end that the connecting pipe is located the inside of alkali separator is provided with the water distribution dish, the below of water distribution dish is provided with the shower nozzle that a plurality of equidistance distribute, the below of shower nozzle is provided with the conical plate, and the conical plate passes through the link with the water distribution dish and fixes.
In a further embodiment, a white clay bed is arranged below the other side of the alkali separator, the white clay bed is connected with the separation cylinder through a hose, the other end of the hose is located at the upper liquid level of the separation cylinder, a regeneration liquid storage tank is arranged below the white clay bed, a regeneration liquid outlet pipe is arranged on one side of the regeneration liquid storage tank, activated alumina is used for adsorbing acidic compounds at a set temperature, and anthrone, anthrone and other degradation products are dehydrogenated and regenerated into 2-ethyl anthraquinone.
In a further embodiment, one end of the raffinate outlet pipe is connected with a raffinate separator, one end of the extract outlet pipe is connected with a purification tower, and a hydrogen peroxide storage tank is connected below the purification tower.
In a further embodiment, the interior of the purification tower is provided with a ceramic saddle ring, and the interior of the ceramic saddle ring is filled with aromatic hydrocarbon gas.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention is characterized in that a movable sieve plate structure is arranged in a purification tower, oxidizing liquid enters an extraction cavity through an oxidizing liquid inlet pipe after the flow is regulated and controlled, pure water flows out of a pure water tank, is added with phosphoric acid and is conveyed to the upper end of the extraction cavity through a pure water pump by a water inlet pipe, a driving motor is started, a driving shaft drives a movable shaft to rotate, the sieve plate rotates along with the movable shaft, the oxidizing liquid is broken into a plurality of fine liquid drops by the shearing force generated by the liquid, strong vortex motion is generated in a liquid phase, the interphase contact area and the mass transfer coefficient are increased, meanwhile, a motor at the rear end of a first sector gear is started to drive the first sector gear to rotate clockwise, when the first sector gear is contacted with a first rack at one side, the first rack is moved upwards, so that a transmission cylinder synchronously moves upwards, and when the first sector gear rotates to a certain angle, the first rack at one side is not meshed with the first rack at one side, the device is meshed with a transmission gear above, the transmission gear is driven to move anticlockwise, and then the transmission cylinder is driven to move downwards under the meshing of the transmission gear and a first rack, the reciprocating motion of the transmission cylinder in the vertical direction is formed along with the continuous rotation of a first sector gear, the transmission cylinder is connected with a movable shaft through a bearing, the autorotation motion of the movable shaft cannot be influenced when the transmission cylinder drives the movable shaft to move up and down, therefore, in an extraction cavity, the movable shaft not only drives a plurality of sieve plates to rotate, but also drives the sieve plates to vertically reciprocate under the transmission of the first sector gear, two liquid phases flowing in a countercurrent mode in a tower are promoted to be sprayed at the sieve holes to cause dispersive mixing, contact mass transfer is carried out, the amplitude and the frequency of the reciprocating motion of the sieve plates can be adjusted, and the device has the advantages of large treatment capacity, high efficiency and large operation elasticity.
2. The invention improves the contact effect of the oxidizing liquid and water by adopting the sieve plate with a special structure, the lower oxidizing liquid is extruded into the sieve plate through the second through holes on the outer wall of the expanding pipe and the inclined pipe in the downward movement of the sieve plate, the upper pure water is extruded into the sieve plate through the first through hole in the cover disc in the upward movement of the sieve plate, countless liquid beads are formed in the sieve plate when the particle floating balls are contacted with the extruded oxidizing liquid by arranging the floating ball bed in the sieve plate, and meanwhile, the pure water can irregularly shake after entering the sieve plate, so that the contact area of the oxidizing liquid and the pure water is enlarged, the surface renewal speed of the liquid beads is improved, and the extraction efficiency is further improved.
3. According to the invention, the efficient separation mechanism is arranged in the alkali separator, raffinate above the extraction tower enters the lower part of the raffinate separator through the raffinate outlet pipe, floats to the upper layer of the tower due to specific gravity, and enters the alkali separator for treatment after coming out of the upper part of the drying tower, working solution is sprayed through the spray head below the water distribution disc under the pressurization of the water pump and contacts the conical plate to rapidly disperse the working solution, and the dispersed working solution contacts the first filter plate, so that the integral filtering uniformity can be improved.
4. In the invention, the movable separating cylinder is arranged below the inside of the alkali separator, the working solution for filtering impurities enters the separating cylinder through the guide groove, the motor at the rear end of the second sector gear is started, when the gear outside the second sector gear is contacted with the second rack on the upper end surface of the sliding rod, the sliding rod is driven to move towards the direction close to the separating cylinder, the position of the separating cylinder is reset under the elastic action of the first spring after the gear ring loses the meshing on the second rack, the separating cylinder is always in a shaking state along with the high-speed rotation of the motor, the potassium carbonate solution in specific gravity sinks to the bottom of the separating cylinder, the working solution with light specific gravity floats upwards, collecting the working solution above, conveying the working solution to a clay bed through a hose, adsorbing acidic compounds by using activated alumina at a set temperature, and dehydrogenating the anthrone, the anthrone and other degradation products to regenerate the 2-ethyl anthraquinone.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is an enlarged view of a portion of the area A of FIG. 1 in accordance with the present invention;
figure 3 is an exploded view of a screen panel of the present invention;
FIG. 4 is a schematic view of a screen deck structure of the present invention;
FIG. 5 is an enlarged view of a portion of the area B of FIG. 1 in accordance with the present invention;
FIG. 6 is an enlarged view of a portion of the invention in the area C of FIG. 1;
fig. 7 is a partial enlarged view of the area D in fig. 1 according to the present invention.
In the figure: 1. an extraction tower; 2. a purification tower; 3. a hydrogen peroxide storage tank; 4. an extract residue separator; 5. a drying tower; 6. an alkali separator; 7. a clay bed; 8. a regeneration liquid storage tank; 9. a drive chamber; 10. a drive motor; 11. an extraction chamber; 12. a movable shaft; 13. a sieve plate; 14. a water inlet pipe; 15. water liquid anti-back mixing filler; 16. feeding an oxidizing liquid into a pipe; 17. the oxidizing liquid is filled with anti-back mixing material; 18. an extract liquid outlet pipe; 19. a raffinate outlet pipe; 20. a transmission cylinder; 21. a first filter plate; 22. a second filter plate; 23. a guide groove; 24. a filter chamber; 25. a separation cylinder; 26. a connecting shaft; 27. a first spring; 28. a hose; 29. a regenerated liquid outlet pipe; 30. a drive shaft; 31. a limiting block; 32. a first rack; 33. a transmission gear; 34. a first sector gear; 35. an inclined tube; 36. a floating ball bed; 37. a cover plate; 38. a first through hole; 39. a second through hole; 40. expanding the pipe; 41. a water distribution plate; 42. a spray head; 43. a tapered plate; 44. a chute; 45. a second spring; 46. a vibration motor; 47. installing a box; 48. a second sector gear; 49. a slide bar; 50. a second rack.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1-7, an embodiment of the present invention is shown: a high-efficiency extraction process in a hydrogen peroxide production process comprises the following steps: firstly, oxidizing liquid is adjusted and controlled in flow rate and then enters the lower end of an extraction cavity 11 through an oxidizing liquid inlet pipe 16, pure water flows out of a pure water tank, is added with phosphoric acid and is conveyed to the upper end of the extraction cavity 11 through a pure water pump through a water inlet pipe 14; secondly, under the transmission of a driving motor 10 and a motor at the rear end of a first sector gear 34, a movable shaft provided with a sieve plate 13 is driven to do reciprocating vertical and rotating motion, oxidation liquid is dispersed into fine liquid beads in the sieve plate 13 by a floating ball bed 36, pure water and the oxidation liquid have different specific weights, enter the tower from the tower and are in countercurrent rapid contact with the oxidation liquid, the water liquid is mutually communicated through a first through hole 38 and an inclined pipe 35 in the sieve plate 13, the concentration of hydrogen peroxide is continuously improved from the top of the tower to the bottom of the tower, and the hydrogen peroxide enters a purification tower 2 through an extract outlet pipe after reaching a set concentration; thirdly, a ceramic saddle ring is arranged inside the purifying tower 2, the extract liquid flows downwards in the purifying tower 2, the heavy aromatic hydrocarbon enters the ceramic saddle ring through a pressure pump and then enters the top of the purifying tower 2, the heavy aromatic hydrocarbon enters the bottom of the purifying tower 2 through potential difference connection or discontinuity to perform countercurrent extraction with the extract liquid, anthraquinone dissolved in the hydrogen peroxide is taken out, and the purified hydrogen peroxide enters a hydrogen peroxide storage tank 3 for storage; step four, the raffinate above the extraction tower 1 enters the lower part of the raffinate separator 4 through a raffinate outlet pipe 19, floats to the upper layer of the tower due to specific gravity, and enters an alkali separator 6 for treatment after the working solution comes out of the upper part of the drying tower 5; fifthly, under the pressurization of a water pump, working liquid is sprayed through a spray head 42 below the water distribution disc 41 and contacts a conical plate 43, so that the working liquid is rapidly dispersed, and the dispersed working liquid contacts the first filter plate 21 and the second filter plate 22 to separate solid impurities in the working liquid under the cooperation of the first filter plate and the second filter plate; step six, the working solution for filtering impurities enters the separation cylinder 25 through the guide groove 23, a motor at the rear end of the second sector gear 48 is started, the separation cylinder 25 is in a shaking state all the time, the potassium carbonate solution in the specific gravity sinks to the bottom of the separation cylinder 25, the working solution with the light specific gravity floats upwards, and the working solution above the separation cylinder 25 is collected; and step seven, the waste water is conveyed to a clay bed 7 through a hose 28, an acidic compound is adsorbed by activated alumina at a set temperature, anthrone and other degradation products are dehydrogenated and regenerated into 2-ethyl anthraquinone, the 2-ethyl anthraquinone is collected in a regeneration liquid storage tank, and the regeneration liquid is injected into the oxidation cycle again through a regeneration liquid outlet pipe 29.
Further, the first step and the second step comprise an extraction tower 1, an extraction cavity 11 is arranged inside the extraction tower 1, a driving cavity 9 is arranged above the extraction tower 1, a driving motor 10 is fixedly arranged inside the driving cavity 9, a driving shaft 30 is arranged on an output shaft of the driving motor 10, a movable shaft 12 is arranged inside the driving shaft 30, the upper end of the movable shaft 12 and the driving shaft 30 are limited by a limiting block 31, the limiting block 31 is in sliding fit with a limiting groove on the inner wall of the driving shaft 30, the lower end of the movable shaft 12 penetrates through the driving cavity 9 and extends to the bottom of the extraction cavity 11, a sieve plate 13 is fixedly arranged at one end of the movable shaft 12, five sieve plates 13 are arranged, a water inlet pipe 14 is arranged above one side of the extraction tower 1, an extraction raffinate outlet pipe 19 is arranged above the water inlet pipe 14, an oxidation liquid inlet pipe 16 is arranged below one side of the extraction tower 1, an extraction liquid outlet pipe 18 is arranged below the other side of the extraction tower 1, the upper end of the extraction cavity 11 is provided with a water liquid anti-back mixing filler 15, the water liquid anti-back mixing filler 15 is positioned between a water inlet pipe 14 and a raffinate outlet pipe 19, the lower end of the extraction cavity 11 is provided with an oxidation liquid anti-back mixing filler 17, the oxidation liquid anti-back mixing filler 17 is positioned between an oxidation liquid inlet pipe 16 and an extract liquid outlet pipe 18, pure water flows out from a pure water tank, is added with phosphoric acid and is conveyed to the upper end of the extraction cavity 11 through the water inlet pipe 14 by a pure water pump, a driving motor 10 is started, a driving shaft 30 is utilized to drive a movable shaft 12 to rotate, a sieve plate 13 rotates along with the movable shaft 12, shearing force generated by liquid enables the oxidation liquid to be broken into a plurality of fine liquid drops, strong vortex motion is generated in a liquid phase, and the interphase contact area and the mass transfer coefficient are increased.
Further, a first sector gear 34 is arranged below the driving cavity 9, two sets of toothed rings are symmetrically arranged outside the first sector gear 34, a transmission gear 33 is arranged above the first sector gear 34, the transmission gear 33 is meshed and connected with the toothed rings outside the first sector gear 34, a transmission cylinder 20 is mounted at the upper end of the movable shaft 12, the transmission cylinder 20 is rotatably matched with the movable shaft 12 through a bearing, a driving shaft 30 is arranged on one side of the transmission cylinder 20, a first rack 32 is arranged on one side of the driving shaft 30, the first rack 32 is respectively meshed and connected with the transmission gear 33 and the toothed rings outside the first sector gear 34, a motor at the rear end of the first sector gear 34 drives the first sector gear 34 to rotate clockwise, when the first sector gear 34 contacts the first rack 32 on one side, the first rack 32 is enabled to move upwards, so that the transmission cylinder 20 moves upwards synchronously, first sector gear 34 loses the meshing to the first rack 32 of one side when rotatory to certain angle, mesh with top drive gear 33 mutually, it is counter-clockwise motion to drive gear 33, and then drive transmission cylinder 20 below the meshing of drive gear 33 and first rack 32 and move, along with the continuous rotation of first sector gear 34, form the reciprocating motion of transmission cylinder 20 on the vertical direction, because transmission cylinder 20 passes through the bearing with loose axle 12 and is connected, can not influence the rotation motion of loose axle 12 when transmission cylinder 20 drives loose axle 12 and reciprocates.
Furthermore, the sieve plate 13 comprises an inclined pipe 35, a floating ball bed 36, a cover disc 37, a first through hole 38, a second through hole 39 and an expanding pipe 40, the inclined pipe 35 is arranged below the inside of the sieve plate 13 in an annular array, the expanding pipe 40 positioned at the bottom of the sieve plate 13 is connected with the sieve plate 13, the first through hole 38 is provided with the outside of the inclined pipe 35, the second through hole 39 is arranged inside the cover disc 37 in an annular array, the cover disc 37 and the sieve plate 13 are fixed through bolts, the floating ball bed 36 is positioned inside the sieve plate 13 and consists of a plurality of independent particle floating balls, when the sieve plate 13 moves downwards, the lower oxidation liquid is extruded into the inside of the sieve plate 13 through the expanding pipe 40 and the second through hole 39 on the outer wall of the inclined pipe 35, when the sieve plate 13 moves upwards, the upper pure water is extruded into the sieve plate 13 through the first through hole 38 inside the cover disc 37, and when the particle floating balls in the floating ball bed 36 are contacted with the extruded oxidation liquid, countless liquid beads are formed inside the sieve plate 13, pure water can be irregularly shaken after entering the sieve plate, and the contact area of oxidizing liquid and the pure water is enlarged, so that the updating speed of the surfaces of the liquid beads is increased, and the extraction efficiency is improved.
Further, the fourth step to the sixth step include an alkali separator 6, a filter chamber 24 is arranged at the upper end inside the alkali separator 6, a first filter plate 21 and a second filter plate 22 are sequentially arranged inside the filter chamber 24 from top to bottom, the first filter plate 21 and the second filter plate 22 are respectively in sliding fit with the inner wall of the drying tower 5 through a chute 44, the first filter plate 21 and the second filter plate 22 are respectively fixedly connected with the chute 44 through a second spring 45, a vibration motor 46 is respectively arranged at one side of the lower end face of the first filter plate 21 and the second filter plate 22, the number of filter holes of the second filter plate 22 is larger than that of the first filter plate 21, a guide groove 23 is arranged below the second filter plate 22, the dispersed working fluid contacts the first filter plate 21, the integral filtering uniformity can be improved, because the second filter plate 22 has a larger number than that of the first filter plate 21, the solid impurities inside are separated under the cooperation of the first filter plate and the second filter plate, then, the vibration motor 46 is started, and the filter plate is driven by the vibration motor 46 to generate high-frequency oscillation, so that the filtering efficiency of the filter plate is further improved.
Furthermore, a separating cylinder 25 is arranged below the guide groove 23, the front side and the rear side of the separating cylinder 25 are connected with the alkali separator 6 through a connecting shaft 26, a first spring 27 is fixedly arranged at the lower end of one side of the separating cylinder 25, a sliding rod 49 is arranged at the lower end of the other side of the separating cylinder 25, one end of the sliding rod 49 is close to the separating cylinder 25, the sliding rod 49 is in sliding connection with the inner wall of the alkali separator 6, a second rack 50 is arranged on the upper end surface of the sliding rod 49, a mounting box 47 is fixedly arranged at one side of the alkali separator 6, a second sector gear 48 is arranged in the mounting box 47, a gear ring outside the second sector gear 48 is in meshing connection with the second rack 50, when a gear outside the second sector gear 48 is in contact with the second rack 50 on the upper end surface of the sliding rod 49, the sliding rod 49 is driven to move towards the direction close to the separating cylinder 25, and after the gear ring loses meshing on the second rack 50, the gear ring is elastically acted by the first spring 27, the position of the separating cylinder 25 is reset, the separating cylinder 25 is always in a shaking state along with the high-speed rotation of the motor, the potassium carbonate solution in specific gravity sinks to the bottom of the separating cylinder, the working solution with light specific gravity floats upwards, and the working solution above the separating cylinder is collected.
Further, a drying tower 5 is arranged outside the alkali separator 6, the drying tower 5 and the alkali separator 6 are hermetically connected through a pipeline, one end of a connecting pipe extends into the alkali separator 6, a water distribution disc 41 is arranged at one end of the connecting pipe located inside the alkali separator 6, a plurality of spray heads 42 distributed at equal intervals are arranged below the water distribution disc 41, a tapered plate 43 is arranged below the spray heads 42, and the tapered plate 43 and the water distribution disc 41 are fixed through a connecting frame.
Further, a white clay bed 7 is arranged below the other side of the alkali separator 6, the white clay bed 7 is connected with the separation cylinder 25 through a hose 28, the other end of the hose 28 is located at the upper liquid level of the separation cylinder 25, a regeneration liquid storage tank 8 is arranged below the white clay bed 7, and a regeneration liquid outlet pipe 29 is arranged on one side of the regeneration liquid storage tank 8.
Further, one end of the raffinate outlet pipe 19 is connected with a raffinate separator 4, one end of the extract outlet pipe 18 is connected with a purification tower 2, and a hydrogen peroxide storage tank 3 is connected below the purification tower 2.
Further, the inside of the purification tower 2 is provided with a ceramic saddle ring, and the inside of the ceramic saddle ring is filled with aromatic hydrocarbon gas.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. A high-efficiency extraction process in a hydrogen peroxide production process is characterized by comprising the following steps:
firstly, oxidizing liquid enters the lower end of an extraction cavity (11) through an oxidizing liquid inlet pipe (16) after the flow of the oxidizing liquid is regulated and controlled, and pure water flows out of a pure water tank, is added with phosphoric acid and is conveyed to the upper end of the extraction cavity (11) through a pure water pump through a water inlet pipe (14);
secondly, under the transmission of a driving motor (10) and a rear end motor of a first sector gear (34), a movable shaft provided with a sieve plate (13) is driven to do reciprocating vertical and rotating motion, oxidation liquid is dispersed into fine liquid beads in the sieve plate (13) by a floating ball bed (36), pure water and the oxidation liquid have different specific weights, the pure water enters the tower from the tower and is in countercurrent quick contact with the oxidation liquid, the water liquid is mutually communicated through a first through hole (38) and an inclined pipe (35) in the sieve plate (13), the concentration of hydrogen peroxide is continuously improved from the tower top to the tower bottom, and the hydrogen peroxide enters a purification tower (2) through an extract outlet pipe after reaching a set concentration;
thirdly, a ceramic saddle ring is arranged inside the purifying tower (2), the extract liquor flows downwards in the purifying tower (2), the heavy aromatic hydrocarbon enters the ceramic saddle ring through a pressure pump and then enters the top of the purifying tower (2), the heavy aromatic hydrocarbon enters the bottom of the purifying tower (2) through potential difference connection or discontinuity to perform countercurrent extraction with the extract liquor, anthraquinone dissolved in the hydrogen peroxide is taken out, and the purified hydrogen peroxide enters a hydrogen peroxide storage tank (3) for storage;
step four, the raffinate above the extraction tower (1) enters the lower part of a raffinate separator (4) through a raffinate outlet pipe (19), floats to the upper layer of the tower due to specific gravity, and enters an alkali separator (6) for treatment after working solution comes out from the upper part of a drying tower (5);
fifthly, under the pressurization of a water pump, working liquid is sprayed through a spray head (42) below a water distribution disc (41) and contacts a conical plate (43) to quickly disperse the working liquid, and the dispersed working liquid contacts a first filter plate (21) and a second filter plate (22) to separate solid impurities in the working liquid under the cooperation of the first filter plate and the second filter plate;
step six, the working solution for filtering impurities enters the separating cylinder (25) through the guide groove (23), a motor at the rear end of the second sector gear (48) is started, the separating cylinder (25) is in a shaking state all the time, the potassium carbonate solution in specific gravity sinks to the bottom of the separating cylinder (25), the working solution with light specific gravity floats upwards, and the working solution above the separating cylinder is collected;
and step seven, conveying the waste water to a white soil bed (7) through a hose (28), adsorbing acidic compounds by using activated alumina at a set temperature, dehydrogenating the anthrone and other degradation products to regenerate the 2-ethyl anthraquinone, collecting the 2-ethyl anthraquinone in a regeneration liquid storage tank, and injecting the regeneration liquid into an oxidation cycle again through a regeneration liquid outlet pipe (29).
2. The efficient extraction process in the hydrogen peroxide production process according to claim 1, which is characterized in that: the extraction device comprises an extraction tower (1) in the first step and the second step, an extraction cavity (11) is arranged inside the extraction tower (1), a driving cavity (9) is arranged above the extraction tower (1), a driving motor (10) is fixedly arranged inside the driving cavity (9), a driving shaft (30) is installed on an output shaft of the driving motor (10), a movable shaft (12) is installed inside the driving shaft (30), the upper end of the movable shaft (12) is limited by a limiting block (31) through the driving shaft (30), the limiting groove of the inner wall of the limiting block (31) and the inner wall of the driving shaft (30) are in sliding fit, the lower end of the movable shaft (12) penetrates through the driving cavity (9) and extends to the bottom of the extraction cavity (11), a sieve plate (13) is fixedly arranged at one end of the movable shaft (12) located in the extraction cavity (11), and five sieve plates (13) are arranged, the top of extraction tower (1) one side is provided with inlet tube (14), the top of inlet tube (14) is provided with raffinate exit tube (19), the below of extraction tower (1) one side is provided with oxidation liquid and advances pipe (16), the below of extraction tower (1) opposite side is provided with extract exit tube (18), the upper end of extraction chamber (11) is provided with water liquid anti-backmixing filler (15), and water liquid anti-backmixing filler (15) are located between inlet tube (14) and raffinate exit tube (19), the lower extreme of extraction chamber (11) is provided with oxidation liquid anti-backmixing filler (17), and oxidation liquid anti-backmixing filler (17) are located oxidation liquid and advance between pipe (16) and extract exit tube (18).
3. The efficient extraction process in the hydrogen peroxide production process according to claim 2, which is characterized in that: the below in drive chamber (9) is provided with first sector gear (34), and the outside of first sector gear (34) is provided with the ring gear of two sets of symmetric distributions, the top of first sector gear (34) is provided with drive gear (33), and drive gear (33) are connected with the outside ring gear meshing of first sector gear (34), driving cylinder (20) are installed to the upper end of loose axle (12), and driving cylinder (20) pass through bearing normal running fit with loose axle (12), one side of driving cylinder (20) is provided with drive shaft (30), one side of drive shaft (30) is provided with first rack (32), and first rack (32) are connected with the outside ring gear meshing of drive gear (33) and first sector gear (34) respectively.
4. The efficient extraction process in the hydrogen peroxide production process according to claim 2, which is characterized in that: sieve (13) are including slope pipe (35), floater bed (36), bent cap (37), first through-hole (38), second through-hole (39) and expand pipe (40), slope pipe (35) are the annular array and set up in the inside below of sieve (13), and are located bent cap (40) and sieve (13) of sieve (13) bottom and are connected, first through-hole (38) are provided with the outside of slope pipe (35), second through-hole (39) are the annular array and set up in the inside of bent cap (37), and bent cap (37) and sieve (13) pass through the bolt fastening, floater bed (36) are located the inside of sieve (13), and floater bed (36) comprise a plurality of independent granule floaters.
5. The efficient extraction process in the hydrogen peroxide production process according to claim 1, which is characterized in that: step four to including alkali separator (6) in step six, the inside upper end of alkali separator (6) is provided with filter chamber (24), the inside of filter chamber (24) has set gradually first filter (21) and second filter (22) from top to bottom, and first filter (21) and second filter (22) pass through spout (44) sliding fit with the inner wall of drying tower (5) respectively, first filter (21) and second filter (22) respectively with spout (44) between through second spring (45) fixed connection, vibrating motor (46) are all installed to one side of terminal surface under first filter (21) and second filter (22), the filtration pore number of second filter (22) is greater than first filter (21), the below of second filter (22) is provided with guide way (23).
6. The efficient extraction process in the hydrogen peroxide production process according to claim 5, which is characterized in that: the below of guide way (23) is provided with cylinder (25), and the front and back side of cylinder (25) is connected through connecting axle (26) with alkali separator (6), the fixed first spring (27) that is provided with of lower extreme of cylinder (25) one side, the lower extreme of cylinder (25) opposite side is provided with slide bar (49), and the one end and the cylinder (25) of slide bar (49) are pressed close to mutually, and the inner wall sliding connection of slide bar (49) and alkali separator (6), the up end of slide bar (49) is provided with second rack (50), one side of alkali separator (6) is fixed and is provided with install bin (47), the internally mounted of install bin (47) has second sector gear (48), and the outside ring gear of second sector gear (48) is connected with second rack (50) meshing.
7. The efficient extraction process in the hydrogen peroxide production process according to claim 5, which is characterized in that: the outside of alkali separator (6) is provided with drying tower (5), and drying tower (5) and alkali separator (6) pass through pipe seal and are connected, and the one end of connecting pipe extends to the inside of alkali separator (6), the one end that the connecting pipe is located alkali separator (6) inside is provided with water distribution dish (41), the below of water distribution dish (41) is provided with shower nozzle (42) that a plurality of equidistance distribute, the below of shower nozzle (42) is provided with tapered plate (43), and tapered plate (43) are fixed through the link with water distribution dish (41).
8. The efficient extraction process in the hydrogen peroxide production process according to claim 6, which is characterized in that: the alkali separator (6) below of opposite side is provided with white soil bed (7), is connected through hose (28) between white soil bed (7) and the cylinder (25), and the other end of hose (28) is located the last liquid level of cylinder (25), the below of white soil bed (7) is provided with regeneration liquid storage tank (8), one side of regeneration liquid storage tank (8) is provided with regeneration liquid exit tube (29).
9. The efficient extraction process in the hydrogen peroxide production process according to claim 2, which is characterized in that: one end of the raffinate outlet pipe (19) is connected with a raffinate separator (4), one end of the extract outlet pipe (18) is connected with a purification tower (2), and a hydrogen peroxide storage tank (3) is connected below the purification tower (2).
10. The efficient extraction process in the hydrogen peroxide production process according to claim 9, which is characterized in that: the inside of the purification tower (2) is provided with a ceramic saddle ring, and aromatic hydrocarbon gas is filled in the ceramic saddle ring.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117482716A (en) * | 2023-11-02 | 2024-02-02 | 江苏嘉宏新材料有限公司 | System for industrially improving concentration of hydrogen peroxide |
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Application publication date: 20220513 |