CN218962650U - Oxidation device for producing hydrogen peroxide - Google Patents
Oxidation device for producing hydrogen peroxide Download PDFInfo
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- CN218962650U CN218962650U CN202320000497.1U CN202320000497U CN218962650U CN 218962650 U CN218962650 U CN 218962650U CN 202320000497 U CN202320000497 U CN 202320000497U CN 218962650 U CN218962650 U CN 218962650U
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Abstract
The utility model discloses an oxidation device for producing hydrogen peroxide, which comprises an oxidation tower (101), wherein gas inlets A (111) and liquid inlets A (112) are respectively arranged on two sides of the lower part of the oxidation tower (101), a gas outlet A (113) is arranged at the top of the oxidation tower, a liquid outlet A (114) is arranged on the side surface of the upper part of the oxidation tower, a gas-liquid separator (103), a gas distributor (104) and arched tower plates (102) are arranged in the oxidation tower (101), the liquid inlets A (112) are positioned below the gas distributor (104), uniformly distributed holes are formed in the arched tower plates (102), and the adjacent arched tower plates (102) are alternately distributed. The air and the working solution flow upwards in parallel flow from the lower part of the oxidation tower and react in the oxidation tower, but the working solution flows in S-shaped cross flow in the oxidation tower due to the influence of the arched tower plates, so that the flow path of the working solution in the oxidation tower is prolonged, the gas and the liquid can be contacted more fully, and the conversion rate of the reaction is improved.
Description
Technical Field
The utility model relates to equipment and a process for gas-liquid two-phase reaction, in particular to an oxidation device for producing hydrogen peroxide.
Background
At present, the preparation of hydrogen peroxide at home and abroad mainly adopts an anthraquinone method preparation process, the process takes alkylanthraquinone (AQ, mainly 2-alkylanthraquinone) as a carrier, and proper solvents for respectively dissolving anthraquinone and anthrahydroquinone, substances for regulating the pH of the solution and the like are selected to jointly form working solution, and the whole preparation process generally comprises the procedures of hydrogenation, oxidation, extraction, purification and the like. The solvent for dissolving anthraquinone generally adopts heavy aromatic hydrocarbon extracted from petroleum industry, C9 aromatic hydrocarbon is adopted in China, and is a mixture containing trimethylbenzene, methyl ethylbenzene and the like, and C10 aromatic hydrocarbon is adopted in China. The solvent for dissolving anthrahydroquinone can be one or more selected from o-methylcyclohexyl acetate, diisobutyl methanol, trioctyl phosphate, tetrabutyl urea, etc. In the hydrogenation step, anthraquinones are hydrogenated to obtain anthrahydroquinones under the action of a catalyst, and the working solution becomes a hydrogenated solution. Then the hydrogenation solution is oxidized by the gas containing oxygen to H in the oxidation step 2 O 2 And anthraquinone oxidizing liquid, wherein the gas containing oxygen can be pure oxygen or oxygen-enriched air, and compressed air is selected in practice for reducing cost and safety.
In the oxidation process, the hydrogenation liquid and air generally react in a parallel flow upward flow mode, and the oxygen content in the air is only about 21%, the reaction pressure in the oxidation tower is 0.18-0.4 MPa, the reaction temperature is 40-55 ℃, the reaction condition is mild, the oxygen concentration at the gas-liquid interface is low, and the reaction speed is low. In order to improve the conversion rate of the reaction, the reaction is industrially carried out in a mode of connecting two towers in series or connecting three towers in series, wherein the towers are mainly empty towers except for a gas distributor, a redistributor and a heat exchanger, and even if the oxidation tower is subjected to long reaction time, the oxidation yield is still about 90-95%, and the tail oxygen content is about 6%. The prior industry has the defects of low oxidation yield, high tail oxygen content and the like.
Disclosure of Invention
The utility model aims to provide an oxidation device for producing hydrogen peroxide, wherein air and working solution of the device flow upwards in parallel flow in a macroscopic way after entering an oxidation tower from the lower part of the oxidation tower and react in the oxidation tower, but the working solution flows in S-shaped cross flow in the oxidation tower due to the influence of a bow-shaped tower plate, the flow path of the working solution in the oxidation tower is prolonged, and gas and liquid can be contacted more fully, so that the conversion rate of the reaction is improved; in addition, the tail oxygen content of the air at the outlet of the oxidation tower can be obviously reduced after passing through the pre-reactor, and the conversion rate of the hydrogenated liquid and the yield of the hydrogen peroxide can be obviously improved after the working solution at the outlet of the oxidation tower passes through the post-reactor, so that the economic benefit of the whole device is improved.
The aim of the utility model is realized by the following technical scheme:
an oxidation device for producing hydrogen peroxide comprises an oxidation tower 101, and is characterized in that gas inlets A111 and liquid inlets A112 are respectively arranged on two sides of the lower part of the oxidation tower 101, a gas outlet A113 is arranged at the top of the oxidation tower, a liquid outlet A114 is arranged on the side surface of the upper part of the oxidation tower, a gas-liquid separator 103, a gas distributor 104 and arched tower plates 102 are arranged in the oxidation tower 101, the liquid inlets A112 are positioned below the gas distributor 104, uniformly distributed holes are formed in the arched tower plates 102, and adjacent arched tower plates 102 are alternately distributed.
Preferably, the first arched tray 102 above the gas distributor 104 is 1-5 m away from the gas distributor 104, and the distance between adjacent arched trays 102 is 30 cm-200 cm.
Preferably, the chord 1021 length of the arched tower plate 102 accounts for 20% -90% of the diameter of the oxidation tower 101, and the area of the arched tower plate 102 accounts for more than half of the cross-sectional area of the oxidation tower 101.
Preferably, the holes uniformly distributed on the arched tower plate 102 are in a shape of a circle or a tongue, the size of the circular holes is 1 mm-30 mm, and the aperture ratio is 0.1% -10%; the aperture ratio of the tongue-shaped hole is 0.1% -10%.
Preferably, 1 to 10 gas inlets of the oxidation tower 101 are arranged in sequence from the bottom of the side surface of the oxidation tower 101 to the top; it is further preferable that the number of gas inlets is 3, which are respectively located at the bottom of the side face of the oxidation column 101, 1/2 height position and 3/4 height position of the side face of the oxidation column 101; preferably each gas inlet is provided with a gas distributor.
Preferably, the liquid feed flow rate is no more than 1 m/s.
Preferably, the gas distributor 104 is a gas distributor with circular holes, the size of the holes of the gas distributor 104 is 20 μm to 1000 μm, the perforation flow rate is 0.1 to m/s to 10 m/s, and more preferably the size of the holes is 20 μm to 100 μm.
Preferably, the gas distributor 104 is a gas distributor having a microporous structure, the microporous structure includes a metal sintered microporous tube, a ceramic sintered microporous tube, a microporous membrane tube or a microchannel with a pore diameter of 0.01-50 μm, and the gas distributor 104 enters the oxidation tower 101 as microbubbles through the microporous structure.
Preferably, the oxidation device is provided with a micro-bubble generator 201 and a post-reactor 202, the oxidation liquid flowing out from the liquid outlet A114 of the oxidation tower 101 and part of fresh air are mixed by the micro-bubble generator 201 to form micro-bubble flow, and then enter the post-reactor 202, and the gas coming out from the top of the post-reactor 202 is mixed with the fresh air and then enters the oxidation tower 101.
Preferably, the oxidizing liquid flowing out of the post-reactor 202 enters a heat exchanger or enters the next process.
Preferably, the fresh air entering the microbubble generator 201 is used in an amount of not more than 50%, preferably 10-30%, of the total air amount in the oxidation tower 101.
Preferably, the microbubble generator 201 is made of a venturi jet device, a metal sintering micro-pore tube, a ceramic sintering micro-pore tube, a micro-pore plate or a micro-pore membrane, or forms a microbubble flow by a pressurized dissolved air release method or a tangential rotational flow method.
Preferably, the oxidation device is provided with a pre-reactor 301, a liquid inlet B311 is arranged at the upper part of the side surface of the pre-reactor 301, a gas outlet B312 is arranged at the top, a gas inlet B313 is arranged at the bottom, a liquid outlet B314 is arranged at the lower part of the side surface, the gas from the oxidation tower 101 enters from the bottom of the pre-reactor 301 and reacts with the working solution, and the reacted gas enters an oxidation tail gas condenser; preferably 10-100% of the gas exiting the oxidation column 101 enters the pre-reactor 301.
Preferably, the main body of the pre-reactor 301 is a cuboid, the left side and the right side are arc surfaces, the liquid inlet B (311) and the liquid outlet B (314) are on the arc surfaces, the length of the cuboid is more than 3 times of the width, the pre-reactor 301 is relatively long and narrow along the flowing direction of the working solution, the working solution enters from one side of the upper part of the pre-reactor 301 and leaves from the other side of the lower part, the gas enters from the bottom of the pre-reactor 301, and the gas is distributed by the gas distributor at the bottom and then contacts with the working solution in a countercurrent mode to react, and then leaves from the top.
The utility model has the following beneficial effects:
(1) According to the utility model, the porous arched tower plates are added into the oxidation tower, so that the liquid main body and the gas flow in a cross flow manner between the arched tower plates under the condition of adopting the parallel flow upward flow of the gas phase and the liquid phase, the contact of the gas phase and the liquid phase can be increased, the mass transfer and the reaction are facilitated, the oxidation yield is improved, and the tail oxygen content is reduced; in addition, the utility model changes the traditional parallel flow oxidation tower from two towers or three towers to a single tower in series, which is beneficial to reducing the equipment size;
(2) The utility model additionally adds a pre-reactor and a post-reactor before and after the original oxidation tower; the interior of the post reactor is in a micro-bubble state, the contact area of the gas phase and the liquid phase is large, the oxidation yield is further improved, the tail oxygen content is reduced, the safety of an oxidation system of the hydrogen peroxide process by an anthraquinone method is improved, the tail oxygen content can be obviously reduced by the arrangement of the pre-reactor, and the economic benefit of the whole device is improved.
Drawings
FIG. 1 is a schematic view of an oxidation apparatus for producing hydrogen peroxide in accordance with the present utility model;
FIG. 2 is a schematic view of an oxidation unit containing a post-reactor for producing hydrogen peroxide in accordance with the present utility model;
FIG. 3 is a schematic view of an oxidation unit comprising a pre-reactor and a post-reactor for producing hydrogen peroxide in accordance with the present utility model;
FIG. 4 is a circular perforated arcuate tray of the present utility model;
FIG. 5 is an arcuate tray of the open-tongue aperture of the present utility model;
in the figure: 101. an oxidation tower; 102. arcuate trays; 103. a gas-liquid separator; 104. a gas distributor; 201. a microbubble generator; 202. a post-reactor; 301. a pre-reactor; 111. a gas inlet A; 112. a liquid inlet A; 113. a gas outlet A; 114. a liquid outlet A; 311. a liquid inlet B; 312. a gas outlet B; 313. a gas inlet B; 314. a liquid outlet B; 1021. the chords of the arcuate trays.
Detailed Description
The utility model is further illustrated by the following examples, which are given by way of illustration only and are not intended to limit the scope of the utility model.
In fig. 1, gas enters from a gas inlet a 111, is distributed by a gas distributor 104, enters into an oxidation tower 101, liquid enters into the oxidation tower 101 from a liquid inlet a 112, flows upwards in a macroscopic manner in parallel flow, reacts in the oxidation tower 101 at a reaction temperature of 40-65 ℃, has a reaction pressure of 0.18-0.6 MPa, and flows out of the oxidation tower 101 from a gas outlet a113 and a liquid outlet a114 respectively after passing through a gas-liquid separator 103.
In fig. 2, the oxidizing liquid flowing out of the liquid outlet a114 is mixed with a part of fresh air, which is not more than 50% of the total air amount of the oxidation tower 101, by the microbubble generator 201 to form a microbubble stream, and then enters the post-reactor 202 for further reaction, the oxidizing liquid for further reaction enters the heat exchanger or the next step, and the air for reaction in the post-reactor 202 is mixed with the air to be introduced into the oxidation tower 101 and then enters the oxidation tower 101.
In fig. 3, the working solution enters the pre-reactor 301 before entering the oxidation tower 101, 10-100% of the air coming out from the gas outlet a at the top of the oxidation tower 101 enters the bottom of the pre-reactor 301, is distributed by the gas distributor and then contacts with the working solution in a countercurrent manner to react, the reacted air enters the oxidation tail gas condenser, and the reacted working solution enters the oxidation tower 101.
Example 1
The oxidation device designed according to the utility model, as shown in fig. 1, comprises an oxidation tower 101, a arched tower plate 102, a gas distributor 104 and a gas-liquid separator 103, wherein a gas inlet A111 and a liquid inlet A112 are arranged on two sides of the lower part of the oxidation tower 101, air and hydrogenation liquid from the hydrogenation tower flow upwards in a macroscopic manner after entering the oxidation tower 101 from the gas inlet A111 and the liquid inlet A112 respectively, react in the oxidation tower, and flow out of the oxidation tower 101 from a gas outlet A113 and a liquid outlet A114 respectively after gas-liquid separation; the chord length of the arched tower plates is 20% of the diameter of the oxidation tower 101, the adjacent arched tower plates are alternately distributed in an S shape, and the distance between the adjacent arched tower plates is 200 cm; circular holes are uniformly distributed on the arched tower plate, the size of the holes is 5 mm, and the aperture ratio is 5%; the flow rate of the working solution is 930 and 930 m 3 And/h, the oxidation reaction temperature is 50 ℃, the air inlet pressure is 0.4 MPa, the apparent residence time of the working solution is 30 min, and the air flow rate is 30995 Nm 3 At/h, the oxidation yield was 96.0% and the tail oxygen content was 5.8%.
Example 2
Other design and operation steps were identical to those of example 1, except that the air flow was 29110 Nm 3 The result obtained at/h was an oxidation yield of 95.6% and a tail oxygen content of 4.7%.
Example 3
Other designs and operating procedures were consistent with example 1 except that the chord length of the arcuate tray 102 was 90% of the column diameter; the spacing between adjacent arched trays is 30 cm; air flow rate is 28877 Nm 3 At/h, the oxidation yield was 95.8% and the tail oxygen content was 4.5%.
Example 4
Other designs and operating procedures were consistent with example 1 except that the arcuate tray 102 had a chord length of 50% of the column diameter; the spacing between adjacent arched trays is 80 cm; air flow rate is 28682 Nm 3 At/h, the oxidation yield was 96.1% and the tail oxygen content was 4.3%.
Example 5
Other design and operation steps are the same as in example 4, except that after the working solution exits the oxidation tower 101, there is another post-reactor 202, the oxidation solution after exiting the gas-liquid separator 103 of the oxidation tower 101 is mixed with a part of fresh air by the micro-bubble generator 201 to form a micro-bubble flow, and the micro-bubble flow enters the post-reactor 202 for further reaction, the part of fresh air is 30% of the total air amount entering the oxidation tower 101, the further reacted oxidation solution enters the heat exchanger, and the air reacted in the post-reactor 202 is mixed with the air to enter the oxidation tower 101 and then enters the oxidation tower 101; air flow rate is 29310 Nm 3 At/h, the oxidation yield was 98.2% and the tail oxygen content was 4.3%.
Example 6
Other design and operation steps are the same as in example 4, except that after the working solution exits the oxidation tower 101, there is another post-reactor 202, the oxidation solution after exiting the gas-liquid separator 103 of the oxidation tower 101 is mixed with a part of fresh air by the micro bubble generator 201 to form a micro bubble flow, and the micro bubble flow enters the post-reactor 202 for further reaction, the part of fresh air is 15% of the total air amount entering the oxidation tower, the oxidation solution for further reaction enters the heat exchanger, and the air reacted in the post-reactor 202 is mixed with the air to enter the oxidation tower 101 and then enters the oxidation tower 101; air flow rate is 29310 Nm 3 At/h, the oxidation yield was 97.3% and the tail oxygen content was 4.5%.
Example 7
Other design and operation steps are the same as in example 4, except that after the working solution exits the oxidation tower 101, there is another post-reactor 202, and the oxidation solution exiting the gas-liquid separator 103 of the oxidation tower 101 is mixed with a part of fresh air through the microbubble generator 201 to form a microbubble stream, and the microbubble stream enters the post-reactor 202 for further reaction, where the part of fresh air enters the oxidation tower50% of the total air amount of the tower, the oxidation liquid of the further reaction enters a heat exchanger, and the air reacted in the post-reactor 202 is mixed with the air to be entered into the oxidation tower 101 and then enters the oxidation tower 101; air flow rate is 29310 Nm 3 At/h, the oxidation yield was 98.3% and the tail oxygen content was 4.3%.
Example 8
Other design and operation steps are the same as in example 5, except that the working solution is first a pre-reactor 301 before entering the oxidation tower 101, 50% of the air from the oxidation tower 101 enters the bottom of the pre-reactor 301, and after being distributed by the gas distributor, the working solution reacts with the air, and the reacted air enters the oxidation tail gas condenser; air flow rate is 26510 Nm 3 At/h, the oxidation yield was 98.2% and the tail oxygen content was 2.1%.
Comparative example 1
A conventional double-tower serial oxidation tower is selected, wherein the conventional double-tower serial oxidation tower comprises an upper tower and a lower tower, a gas-liquid separator is arranged at the top of each of the upper tower and the lower tower, hydrogenated liquid enters from the lower part of the upper tower, gas-liquid parallel flow upwards reacts, then enters the lower part of the lower tower after being separated by the gas-liquid separator, and after gas-liquid parallel flow upwards reacts again, leaves from the upper part of the lower tower after gas-liquid separation, and enters an extraction section; air enters from the lower part of the lower tower, enters the lower part of the upper tower after being subjected to gas-liquid separation from the upper part of the lower tower, and enters the tail gas treatment part after being subjected to gas-liquid separation from the upper part of the upper tower; the flow rate of the working solution is 930 and 930 m 3 And/h, the oxidation reaction temperature is 50 ℃, the air inlet pressure is 0.4 MPa, the apparent residence time of the working solution is 30 min, and the air flow rate is 30995 Nm 3 And/h, the oxidation yield is 94.0%, and the tail oxygen content is 6.2%.
Comparative example 2
The oxidation column 101 had no arcuate tray, and the rest was identical to example 1, and the flow rate of the working fluid was 930 m 3 And/h, the oxidation reaction temperature is 50 ℃, the air inlet pressure is 0.4 MPa, the apparent residence time of the working solution is 30 min, and the air flow rate is 30995 Nm 3 And/h, the oxidation yield is 84.1%, and the tail oxygen content is 8.0%.
Comparative example 3
Other designs and operating procedures were consistent with example 4, except thatThe working solution is discharged from the oxidation tower 101, then a post-reactor 202 is arranged, the oxidation solution discharged from the gas-liquid separator 103 of the oxidation tower 101 is mixed with part of fresh air through a micro-bubble generator 201 to form a micro-bubble flow, the micro-bubble flow enters the post-reactor 202 for further reaction, the part of fresh air is 60% of the total air quantity entering the oxidation tower, the further reacted oxidation solution enters a heat exchanger, and the air reacted in the post-reactor 202 is mixed with the air to be entering the oxidation tower 101 and then enters the oxidation tower 101; air flow rate is 29310 Nm 3 At/h, the oxidation yield was 97.7% and the tail oxygen content was 4.4%.
Claims (16)
1. The utility model provides an oxidation unit of production hydrogen peroxide, including oxidation tower (101), its characterized in that, oxidation tower (101) lower part both sides are provided with gas inlet A (111) and liquid inlet A (112) respectively, the top is provided with gas outlet A (113), upper portion side is provided with liquid outlet A (114), be provided with gas-liquid separator (103) in oxidation tower (101), gas distributor (104), bow-shaped column plate (102), liquid inlet A (112) are located the below of gas distributor (104), be provided with evenly distributed's hole on bow-shaped column plate (102), adjacent bow-shaped column plate (102) are distributed in turn.
2. The oxidation apparatus of claim 1, wherein a first arcuate tray (102) above the gas distributor (104) is 1-5 m from the gas distributor (104), and adjacent arcuate trays (102) are spaced apart by 30 cm-200 cm.
3. The oxidation apparatus according to claim 2, wherein the chord (1021) length of the arcuate tray (102) is 20% -90% of the column diameter, and the area of the arcuate tray (102) is more than half of the cross-sectional area of the oxidation column (101).
4. The oxidation device according to claim 1, wherein the holes on the arched tower plate (102) are circular or tongue-shaped, the circular holes have a size of 1 mm-30 mm and an opening ratio of 0.1% -10%; the aperture ratio of the tongue-shaped hole is 0.1% -10%.
5. The oxidation device according to claim 1, wherein the number of gas inlets of the oxidation tower (101) is 1-10, and the gas inlets are sequentially arranged from the bottom of the side surface of the oxidation tower (101) upwards.
6. An oxidation unit according to claim 5, characterized in that the number of gas inlets of the oxidation column (101) is 3, which are located at the bottom of the side of the oxidation column (101), at 1/2 height position and at 3/4 height position of the side of the oxidation column (101), respectively.
7. The oxidation apparatus according to claim 1, wherein the gas distributor (104) is a gas distributor with circular holes, the size of the holes of the gas distributor (104) is 20 μm to 1000 μm, and the perforation flow rate is 0.1 m/s to 10 m/s.
8. The oxidizing apparatus of claim 7, wherein the gas distributor (104) has a pore size of 20-100 μm.
9. The oxidation apparatus according to claim 1, wherein the gas distributor (104) is a gas distributor having a microporous structure including a metal sintered microporous tube, a ceramic sintered microporous tube, a microporous membrane or a microporous membrane tube having a pore diameter of 0.01 to 50 μm, and the gas distributor (104) introduces the gas into the oxidation tower (101) in the form of microbubbles through the microporous structure.
10. An oxidation unit according to any one of claims 1-9, characterized in that the oxidation unit is provided with a micro-bubble generator (201) and a post-reactor (202), that the oxidizing liquid flowing out of the liquid outlet a (114) of the oxidation tower (101) and part of the fresh air are mixed by the micro-bubble generator (201) to form a micro-bubble flow, and that the gas coming out of the top of the post-reactor (202) is mixed with the fresh air and then enters the oxidation tower (101).
11. An oxidation device according to claim 10, characterized in that the fresh air quantity entering the microbubble generator (201) is not more than 50% of the total air quantity of the oxidation tower (101).
12. An oxidation device according to claim 11, characterized in that the fresh air quantity entering the microbubble generator (201) is not more than 10-30% of the total air quantity of the oxidation tower (101).
13. The oxidizing apparatus of claim 10, wherein the microbubble generator (201) is made of a venturi jet, a metal sintered microporous tube, a ceramic sintered microporous tube, a microporous plate, or a microporous membrane, or forms a flow of microbubbles by a pressurized gas-dissolving gas-releasing method, a tangential swirling method.
14. The oxidizing apparatus according to claim 10, wherein the oxidizing apparatus is provided with a pre-reactor (301), a liquid inlet B (311) is provided at an upper side of the pre-reactor (301), a gas outlet B (312) is provided at a top, a gas inlet B (313) is provided at a bottom, a liquid outlet B (314) is provided at a lower side, and a gas discharged from the oxidizing tower (101) enters from the bottom of the pre-reactor (301) and reacts with the working fluid, and the reacted gas enters the oxidizing tail gas condenser.
15. An oxidation device according to claim 14, characterized in that 10-100% of the gas coming out of the oxidation column (101) enters the pre-reactor (301).
16. The oxidizing apparatus of claim 14, wherein the pre-reactor (301) body is a rectangular parallelepiped, the left and right sides are arc surfaces, the liquid inlet B (311) and the liquid outlet B (314) are on the arc surfaces, and the length of the rectangular parallelepiped is 3 times or more the width.
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| CN202320000497.1U CN218962650U (en) | 2023-01-02 | 2023-01-02 | Oxidation device for producing hydrogen peroxide |
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| CN202320000497.1U CN218962650U (en) | 2023-01-02 | 2023-01-02 | Oxidation device for producing hydrogen peroxide |
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