CN111717893A - Oxidation device and method for producing hydrogen peroxide by anthraquinone process - Google Patents
Oxidation device and method for producing hydrogen peroxide by anthraquinone process Download PDFInfo
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- CN111717893A CN111717893A CN201910223487.2A CN201910223487A CN111717893A CN 111717893 A CN111717893 A CN 111717893A CN 201910223487 A CN201910223487 A CN 201910223487A CN 111717893 A CN111717893 A CN 111717893A
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- C01—INORGANIC CHEMISTRY
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- 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
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Abstract
The invention relates to the field of hydrogen peroxide preparation, and discloses an oxidation device and method for producing hydrogen peroxide by an anthraquinone process. The oxidation device comprises an oxidation tower (4) and an oxidation liquid receiving tank (7); wherein the oxidation tower (4) is used for supplying oxygen-containing gas through a gas supply unit (3), introducing hydrogenated liquid through a hydrogenated liquid inlet (1) for carrying out oxidation reaction on the hydrogenated liquid and the oxygen-containing gas to obtain oxidation liquid containing hydrogen peroxide, and leading out and storing the oxidation liquid in an oxidation liquid receiving tank (7) through an oxidation liquid leading-out pipe (6). The device and the method have good safety, can ensure the safe and stable operation of the device, reasonably utilize oxygen generated by the decomposition of the hydrogen peroxide in the oxidizing liquid receiving tank, reduce the emission of VOCs and improve the environmental protection level of the device.
Description
Technical Field
The invention relates to the field of hydrogen peroxide preparation, in particular to an oxidation device and method for producing hydrogen peroxide by an anthraquinone method.
Background
Hydrogen peroxide is one of the main basic chemical products in the world, and the production process of hydrogen peroxide by an anthraquinone method is the main production method of the hydrogen peroxide. The production process of the anthraquinone method comprises the following steps: in the presence of a catalyst, under a certain temperature and pressure, anthraquinone in working solution prepared by alkyl anthraquinone and mixed organic solvent according to a certain proportion and hydrogen are subjected to hydrogenation reaction to produce corresponding hydrogen anthraquinone (hydrogenation stage), and at the moment, the working solution becomes hydrogenation solution; then, the hydrogenated liquid enters an oxidation tower, the hydroanthraquinone in the tower reacts with oxygen to produce anthraquinone and hydrogen peroxide (oxidation stage), and the hydrogenated liquid becomes oxidation liquid at the moment; and then, the oxidation liquid enters an extraction tower, pure water is used for extraction to obtain hydrogen peroxide water, namely hydrogen peroxide, and raffinate is subjected to post-treatment to become working liquid and is circulated back to the hydrogenation unit for continuous hydrogenation reaction.
In the existing production process, working liquid is hydrogenated and oxidized into oxidation liquid, the oxidation liquid enters an oxidation liquid receiving tank, the oxidation liquid contains hydrogen peroxide and can be decomposed to generate oxygen to form an oxygen-enriched environment, and the actual test data of a factory shows that the concentration of the oxygen in the oxidation liquid receiving tank can reach about 25%. Meanwhile, light components in the working solution can volatilize into a gas phase space to form a gas composition entering an explosion interval, and the danger is very high. For example, the explosion limit of mesitylene in air is 0.9% -7%, and the explosion limit is wider in an oxygen-rich environment. Therefore, safety measures need to be taken in the oxidizing liquid receiving tank to eliminate the potential safety hazard. The current treatment method is to set a nitrogen line at the top of the tank and continuously blow nitrogen to dilute the gas space, but the gas phase composition cannot be reduced below the lower explosion limit because the amount of nitrogen is too small.
Disclosure of Invention
The invention aims to solve the problem of gas phase blasting of an oxidizing liquid in a receiving tank in the prior art, and provides an oxidizing device and a method for producing hydrogen peroxide by an anthraquinone method.
In order to achieve the above object, the present invention provides an oxidation apparatus for producing hydrogen peroxide by an anthraquinone process, the oxidation apparatus comprising an oxidation tower and an oxidation liquid receiving tank; wherein the oxidation tower is used for supplying oxygen-containing gas through a gas supply unit, introducing hydrogenated liquid through a hydrogenated liquid inlet, carrying out oxidation reaction on the hydrogenated liquid and the oxygen-containing gas to obtain oxidation liquid containing hydrogen peroxide, and leading out and storing the oxidation liquid in the oxidation liquid receiving tank through an oxidation liquid leading-out pipe; and the tail gas outlet of the oxidizing liquid receiving tank is connected with an oxygen-containing gas inlet pipeline of the gas supply unit through an oxidizing liquid receiving tank tail gas circulating pipeline.
Preferably, an oxidation tower tail gas outlet pipe of the oxidation tower is connected with the oxidation liquid receiving tank through an oxidation tower tail gas circulating pipeline.
Preferably, the gas supply unit is an air compressor.
The second aspect of the present invention provides an oxidation method for producing hydrogen peroxide by the anthraquinone process, which is carried out by the above-mentioned oxidation apparatus of the present invention, comprising oxidizing a hydrogenated liquid to obtain an oxidized liquid containing hydrogen peroxide, and storing the oxidized liquid in an oxidized liquid receiving tank; wherein the off gas from the oxidizing liquid receiving tank is returned to the oxygen-containing gas introduction line before the gas supply means and supplied to the oxidation tower as the oxygen-containing gas.
Preferably, at least part of the tail gas of the oxidation tower is sent to the oxidation liquid receiving tank.
Preferably, the off-gas of the oxidation tower fed to the oxidation liquid receiver accounts for 5 to 10 vol% of the entire off-gas of the oxidation tower.
Preferably, the off-gas of the oxidation tower is fed to the oxidation liquid receiving tank so that the oxygen content in the gas phase space of the oxidation liquid receiving tank is 8 vol% or less, preferably 6 vol% or less.
Preferably, at least part of the off-gas of the oxidation tower is supplied to the oxidation tower as an oxygen-containing gas before being returned to the gas supply unit.
Through the technical scheme, the lean oxygen at the top of the oxidation tower is adopted to dilute the gas in the gas phase space at the top of the oxidation liquid receiving tank, and the diluted gas is introduced into the gas supply unit, so that the recycling of the oxygen is realized; meanwhile, the unorganized exhaust gas of the oxidizing liquid receiving tank is eliminated, and the requirement of environmental protection is met.
Drawings
FIG. 1 is a schematic view showing the structure of an oxidation apparatus for producing hydrogen peroxide by an anthraquinone process according to the present invention.
FIG. 2 is a schematic view showing the structure of another oxidation apparatus for producing hydrogen peroxide by the anthraquinone process according to the present invention.
Description of the reference numerals
1. Hydrogenation liquid inlet 2, oxygen-containing gas introduction line
3. Gas supply unit 4 and oxidation tower
5. An oxidation tower tail gas eduction tube 6 and an oxidation liquid eduction tube
7. Oxidizing liquid receiving tank 8 and oxidizing liquid receiving tank tail gas circulation pipeline
9. Oxidation liquid leading-out pipe 10 and oxidation tower tail gas circulation pipeline
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
As shown in figures 1-2, the oxidation device for producing hydrogen peroxide by anthraquinone process provided by the invention comprises an oxidation tower 4 and an oxidation liquid receiving tank 7; wherein, the oxidation tower 4 is used for supplying oxygen-containing gas through a gas supply unit 3, introducing hydrogenated liquid through a hydrogenated liquid inlet 1, carrying out oxidation reaction on the hydrogenated liquid and the oxygen-containing gas to obtain oxidation liquid containing hydrogen peroxide, and leading out and storing the oxidation liquid in an oxidation liquid receiving tank 7 through an oxidation liquid leading-out pipe 6; the tail gas outlet of the oxidizing liquid receiving tank 7 is connected to the oxygen-containing gas inlet line 2 of the gas supply unit 3 through an oxidizing liquid receiving tank tail gas circulation line 8.
In the present invention, the production of hydrogen peroxide by the anthraquinone process may be carried out using any conditions, catalysts, and the like that are currently available for the production of hydrogen peroxide, and is not particularly limited. In the present invention, the oxygen-containing gas is used for supplying oxygen gas required for the oxidation of the hydrogenated liquid, wherein the oxygen content is 21-30% by volume, and the rest of the components can be one or more of nitrogen, argon, helium and carbon dioxide, and nitrogen is preferred. The hydrogenation liquid refers to the liquid from the hydrogenation stage of the anthraquinone process for producing hydrogen peroxide, which contains hydroanthraquinone. The oxidation liquid is a liquid obtained by subjecting the hydrogenated liquid to an oxidation reaction in the oxidation tower 4, and contains alkylanthraquinone and hydrogen peroxide.
Specifically, the hydrogenated liquid is an organic solution generated by reacting the working liquid with hydrogen in the presence of a catalyst at a certain temperature and pressure. The working solution is prepared by dissolving alkyl anthraquinone in an organic solvent. The alkylanthraquinones are preferably 2-alkyl-9, 10-anthraquinones or their tetrahydroderivatives, where the alkyl substituent may contain 1 to 5 carbon atoms, such as methyl, ethyl, sec-butyl, tert-amyl, isoamyl and the like. The organic solvent is preferably a mixture of a non-polar compound and a polar compound. The nonpolar compound is preferably a petroleum fraction having a boiling point of 140 ℃ or higher, which contains mainly aromatic hydrocarbons having at least 9 carbon atoms, such as isomers of trimethylbenzene, isomers of tetramethylbenzene, tert-butylbenzene, isomers of methylnaphthalene and isomers of dimethylnaphthalene. The nonpolar compound is preferably a saturated alcohol (more preferably a saturated alcohol having 7 to 11 carbon atoms), a carboxylic acid ester, a phosphoric acid ester, a tetra-substituted urea, etc., such as diisobutylcarbinol, 3,5, 5-trimethylhexanol, isoheptanol, methylcyclohexyl acetate, heptyl acetate, butyl benzoate and ethyl heptanoate, trioctyl phosphate, tri-2-ethylbutyl phosphate, tri-2-ethylhexyl phosphate and tri-n-octyl phosphate, tetra-n-butylurea, etc. The hydrogenation solution is the solution obtained after the alkyl anthraquinone in the working solution is hydrogenated to generate the corresponding alkyl hydrogen anthraquinone.
In the present invention, as the conditions of the oxidation reaction in the oxidation tower 4, there may be included: the pressure is 0.1-1.0MPa, preferably 0.2-0.5 MPa; the temperature is 30-60 deg.C, preferably 40-55 deg.C.
In the present invention, most of the oxygen in the oxygen-containing gas is consumed by the oxidation reaction in the oxidation tower 4, the remaining oxygen content in the off gas from the oxidation tower 4 is generally 7% by volume or less, preferably 5% by volume or less, and the off gas from the oxidation tower 4 contains a small amount of components such as aromatic hydrocarbons due to volatilization of organic components in the oxidation tower 4.
In the present invention, the oxidizing solution receiving tank 7 is used for storing the oxidizing solution containing hydrogen peroxide and buffering the subsequent processes. Due to the decomposition of hydrogen peroxide, oxygen gas generated by the decomposition is present in the gas phase space of the oxidizing liquid receiving tank 7, so that there is a possibility that the oxidizing liquid receiving tank 7 may be explosive.
According to the present invention, by providing the oxidizing liquid receiving tank off-gas circulation line 8, the off-gas of the oxidizing liquid receiving tank 7 (i.e., the gas in the gas phase space of the oxidizing liquid receiving tank 7) can be returned to the gas supply means 3, thereby making it possible to utilize the oxygen in the off-gas of the oxidizing liquid receiving tank 7 in a rational manner.
According to a preferred embodiment of the present invention, the oxidation tower tail gas export pipe 5 of the oxidation tower 4 is connected with the oxidation liquid receiving tank 7 through an oxidation tower tail gas recycling pipeline 10. By providing this oxidation tower off-gas circulation line 10, the off-gas from the oxidation tower 4 can be introduced into the oxidation liquid receiving tank 7, and the gas in the gas phase space of the oxidation liquid receiving tank 7 can be diluted so that the oxygen concentration therein becomes 8% or less, preferably 5% or less, lower than the lower explosion limit of the gas in the gas phase space. Therefore, the safe operation of the oxidizing liquid receiving tank 7 is realized, the tail gas of the oxidation tower 4 is reasonably utilized, and the cost of introducing nitrogen is saved.
In the present invention, the gas supply means 3 is not particularly limited as long as it can supply the oxygen-containing gas to the oxidation tower 4, that is, it can compress the oxygen-containing gas to a pressure required for the oxidation tower 4. For example, a compressor, a supercharger, etc., may be mentioned, and an air compressor is preferable.
According to the present invention, preferably, the tail gas outlet pipe of the oxidation tower is further connected with a condenser and a gas-liquid separator, and organic components in the tail gas of the oxidation tower 4 can be removed through condensation and gas-liquid separation, so as to reduce pollution of the tail gas. More preferably, the temperature of the condensed tail gas is-5-10 ℃.
In the present invention, the positions where the gas supply unit 3 and the hydrogenation liquid inlet 1 are provided on the oxidation tower 4 are not particularly limited, and for example, as shown in fig. 2, the gas supply unit 3 and the hydrogenation liquid inlet 1 may be both provided at a lower portion (e.g., a bottom) of the oxidation tower 4 so that the oxygen-containing gas supplied from the gas supply unit 3 and the hydrogenation liquid supplied from the hydrogenation liquid inlet 1 are brought into co-current contact reaction; as shown in fig. 1, the gas supply unit 3 may be disposed at an upper portion (e.g., a top portion) of the oxidation tower 4, and the hydrogenation liquid inlet 1 may be disposed at a lower portion (e.g., a bottom portion) of the oxidation tower 4, so that the oxygen-containing gas supplied from the gas supply unit 3 and the hydrogenation liquid supplied from the hydrogenation liquid inlet 1 are subjected to a counter-current contact reaction. Among them, the above-mentioned co-current contact reaction method is preferably used, so that the reaction efficiency is improved, and the oxygen in the oxygen-containing gas is maximally contacted with the hydrogenated liquid for reaction, thereby achieving the purpose of reducing the oxygen content in the tail gas of the oxidation tower 4.
The second aspect of the present invention provides an oxidation method for producing hydrogen peroxide by the anthraquinone process, which is carried out by the above-mentioned oxidation apparatus of the present invention, comprising oxidizing a hydrogenated liquid to obtain an oxidized liquid containing hydrogen peroxide, and storing the oxidized liquid in an oxidized liquid receiver tank 7; wherein the oxygen-containing gas is supplied to the oxidation tower 4 as the oxygen-containing gas through the oxygen-containing gas introduction line 2 before the off gas of the oxidizing liquid receiving tank 7 is returned to the gas supply means 3.
Specifically, the process of introducing the oxygen-containing gas into the line 2 before returning the off gas from the oxidizing liquid receiver 7 to the gas supply unit 3 is performed through the oxidizing liquid receiver off gas circulation line 8. Thereby, the oxygen gas obtained by decomposing the oxidizing liquid with the hydrogen peroxide in the tank 7 is recycled to the oxidation tower 4.
According to a preferred embodiment of the present invention, at least a part of the off-gas of the oxidation tower 4 is sent to the oxidation liquid receiving tank 7. Specifically, the process is carried out via an oxidation column tail gas recycle line 10. Therefore, the tail gas of the oxidation tower 4 can be used for reducing the oxygen content in the gas phase space of the oxidation liquid receiving tank, and the safety is improved.
Preferably, the off gas from the oxidation tower 4 is fed to the oxidizing liquid receiving tank 7, so that the oxygen content in the gas phase space of the oxidizing liquid receiving tank 7 is 8% or less, preferably 5% or less. By setting the oxygen content within the above range, it is possible to ensure that the oxidizing liquid receiving tank 7 does not cause explosion risk.
According to a preferred embodiment of the present invention, the off-gas of the oxidation tower 4 fed to the oxidation liquid receiver 7 accounts for 5 to 10% by volume, preferably 7 to 10% by volume, of the whole off-gas of the oxidation tower 4. The specific ratio can be determined according to the oxygen content in the tail gas of the oxidation tower 4.
In order to satisfy the requirements of the oxidation reaction in the oxidation tower 4, preferably, an oxygen-containing gas, which may have an oxygen content of 21 to 30 vol%, more preferably 21 to 25 vol%, is introduced into the gas supply unit 3 through an oxygen-containing gas introduction line 2. The other gas contained in the oxygen-containing gas may be one or more of nitrogen, argon, helium, carbon dioxide, preferably nitrogen, in addition to oxygen. The oxygen-containing gas is preferably air.
In the present invention, the subsequent treatment step of the oxidizing solution is not limited at all, and may be a treatment that can be performed by a conventional method for separating hydrogen peroxide, such as extracting hydrogen peroxide in the oxidizing solution with pure water containing phosphoric acid to obtain a hydrogen peroxide solution having a certain concentration.
The present invention will be described in detail below by way of examples.
Example 1
The hydrogen peroxide was produced using an oxidation apparatus for producing hydrogen peroxide by the anthraquinone process as follows.
As shown in fig. 1, the oxidation apparatus comprises an oxidation tower 4 and an oxidation liquid receiving tank 7; wherein, the oxidation tower 4 is used for supplying oxygen-containing gas through a gas supply unit 3 (an air compressor), introducing hydrogenated liquid through a hydrogenated liquid inlet 1, carrying out oxidation reaction on the hydrogenated liquid and the oxygen-containing gas to obtain oxidation liquid containing hydrogen peroxide, and leading out and storing the oxidation liquid in an oxidation liquid receiving tank 7 through an oxidation liquid leading-out pipe 6;
the gas supply unit 3 is arranged at the top of the oxidation tower 4, and the hydrogenated liquid inlet 1 is arranged at the bottom of the oxidation tower 4;
the tail gas outlet of the oxidizing liquid receiving tank 7 is connected with the oxygen-containing gas inlet pipeline 2 of the gas supply unit 3 through an oxidizing liquid receiving tank tail gas circulating pipeline 8;
the tail gas delivery pipe 5 of the oxidation tower 4 is provided with a branch which is connected with the oxidation liquid receiving tank 7 through an oxidation tower tail gas circulating pipeline 10.
The oxidation process of the present invention comprises: by using the device, under the conditions that the temperature is 50 ℃ and the pressure is 0.2MPa, the hydrogenated liquid flows from top to bottom in the tower, and the oxygen-containing gas flows from bottom to top in the tower, so that the hydrogenated liquid and the oxygen-containing gas are subjected to a countercurrent oxidation reaction to obtain an oxidation liquid containing hydrogen peroxide, and the oxidation liquid is stored in an oxidation liquid receiving tank 7; wherein the off gas from the oxidation liquid receiver 7 is supplied as an oxygen-containing gas to the oxidation tower 4 before being returned to the gas supply unit 3 through an oxidation liquid receiver off gas circulation line 8;
5% of the tail gas of the oxidation tower 4 is sent into the oxidation liquid receiving tank 7 through an oxidation tower tail gas circulating pipeline 10, and the oxygen content in the gas phase space of the oxidation liquid receiving tank 7 is adjusted to be 7%;
air is introduced from the oxygen-containing gas introduction line 2, mixed with the tail gas from the oxidizing liquid receiving tank 7, introduced into the oxidation tower 4, subjected to an oxidation reaction with the hydrogenated liquid from the hydrogenated liquid inlet to obtain an oxidized liquid, and introduced into the oxidizing liquid receiving tank 7 for storage.
Example 2
Hydrogen peroxide was produced using the method of example 1, except that an oxidation unit as shown in fig. 2 was used, which was different from the oxidation unit shown in fig. 1 in that: the gas supply unit 3 and the hydrogenation liquid inlet 1 are both arranged at the bottom of the oxidation tower 4; in the reaction process, the hydrogenated liquid and the oxygen-containing gas flow from bottom to top in the tower, so that the hydrogenated liquid and the oxygen-containing gas are subjected to cocurrent oxidation reaction to obtain the oxidation liquid containing hydrogen peroxide.
By using the oxidation apparatus and method for producing hydrogen peroxide by the anthraquinone process according to the above embodiments 1 to 2, hydrogen peroxide can be prepared, and compared with the existing oxidation apparatus and method in which no tail gas of the oxidation liquid receiving tank is recycled, the oxidation liquid receiving tank can be ensured to operate within a safe oxygen content range without using additional purchased nitrogen, the safety of the apparatus is ensured, and the steps of treating the tail gas are reduced by reasonably utilizing oxygen generated by decomposition of hydrogen peroxide.
In addition, the method of the embodiment 1 can realize the oxidation reaction of the hydrogenation liquid and the oxygen-containing gas by countercurrent contact, thereby improving the reaction efficiency and the oxygen utilization rate, reducing the oxygen content in the waste gas of the oxidation tower and being more beneficial to the reaction.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. An oxidation device for producing hydrogen peroxide by an anthraquinone process is characterized by comprising an oxidation tower (4) and an oxidation liquid receiving tank (7);
wherein the oxidation tower (4) is used for supplying oxygen-containing gas through a gas supply unit (3), introducing hydrogenated liquid through a hydrogenated liquid inlet (1), carrying out oxidation reaction on the hydrogenated liquid and the oxygen-containing gas to obtain oxidation liquid containing hydrogen peroxide, and leading out and storing the oxidation liquid in an oxidation liquid receiving tank (7) through an oxidation liquid leading-out pipe (6);
the tail gas outlet of the oxidizing liquid receiving tank (7) is connected with the oxygen-containing gas inlet pipeline (2) of the gas supply unit (3) through an oxidizing liquid receiving tank tail gas circulating pipeline (8).
2. An oxidation unit according to claim 1, wherein the oxidation tower tail gas outlet pipe (5) of the oxidation tower (4) is connected to the oxidation liquid receiving tank (7) through an oxidation tower tail gas circulation line (10).
3. An oxidation arrangement according to claim 1 or 2, wherein the gas supply unit (3) is an air compressor.
4. An oxidation process for producing hydrogen peroxide by an anthraquinone process, which is carried out by the oxidation apparatus according to claim 1 or 2, comprising oxidizing a hydrogenated liquid to obtain an oxidized liquid containing hydrogen peroxide, and storing the oxidized liquid in an oxidized liquid receiver tank (7);
wherein the oxygen-containing gas is supplied as an oxygen-containing gas to the oxidation tower (4) through an oxygen-containing gas introduction line (2) before the off gas from the oxidizing liquid receiving tank (7) is returned to the gas supply means (3).
5. An oxidation process according to claim 4, wherein at least part of the off-gas of the oxidation tower (4) is sent to the oxidizing liquid receiving tank (7).
6. An oxidation process according to claim 5, wherein the off-gas fed to said oxidation tower (4) in said oxidation liquid receiver (7) accounts for 5 to 10 vol.% of the whole off-gas of said oxidation tower (4).
7. An oxidation process according to claim 6, wherein the off-gas fed to said oxidation tower (4) in said oxidation liquid receiver (7) accounts for 7 to 10 vol.% of the whole off-gas of said oxidation tower (4).
8. An oxidation process according to claim 5, wherein the oxygen content in the gas phase space of the oxidizing liquid receiver tank (7) is made 8% by volume or less by feeding the off gas of the oxidation tower (4) into the oxidizing liquid receiver tank (7).
9. An oxidation process according to claim 9, wherein the oxygen content in the gas phase space of the oxidizing liquid receiver tank (7) is made 6% by volume or less by feeding the off gas of the oxidation tower (4) into the oxidizing liquid receiver tank (7).
10. An oxidation process according to any one of claims 4-9, wherein at least part of the off-gas of the oxidation column (4) is fed to the oxidation column (4) as oxygen-containing gas before being returned to the gas feed unit (3).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111437691A (en) * | 2020-04-01 | 2020-07-24 | 安徽晋煤中能化工股份有限公司 | Organic waste gas treatment method for producing hydrogen peroxide by anthraquinone process |
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