CN112499595A - Production process of multi-component full-acidic fixed bed hydrogen peroxide - Google Patents
Production process of multi-component full-acidic fixed bed hydrogen peroxide Download PDFInfo
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 239000012224 working solution Substances 0.000 claims abstract description 31
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000605 extraction Methods 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 27
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 25
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 22
- 230000003647 oxidation Effects 0.000 claims abstract description 22
- 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 abstract description 20
- 150000004056 anthraquinones Chemical class 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 17
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 15
- 230000008929 regeneration Effects 0.000 claims abstract description 13
- 238000011069 regeneration method Methods 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 239000010931 gold Substances 0.000 claims abstract description 8
- 229910052737 gold Inorganic materials 0.000 claims abstract description 8
- -1 hydrogen anthraquinone Chemical class 0.000 claims abstract description 8
- 230000009471 action Effects 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 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 claims description 17
- SNDGLCYYBKJSOT-UHFFFAOYSA-N 1,1,3,3-tetrabutylurea Chemical compound CCCCN(CCCC)C(=O)N(CCCC)CCCC SNDGLCYYBKJSOT-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 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 11
- 239000002904 solvent Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 239000004927 clay Substances 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 25
- 230000008569 process Effects 0.000 abstract description 16
- 239000002253 acid Substances 0.000 abstract description 11
- 239000000428 dust Substances 0.000 abstract description 5
- 239000000284 extract Substances 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 238000004581 coalescence Methods 0.000 description 3
- 238000000622 liquid--liquid extraction Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000012840 feeding operation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
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- 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
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Abstract
The invention relates to a multi-component full-acidic fixed bed hydrogen peroxide production process, which comprises the following steps: (1) in a hydrogenation tower, raw material hydrogen and carrier anthraquinone are subjected to hydrogenation reaction under the action of a palladium-gold catalyst to generate hydrogen anthraquinone hydrogenation liquid; (2) adding phosphoric acid into the hydroanthraquinone hydrogenation solution to adjust the pH value to 3.5 +/-0.2, and reacting the hydroanthraquinone hydrogenation solution with oxygen in the air to obtain an oxidation solution; (3) pure water is used as an extracting agent, countercurrent extraction is carried out in an extraction tower to obtain extract containing hydrogen peroxide, and then heavy aromatic hydrocarbon is used for purification in a purification tower to obtain qualified hydrogen peroxide product. The production process adopts a full-acid fixed bed process technology, the balance regeneration of a working solution system is optimally controlled, part of aluminum peroxide is used for adsorption regeneration, the dust entrainment is reduced, the filtration precision is improved, the dust and salt entrainment in the product is greatly reduced, indexes such as free acid, organic carbon, non-volatile matter and the like are far away, and the product purity is superior to the national standard and the same industry.
Description
Technical Field
The invention relates to a hydrogen peroxide production process, in particular to a multi-component full-acidic fixed bed hydrogen peroxide production process, and belongs to the technical field of chemical production.
Background
The prior art for producing hydrogen peroxide mainly adopts an anthraquinone method, wherein a fixed bed hydrogen peroxide production process of the anthraquinone method uses 2-ethyl anthraquinone as a working carrier, uses arene, trioctyl phosphate and tetrabutyl urea as solvents, prepares working solution in a certain proportion, carries out hydrogenation reaction with hydrogen in a fixed bed under the catalysis of a palladium-gold catalyst at a certain temperature and pressure, generates hydrogenated solution, carries out oxidation reaction with oxygen in the air, obtains an oxidation solution, extracts and purifies the oxidation solution by pure water to obtain a finished hydrogen peroxide, and the working solution is recycled after treatment.
In the production process of hydrogen peroxide by the anthraquinone method, a hydrogenation unit is a gas-liquid-solid three-phase reaction process carried out in a fixed bed reactor filled with a catalyst, the reaction temperature is generally 45-75 ℃, and the reaction pressure is generally 0.2-0.4 MPa; the oxidation unit is used for carrying out automatic oxidation reaction on the hydroanthraquinone generated by the hydrogenation unit and oxygen in the air without a catalyst, the pressure of the oxidation tower is generally 0.20-0.22 Mpa, and the reaction temperature is 50-55 ℃; the extraction unit is used for separating hydrogen peroxide by utilizing the solubility difference between water and working solution and the density difference between the working solution and the water, the extraction pressure is normal pressure, and the extraction temperature is determined by the oxidation temperature and is generally 45-55 ℃.
In the hydrogen peroxide production process, the key is how to keep the whole device stable and safe in production, high in production efficiency, low in energy consumption and other indexes, and the whole device can be operated safely, stably, efficiently and low in consumption only by maintaining all unit operations including a hydrogenation unit to generate higher hydrogen efficiency and fewer degradation products, enabling working liquid to be in an ideal state and enabling an oxidation unit and an extraction unit to fully exert the performance of the oxidation unit and the extraction unit along with proper improvement. CN1673069A discloses an operation method for the hydrogenation reaction of anthraquinone working solution in hydrogen peroxide production, which improves the conversion rate of the anthraquinone working solution and effectively reduces the degradation rate of anthraquinone compared with a continuous feeding operation method. The method aims to inhibit the occurrence of side reactions by periodic feeding of the working solution, but the working solution is periodic feeding, so that the method is difficult to combine with subsequent continuous production processes such as oxidation, extraction, post-treatment and the like, and the total production efficiency and the production capacity of the device are reduced. CN102009961A proposes an oxidation method for producing hydrogen peroxide by anthraquinone process, which is to disperse the gas phase containing oxygen into the working solution containing oil hydrogenated anthraquinone derivative to obtain a gas-liquid mixed fluid containing micron-sized bubbles, and then to complete the oxidation reaction in the process that the gas-liquid mixed fluid flows through the delay pipeline. However, the method has the problems that micron-sized bubbles grow rapidly, the tail oxygen content is high, the number of microreactors is large, the investment is high, hydroanthraquinone is easy to separate out to block the microreactors, and the like.
Therefore, based on the whole hydrogen peroxide production process, how to coordinate the operation of each production unit is very important to ensure the production efficiency and the efficient and safe long-period operation of the whole device.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a multi-component full-acidic fixed bed hydrogen peroxide production process, which adopts a multi-component full-acidic fixed bed process technology, no alkaline medium is introduced in the production process, and simultaneously, the balance regeneration of a working solution system is optimized and controlled, so that the purity of the hydrogen peroxide product is greatly improved, the amount of waste water generated by the full-acidic production process is small, the COD equivalent is low, the operation cost of a sewage treatment facility is low, the treated water quality is good, and the hydrogen peroxide product can be recycled as the water supplement of circulating water.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a multi-component full-acidic fixed bed hydrogen peroxide production process comprises the following steps:
(1) in a hydrogenation tower, raw material hydrogen and carrier anthraquinone are subjected to hydrogenation reaction under the action of a palladium-gold catalyst to generate hydrogen anthraquinone hydrogenation liquid;
(2) adding phosphoric acid into the hydroanthraquinone hydrogenation solution to adjust the pH value to 3.5 +/-0.2, and reacting the hydroanthraquinone hydrogenation solution with oxygen in the air to obtain an oxidation solution;
(3) pure water is taken as an extracting agent, phosphoric acid is used for adjusting the pH value of the pure water to be 3.0 +/-0.2, then the pure water is mixed with the oxidizing liquid obtained in the step (2), an extraction liquid containing hydrogen peroxide is obtained by countercurrent extraction in an extraction tower, then heavy aromatic hydrocarbon is used for purification in a purification tower to obtain a qualified hydrogen peroxide product,
(4) after vacuum dehydration, 25-35 v% of raffinate discharged from the extraction tower flows through a clay bed for regeneration treatment, regenerated treatment liquid is mixed with liquid which is not subjected to regeneration treatment, trioctyl phosphate, tetrabutyl urea and heavy aromatics which are lost in the reaction of the system are supplemented in proportion, and then the mixture is returned to the hydrogenation tower as circulating working liquid for continuous reaction.
The production process adopts a full-acid fixed bed process technology, the balance regeneration of a working solution system is optimally controlled, part of aluminum peroxide is used for adsorption regeneration, the dust entrainment is reduced, the filtration precision is improved, the dust and salt entrainment in the product is greatly reduced, indexes such as free acid, organic carbon, non-volatile matter and the like are far away, and the product purity is superior to the national standard and the same industry.
Preferably, the anthraquinone comprises one or two of 2-ethyl anthraquinone or tetrahydro-diethyl anthraquinone.
Preferably, the mixed solvent of trioctyl phosphate, tetrabutyl urea and heavy aromatic hydrocarbon is used as the carrier solvent in the step (1), and the volume ratio of trioctyl phosphate, tetrabutyl urea and heavy aromatic hydrocarbon is 10-15:10-15: 70-75.
Preferably, the carrier solvent is mixed with anthraquinone to prepare working solution, and the concentration of the anthraquinone in the working solution is 140-165 g/L.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the traditional process, alkali liquor is used as working solution for regeneration balance, hydrogen peroxide decomposition, acidity neutralization and dehydration, so that the alkali liquor is separated from the situation that the balance of the working solution is broken, and the production cannot normally run; the production process of the invention does not introduce an alkali medium, but carries out the balance of the working solution through hydrogenation optimization of the hydrogenation tower (the working solution of the invention is an acidic working solution, and the balance of the acidic working solution is carried out), thereby avoiding the product brought by a large amount of salts and ions generated by acid-base neutralization;
(2) the working solution system balance regeneration is optimally controlled, and partial aluminum peroxide is adopted for adsorption regeneration, so that dust entrainment is reduced, the filtration precision is improved, and the product purity is improved;
(3) the production process disclosed by the invention has the advantages that the amount of waste water generated is small (12-15 t/d), the COD (chemical oxygen demand) and total phosphorus equivalent weight are low, the operating cost of a sewage treatment facility is low, the treated water quality is good, and the treated water can be recycled as circulating water for water replenishing;
(4) compared with the conventional hydrogen peroxide production process, the heavy aromatic hydrocarbon, trioctyl phosphate and phosphoric acid auxiliary materials in the production process are greatly reduced, the material consumption of the device is reduced, and the economic cost is reduced.
Drawings
FIG. 1 is a flow chart of a production process of multi-component full-acidic fixed bed hydrogen peroxide.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples. It is to be understood that the practice of the invention is not limited to the following examples, and that any variations and/or modifications may be made thereto without departing from the scope of the invention.
In the present invention, all parts and percentages are by weight, unless otherwise specified, and the equipment and materials used are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified.
Sources of reagents used in the following examples:
heavy aromatics, purchased from Nanjing oil refinery, Inc., model 100C;
the palladium-gold catalyst is purchased from Futai Baichuan Funton technologies Co., Ltd, and has the model AHC-GIII;
acid pure water means pure water after adjusting pH to 3.0 with phosphoric acid, the phosphoric acid concentration being 25 wt%.
Example 1
A process for producing multi-component full-acidic fixed bed hydrogen peroxide, which has a process flow diagram shown in figure 1, comprises the following specific steps:
1. the mixture of trioctyl phosphate (TOP), tetrabutyl urea (TBU) and heavy aromatic hydrocarbon (AR) is used as a carrier solvent, 2-Ethyl Anthraquinone (EAQ) is used as a carrier, and the mixture is prepared into working solution (900 m)3H). In the reaction process, the volume ratio of trioctyl phosphate, tetrabutyl urea and heavy aromatic hydrocarbon is controlled within the range of 10-15:10-15:70-75, and the concentration of the 2-ethyl anthraquinone in the working solution is 140-165 g/L.
The working fluid was pumped with hydrogen (5000 Nm)3H) entering a hydrogenation tower together, carrying out hydrogenation under the action of a palladium-gold catalyst to generate a hydrogenation solution,
2. adding phosphoric acid into the hydrogenated liquid to adjust the pH value to about 3.5, mixing the hydrogenated liquid and the phosphoric acid, and pumping the mixture by a hydrogenated liquid delivery pump (900 m)3H) is fed into the oxidation column with air (32000 Nm)3H) carrying out cocurrent reaction to generate an oxidation liquid,
3. the oxidizing solution passes through an oxidizing solution pump (900 m)3H) is conveyed to the bottom of the extraction tower, and acid pure water (18 m) is obtained after the pure water is added with acid3And/h) entering the upper part of the extraction tower, and performing countercurrent extraction with the oxidizing solution entering the tower bottom to obtain an extraction liquid containing hydrogen peroxide. Extract (20 m)3H) entering a purification tower, carrying out liquid-liquid extraction on the heavy aromatic hydrocarbon in the purification tower and the heavy aromatic hydrocarbon in the purification tower, and then entering a finished product tank area;
4. raffinate (900 m) from the top of the extraction column3H) after coalescence and vacuum dehydration, the mixture enters a regenerated liquid storage tank (900 m) after regeneration treatment of a carclazyte bed3And/h), preparing and supplementing the working solution lost in the circulation process of the system according to the proportion, and maintaining the system to complete and resume circulation.
Example 2
A multi-component full-acidic fixed bed hydrogen peroxide production process comprises the following specific steps:
working solution (950 m) is prepared by taking trioctyl phosphate (TOP), tetrabutyl urea (TBU) and heavy aromatic hydrocarbon (AR) as solvents and 2-Ethyl Anthraquinone (EAQ) as a carrier3And h), controlling the volume ratio of trioctyl phosphate, tetrabutyl urea and heavy aromatic hydrocarbon within the range of 10-15:10-15:70-75 in the reaction process, and enabling the concentration of the 2-ethyl anthraquinone in the working solution to be 140-165 g/L.
The working fluid was pumped with hydrogen (5200 Nm)3H) hydrogenating under the action of a palladium-gold catalyst to generate hydrogenated liquid, adding phosphoric acid into the hydrogenated liquid to adjust the pH to about 3.5, mixing with the phosphoric acid, and then passing through a hydrogenated liquid delivery pump (960 m)3H) into an oxidation column with air (34000 Nm)3The reaction is carried out in a concurrent flow manner to generate oxidation liquid, and the oxidation liquid passes through an oxidation liquid pump (950 m)3H) is conveyed to the bottom of the extraction tower, and acid pure water (21 m) is obtained after the pure water is added with acid3H) enters the upper part of the extraction tower and is extracted in countercurrent with the oxidizing liquid entering the bottom of the extraction tower to generate hydrogen peroxide (extract liquid is 24 m)3H) entering a purification tower, carrying out liquid-liquid extraction with heavy aromatic hydrocarbons in the tower, and then entering a finished product tank area; raffinate (960 m) from the top of the extraction column3H) after coalescence and vacuum dehydration, the mixture enters a regenerated liquid storage tank (950 m) after being regenerated by a carclazyte bed3And h), preparing and supplementing the working solution lost in the circulation process of the system according to the proportion in the preparation process, and maintaining the system to start circulation again at the end.
Example 3
A multi-component full-acidic fixed bed hydrogen peroxide production process comprises the following specific steps:
working solution (1000 m) is prepared by taking trioctyl phosphate (TOP), tetrabutyl urea (TBU) and heavy aromatic hydrocarbon (AR) as solvents and 2-Ethyl Anthraquinone (EAQ) as a carrier3H) with hydrogen (5500 Nm) by means of a pump3H) hydrogenating under the action of palladium-gold catalyst to generate hydrogenated liquid, adding phosphoric acid into the hydrogenated liquid to adjust the pH to about 3.5, mixing with the phosphoric acid, and passing through a hydrogenated liquid delivery pump (1000 m)3H) is fed into an oxidation tower and air (36000 Nm)3The reaction is carried out in a concurrent flow manner to generate oxidation liquid, and the oxidation liquid passes through an oxidation liquid pump (1000 m)3H) is conveyed to the bottom of the extraction tower, and acid pure water (25 m) is obtained after the pure water is added with acid3H) enters the upper part of the extraction tower and is extracted in countercurrent with the oxidizing liquid entering the bottom of the extraction tower to generate hydrogen peroxide (extract liquid is 28 m)3H) entering a purification tower, carrying out liquid-liquid extraction with heavy aromatic hydrocarbons in the tower, and then entering a finished product tank area; raffinate (1000 m) from the top of the extraction column3H) after coalescence and vacuum dehydration, the mixture enters a regenerated liquid storage tank (1000 m) after being regenerated by a carclazyte bed3H), system circulationThe working solution lost in the process is prepared and supplemented according to the proportion in the preparation process, and the system is maintained to be circulated again and again.
Compared with the traditional process, the hydrogen peroxide production process disclosed by the invention is small in waste water amount (12-15 t/d), low in COD (chemical oxygen demand) and total phosphorus equivalent (shown in table 1), low in running cost of sewage treatment facilities, good in treated water quality and capable of being used as circulating water for water replenishing and recycling.
TABLE 1 comparison of wastewater indexes generated by the process of the present invention and the conventional process
Compared with the hydrogen peroxide process in the same industry, the heavy aromatic hydrocarbon, trioctyl phosphate and phosphoric acid auxiliary materials in the production process are greatly reduced in dosage, so that the material consumption of the device is reduced, and the economic cost is reduced.
TABLE 2 amount of carrier solvent used in examples 1-3
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (4)
1. A multi-component full-acidic fixed bed hydrogen peroxide production process is characterized by comprising the following steps:
(1) in a hydrogenation tower, raw material hydrogen and carrier anthraquinone are subjected to hydrogenation reaction under the action of a palladium-gold catalyst to generate hydrogen anthraquinone hydrogenation liquid;
(2) adding phosphoric acid into the hydroanthraquinone hydrogenation solution to adjust the pH value to 3.5 +/-0.2, and reacting the hydroanthraquinone hydrogenation solution with oxygen in the air to obtain an oxidation solution;
(3) pure water is taken as an extracting agent, phosphoric acid is used for adjusting the pH value of the pure water to be 3.0 +/-0.2, then the pure water is mixed with the oxidizing liquid obtained in the step (2), an extraction liquid containing hydrogen peroxide is obtained by countercurrent extraction in an extraction tower, then heavy aromatic hydrocarbon is used for purification in a purification tower to obtain a qualified hydrogen peroxide product,
(4) after vacuum dehydration, 25-35 v% of raffinate discharged from the extraction tower flows through a clay bed for regeneration treatment, regenerated treatment liquid is mixed with liquid which is not subjected to regeneration treatment, trioctyl phosphate, tetrabutyl urea and heavy aromatics which are lost in the reaction of the system are supplemented in proportion, and then the mixture is returned to the hydrogenation tower as circulating working liquid for continuous reaction.
2. The production process of the multi-component full-acidic fixed bed hydrogen peroxide according to claim 1, which is characterized by comprising the following steps: the anthraquinone comprises one or two of 2-ethyl anthraquinone or tetrahydrodiethyl anthraquinone.
3. The production process of the multi-component full-acidic fixed bed hydrogen peroxide according to claim 1, which is characterized by comprising the following steps: the mixed solvent of trioctyl phosphate, tetrabutyl urea and heavy aromatic hydrocarbon is used as a carrier solvent in the step (1), and the volume ratio of trioctyl phosphate to tetrabutyl urea to heavy aromatic hydrocarbon is 10-15:10-15: 70-75.
4. The production process of the multi-component full-acidic fixed bed hydrogen peroxide according to claim 3, which is characterized by comprising the following steps: the carrier solvent and the anthraquinone are mixed to prepare the working solution, and the concentration of the anthraquinone in the working solution is 140-165 g/L.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113753863A (en) * | 2021-09-22 | 2021-12-07 | 福建永荣科技有限公司 | Method for purifying organic matters in hydrogen peroxide extraction liquid produced by anthraquinone process |
| CN114477096A (en) * | 2022-03-02 | 2022-05-13 | 潜江益和化学品有限公司 | High-efficiency extraction process in hydrogen peroxide production process |
| CN114671409A (en) * | 2022-03-14 | 2022-06-28 | 贵州赛邦科技发展有限公司 | Method for producing hydrogen peroxide by full acidity |
| CN114906821A (en) * | 2022-06-17 | 2022-08-16 | 贵州赛邦科技发展有限公司 | Method for producing hydrogen peroxide by full acidity |
| CN115504437A (en) * | 2021-06-23 | 2022-12-23 | 中国石油化工股份有限公司 | Preparation method and application of hydrogen peroxide |
| CN115650179A (en) * | 2022-11-02 | 2023-01-31 | 中盐常州化工股份有限公司 | Quality improvement method for electronic grade hydrogen peroxide |
| CN116477579A (en) * | 2023-02-16 | 2023-07-25 | 浙江恒逸石化研究院有限公司 | Method for improving extraction yield and product quality of hydrogen peroxide produced by anthraquinone process |
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| CN115504437A (en) * | 2021-06-23 | 2022-12-23 | 中国石油化工股份有限公司 | Preparation method and application of hydrogen peroxide |
| CN113753863A (en) * | 2021-09-22 | 2021-12-07 | 福建永荣科技有限公司 | Method for purifying organic matters in hydrogen peroxide extraction liquid produced by anthraquinone process |
| CN114477096A (en) * | 2022-03-02 | 2022-05-13 | 潜江益和化学品有限公司 | High-efficiency extraction process in hydrogen peroxide production process |
| CN114671409A (en) * | 2022-03-14 | 2022-06-28 | 贵州赛邦科技发展有限公司 | Method for producing hydrogen peroxide by full acidity |
| CN114906821A (en) * | 2022-06-17 | 2022-08-16 | 贵州赛邦科技发展有限公司 | Method for producing hydrogen peroxide by full acidity |
| CN115650179A (en) * | 2022-11-02 | 2023-01-31 | 中盐常州化工股份有限公司 | Quality improvement method for electronic grade hydrogen peroxide |
| CN116477579A (en) * | 2023-02-16 | 2023-07-25 | 浙江恒逸石化研究院有限公司 | Method for improving extraction yield and product quality of hydrogen peroxide produced by anthraquinone process |
| CN116477579B (en) * | 2023-02-16 | 2024-07-23 | 浙江恒逸石化研究院有限公司 | Method for improving extraction yield and product quality of hydrogen peroxide produced by anthraquinone process |
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