CN114671409A - Method for producing hydrogen peroxide by full acidity - Google Patents
Method for producing hydrogen peroxide by full acidity Download PDFInfo
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- CN114671409A CN114671409A CN202210246649.6A CN202210246649A CN114671409A CN 114671409 A CN114671409 A CN 114671409A CN 202210246649 A CN202210246649 A CN 202210246649A CN 114671409 A CN114671409 A CN 114671409A
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- 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 discloses a method for producing hydrogen peroxide by full acidity, which comprises the following steps: a hydrogenation section: carrying out hydrogenation reaction on the working solution and hydrogen in a hydrogenation tower under the catalysis of palladium to obtain hydrogenated working solution containing anthraquinone; an oxidation section: adding phosphoric acid into the hydrogenated working solution obtained in the hydrogenation section, flowing into an oxidation tower, and introducing air into the oxidation tower to perform oxidation reaction to generate hydrogen peroxide and anthraquinone; an extraction section: extracting a reaction product obtained in an oxidation section by water to obtain hydrogen peroxide aqueous solution; a purification section: adding heavy aromatic hydrocarbon into the hydrogen peroxide water solution for purification to obtain hydrogen peroxide. The invention has the beneficial effects that: the application provides a method for producing hydrogen peroxide in a full-acidic mode, which reduces the number and complexity of system equipment, achieves intrinsic safety, enables the production process to be easier to manage, has higher operation flexibility, reduces the consumption of chemicals in the production process due to the elimination of an alkaline working solution process, and can provide more reasonable 'package' service for owners.
Description
Technical Field
The invention belongs to the technical field of inorganic chemical industry, and particularly relates to a method for producing hydrogen peroxide in a full-acidic manner.
Background
The hydrogen peroxide is also called as hydrogen peroxide, is a green chemical product, has almost no pollution in the production and use processes, and is called as a 'clean' chemical product. Under the condition of increasingly severe environmental protection forms, the hydrogen peroxide industry has wide prospects.
At present, hydrogen peroxide is mainly used in the fields of bleaching, chemical synthesis, environmental protection and the like. The application in the bleaching field has the advantages of small damage to the fiber strength, difficult yellowing of fabrics, proper hand feeling and no pollution to the environment. The demand for additives for detergent production and the like is increasing in the field of chemical synthesis. Can be applied to the environmental protection field to treat toxic waste gases such as sulfur dioxide, nitric oxide, hydrogen sulfide and the like, has good effect and can not generate secondary pollution.
The industrial preparation method of hydrogen peroxide is mainly divided into the following four methods: the alkaline hydrogen peroxide preparation method, the phosphoric acid neutralization method, the electrolytic sulfuric acid method and the 2-ethyl anthraquinone method, but the existing preparation processes are dangerous in the preparation process and are easy to cause safety accidents.
Hydrogen peroxide is easily decomposed by alkali, which may cause safety accidents, so that phosphoric acid needs to be added to maintain the working solution in the hydrogenation, oxidation and extraction sections to be acidic due to the presence of hydrogen peroxide so as to ensure that the hydrogen peroxide is relatively stable. The circulating working solution after extracting the product hydrogen peroxide may contain hydrogen peroxide, in order to avoid safety accidents caused by decomposition of the hydrogen peroxide in the working solution returned to hydrogenation when encountering the hydrogenation working solution, the hydrogen peroxide in the working solution returned to hydrogenation needs to be reduced to below safe content, the existing anthraquinone method hydrogen peroxide production process adopts the process flows of acidic working solution and alkaline working solution, namely, the aim of decomposing the hydrogen peroxide in the working solution is achieved by adding alkali solution in a post-treatment working section, then the working solution and the alkali solution are separated and returned to hydrogenation, and phosphoric acid is added in the hydrogenation working solution to convert the working solution into acidity again, so that the working solution is brought with alkali due to incomplete separation of the working solution and the alkali in the process, and the safety accidents of a hydrogen peroxide device can be caused.
Disclosure of Invention
The method mainly aims to improve the intrinsic safety of the production process of the hydrogen peroxide device, and adopts a full-acid method for producing the hydrogen peroxide by canceling an alkaline working solution system in the production process of the hydrogen peroxide device.
In order to achieve the above purpose, the invention provides the following technical scheme:
a wholly acidic process for the production of hydrogen peroxide comprising the steps of:
(1) a hydrogenation section: carrying out hydrogenation reaction on the working solution and hydrogen in a hydrogenation tower under the catalysis of palladium to obtain hydrogenated working solution containing anthraquinone Hydride (HEAQ);
(2) an oxidation section: adding phosphoric acid into the hydrogenated working solution obtained in the hydrogenation section, flowing into an oxidation tower, and introducing air into the oxidation tower to perform oxidation reaction to generate hydrogen peroxide and anthraquinone (EAQ);
(3) an extraction section: extracting the reaction product obtained in the step (2) with water to obtain hydrogen peroxide aqueous solution;
(4) a purification section: adding heavy aromatic hydrocarbon into the hydrogen peroxide water solution for purification to obtain hydrogen peroxide.
Compared with the existing hydrogen peroxide production technology, the method for producing the hydrogen peroxide by the full acidity process comprises the steps of hydrogenation, oxidation, extraction, purification and the like, and the novel intrinsic safety hydrogen peroxide production method avoids the safety risk caused by alkali brought by working liquid in the traditional hydrogen peroxide production process, and meanwhile, the production method has no acid-base neutralization process, so that the product hydrogen peroxide has less impurity content and higher purity.
According to the method for producing hydrogen peroxide in a fully acidic manner, in a hydrogenation working section, a working solution and hydrogen gas are subjected to hydrogenation reaction on the surface of a palladium catalyst in a hydrogenation tower to obtain a hydrogenation working solution containing anthraquinone Hydride (HEAQ); in an oxidation working section, the hydrogenation working solution and oxygen in the air are subjected to peroxidation reaction to generate hydrogen peroxide, and the HEAQ is recovered into EAQ; in an extraction working section, extracting an oxidizing solution by using pure water by utilizing the difference of the solubility of hydrogen peroxide in water and a working solution and the density difference of the working solution and the water to obtain an aqueous solution (27.5-35%) of the hydrogen peroxide; in the purification section, the hydrogen peroxide solution is purified by heavy aromatics to remove impurities, and the product hydrogen peroxide is obtained; the extracted working solution is subjected to flash evaporation treatment and then returns to the hydrogenation process for recycling.
As a preferred embodiment, in the step (1), each liter of the working solution in the step (1) contains 180g of solute 2-B-grade anthraquinone 170-plus, and the balance is solvent aromatic hydrocarbon and tetrabutyl urea; the volume ratio of the aromatic hydrocarbon to the tetrabutyl urea is 2.5-3.5: 1.
as a preferred embodiment, in the above-mentioned all-acidic method for producing hydrogen peroxide, in step (1), the flow rate of the working solution is 25-30m 3The hydrogen flow rate of the hydrogen peroxide product is 186-200Nm3T hydrogen peroxide product, the catalyst packing amount is 1.2-1.5m3H/t hydrogen peroxide product; the temperature of the hydrogenation reaction is 55-85 ℃, and the reaction pressure is 0.15-0.5 MPa.
In the above-described fully acidic process for producing hydrogen peroxide, as a preferred embodiment, in the step (2), phosphoric acid is added to the hydrogenation working solution so that the acidity of the hydrogenation working solution is 0.003 g/L.
In the above-mentioned all-acidic process for producing hydrogen peroxide, as a preferred embodiment, in the step (2), the flow rate of the introduced air is 1200Nm3The temperature of the oxidation reaction is 48-55 ℃.
In the above-mentioned fully acidic process for producing hydrogen peroxide, as a preferred embodiment, in the step (4), the heavy aromatic hydrocarbon is a mixture of aromatic hydrocarbons of C9-C10, and the flash point of the heavy aromatic hydrocarbon is 56-60 ℃.
In the above-mentioned fully acidic process for producing hydrogen peroxide, as a preferred embodiment, in step (4), the heavy aromatic hydrocarbon is added in an amount of 3 to 6L/t hydrogen peroxide product.
The beneficial effects of the invention are as follows: the application provides a novel intrinsically safe anthraquinone process hydrogen peroxide production process, which can enable a system to achieve intrinsic safety and improve the system safety after project construction. The method for producing hydrogen peroxide in full acidity provided by the invention can reduce the number and complexity of system equipment, reduce purchasing and construction management links in the construction process, reduce the operation difficulty of the system after project production, achieve intrinsic safety, simultaneously make the production process easier to manage, and have higher operation flexibility.
Detailed Description
In order to make the technical solutions in the embodiments of the present application better understood, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to examples, and it is obvious that the described embodiments are only some embodiments of the present application, and not all embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments in the present application without making any creative effort shall fall within the protection scope of the present application.
Example 1
A wholly acidic process for the production of hydrogen peroxide as described in example 1 comprising the steps of:
(1) a hydrogenation section: carrying out hydrogenation reaction on working solution (each liter of working solution contains 170g of solute 2-B-grade anthraquinone, and the balance is solvent aromatic hydrocarbon and tetrabutyl urea, wherein the volume ratio of the aromatic hydrocarbon to the tetrabutyl urea is 2.5: 1) and hydrogen in a hydrogenation tower under the catalysis of palladium to obtain hydrogenation working solution containing hydroanthraquinone; the temperature of the hydrogenation reaction is 55 ℃, the reaction pressure in the hydrogenation tower is 0.15MPa, and the flow rate of the working solution in the hydrogenation tower is 25m3A hydrogen peroxide product at a hydrogen flow rate of 186Nm3Pert hydrogen peroxide product, catalyst loading 1.2m3H/t hydrogen peroxide product;
(2) An oxidation section: adding phosphoric acid into the hydrogenated working solution obtained in the hydrogenation section to ensure that the acidity of the hydrogenated working solution is 0.003g/L, flowing into an oxidation tower, introducing air into the oxidation tower to perform oxidation reaction at the temperature of 48 ℃, wherein the flow rate of the introduced air is 1200Nm3A/h.t hydrogen peroxide product to produce hydrogen peroxide and anthraquinone;
(3) an extraction section: extracting the reaction product obtained in the step (2) with water to obtain hydrogen peroxide aqueous solution;
(4) a purification section: adding heavy aromatic hydrocarbon into the aqueous hydrogen peroxide solution for purification and demixing, wherein the adding amount of the heavy aromatic hydrocarbon is 3L/t hydrogen peroxide product (the heavy aromatic hydrocarbon is a C9-C10 aromatic hydrocarbon mixture, and the flash point of the heavy aromatic hydrocarbon is 58 ℃), and obtaining 27.5% hydrogen peroxide.
Example 2
Example 2 a wholly acidic process for the production of hydrogen peroxide comprising the steps of:
(1) hydrogenation section: carrying out hydrogenation reaction on working solution (each liter of working solution contains 175g of solute 2-ethide anthraquinone, and the balance of solvent aromatic hydrocarbon and tetrabutyl urea, wherein the volume ratio of the aromatic hydrocarbon to the tetrabutyl urea is 3: 1) and hydrogen in a hydrogenation tower under the catalysis of palladium to obtain hydrogenated working solution containing hydroanthraquinone; the temperature of the hydrogenation reaction is 60 ℃, the reaction pressure in the hydrogenation tower is 0.25MPa, and the flow rate of the working solution in the hydrogenation tower is 26m 3Pert hydrogen peroxide product, hydrogen flow rate of 190Nm3Pert hydrogen peroxide product, catalyst loading 1.3m3H/t hydrogen peroxide product;
(2) an oxidation section: adding phosphoric acid into the hydrogenated working solution obtained in the hydrogenation section to ensure that the acidity of the hydrogenated working solution is 0.003g/L, flowing into an oxidation tower, introducing air into the oxidation tower to perform oxidation reaction at the temperature of 50 ℃, wherein the flow rate of the introduced air is 1200Nm3A/h.t hydrogen peroxide product to produce hydrogen peroxide and anthraquinone;
(3) an extraction section: extracting the reaction product obtained in the step (2) with water to obtain hydrogen peroxide aqueous solution;
(4) a purification section: adding heavy aromatic hydrocarbon into the aqueous hydrogen peroxide solution for purification and demixing, wherein the adding amount of the heavy aromatic hydrocarbon is 4L/t hydrogen peroxide product (the heavy aromatic hydrocarbon is a C9-C10 aromatic hydrocarbon mixture, and the flash point of the heavy aromatic hydrocarbon is 58 ℃), and obtaining 27.5% hydrogen peroxide.
Example 3
A fully acidic process for the production of hydrogen peroxide as described in example 3 comprising the steps of:
(1) hydrogenation section: carrying out hydrogenation reaction on working solution (each liter of working solution contains 180g of solute 2-B-grade anthraquinone, and the balance is solvent aromatic hydrocarbon and tetrabutyl urea, wherein the volume ratio of the aromatic hydrocarbon to the tetrabutyl urea is 3.5: 1) and hydrogen in a hydrogenation tower under the catalysis of palladium to obtain hydrogenation working solution containing hydroanthraquinone; the temperature of the hydrogenation reaction was 80 c, The reaction pressure in the hydrogenation tower is 0.4MPa, and the flow of the working solution in the hydrogenation tower is 28m3Hydrogen flow rate of 195 Nm/t hydrogen peroxide product3T hydrogen peroxide product, catalyst loading 1.3m3H/t hydrogen peroxide product;
(2) an oxidation section: adding phosphoric acid into the hydrogenated working solution obtained in the hydrogenation section to ensure that the acidity of the hydrogenated working solution is 0.003g/L, flowing into an oxidation tower, introducing air into the oxidation tower to perform oxidation reaction at the temperature of 53 ℃, wherein the flow rate of the introduced air is 1200Nm3A/h.t hydrogen peroxide product to produce hydrogen peroxide and anthraquinone;
(3) an extraction section: extracting the reaction product obtained in the step (2) with water to obtain hydrogen peroxide aqueous solution;
(4) a purification section: adding heavy aromatic hydrocarbon into the aqueous hydrogen peroxide solution for purification and demixing, wherein the adding amount of the heavy aromatic hydrocarbon is 5L/t hydrogen peroxide product (the heavy aromatic hydrocarbon is a C9-C10 aromatic hydrocarbon mixture, and the flash point of the heavy aromatic hydrocarbon is 58 ℃), and obtaining 27.5% hydrogen peroxide.
Example 4
Example 4 a wholly acidic process for the production of hydrogen peroxide comprising the steps of:
(1) hydrogenation section: carrying out hydrogenation reaction on working solution (each liter of working solution contains 175g of solute 2-ethide anthraquinone, and the balance of solvent aromatic hydrocarbon and tetrabutyl urea, wherein the volume ratio of the aromatic hydrocarbon to the tetrabutyl urea is 3: 1) and hydrogen in a hydrogenation tower under the catalysis of palladium to obtain hydrogenated working solution containing hydroanthraquinone; the temperature of the hydrogenation reaction is 85 ℃, the reaction pressure in the hydrogenation tower is 0.5MPa, and the flow of the working solution in the hydrogenation tower is 30m 3Pert hydrogen peroxide product, hydrogen flow 200Nm3Pert hydrogen peroxide product, catalyst loading 1.5m3H/t hydrogen peroxide product;
(2) an oxidation section: adding phosphoric acid into the hydrogenated working solution obtained in the hydrogenation section to ensure that the acidity of the hydrogenated working solution is 0.003g/L, flowing into an oxidation tower, introducing air into the oxidation tower to perform oxidation reaction at the temperature of 55 ℃, wherein the flow rate of the introduced air is 1200Nm3A/h.t hydrogen peroxide product to produce hydrogen peroxide and anthraquinone;
(3) an extraction section: extracting the reaction product obtained in the step (2) with water to obtain hydrogen peroxide aqueous solution;
(4) a purification section: adding heavy aromatic hydrocarbon into the aqueous hydrogen peroxide solution for purification and demixing, wherein the addition amount of the heavy aromatic hydrocarbon is 6L/t hydrogen peroxide product (the heavy aromatic hydrocarbon is a C9-C10 aromatic hydrocarbon mixture, and the flash point of the heavy aromatic hydrocarbon is 58 ℃), and obtaining 27.5% hydrogen peroxide.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and additions can be made without departing from the method of the present invention, and these modifications and additions should also be regarded as the protection scope of the present invention.
Claims (7)
1. A fully acidic process for the production of hydrogen peroxide, comprising the steps of:
(1) Hydrogenation section: carrying out hydrogenation reaction on the working solution and hydrogen in a hydrogenation tower under the catalysis of palladium to obtain hydrogenated working solution containing anthraquinone;
(2) an oxidation section: adding phosphoric acid into the hydrogenated working solution obtained in the hydrogenation section, flowing into an oxidation tower, and introducing air into the oxidation tower to perform oxidation reaction to generate hydrogen peroxide and anthraquinone;
(3) an extraction section: extracting the reaction product obtained in the step (2) with water to obtain hydrogen peroxide aqueous solution;
(4) a purification section: adding heavy aromatic hydrocarbon into the hydrogen peroxide water solution for purification to obtain hydrogen peroxide.
2. The fully acidic method for producing hydrogen peroxide as claimed in claim 1, wherein in the step (1), each liter of the working solution contains 170 g of solute 2-B-anthraquinone, and the balance is solvent aromatic hydrocarbon and tetrabutyl urea; the volume ratio of the aromatic hydrocarbon to the tetrabutyl urea is 2.5-3.5: 1.
3. the fully acidic process for producing hydrogen peroxide according to claim 1, wherein the flow rate of the working solution in step (1) is 25-30m3T hydrogen peroxide product, hydrogen flow 186-200Nm3The filling amount of the catalyst is 1.2-1.5m3H/t hydrogen peroxide product; the temperature of the hydrogenation reaction is 55-85 ℃, and the reaction pressure is 0.15-0.5 MPa.
4. The wholly acidic method for producing hydrogen peroxide as claimed in claim 1, wherein in the step (2), phosphoric acid is added to the hydrogenation working solution so that the acidity of the hydrogenation working solution is 0.003 g/L.
5. The wholly acidic process for producing hydrogen peroxide as claimed in claim 1, wherein in the step (2), the flow rate of the introduced air is 1200Nm3The temperature of the oxidation reaction is 48-55 ℃.
6. The wholly acidic process for producing hydrogen peroxide according to claim 1, wherein in the step (4), the heavy aromatic hydrocarbon is a mixture of aromatic hydrocarbons having a carbon number of from 9 to 10, and the flash point of the heavy aromatic hydrocarbon is from 56 to 60 ℃.
7. The fully acidic hydrogen peroxide production process according to claim 1, wherein the heavy aromatics are added in an amount of 3-6L/t hydrogen peroxide product in step (4).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496674A (en) * | 2013-10-18 | 2014-01-08 | 湖南兴鹏化工科技有限公司 | Method of preparing hydrogen peroxide from all-acid working solution system by anthraquinone process |
| CN112499595A (en) * | 2020-11-30 | 2021-03-16 | 平湖石化有限责任公司 | Production process of multi-component full-acidic fixed bed hydrogen peroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496674A (en) * | 2013-10-18 | 2014-01-08 | 湖南兴鹏化工科技有限公司 | Method of preparing hydrogen peroxide from all-acid working solution system by anthraquinone process |
| CN112499595A (en) * | 2020-11-30 | 2021-03-16 | 平湖石化有限责任公司 | Production process of multi-component full-acidic fixed bed hydrogen peroxide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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