CN101837956B - Oxidation system for producing hydrogen peroxide - Google Patents
Oxidation system for producing hydrogen peroxide Download PDFInfo
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- CN101837956B CN101837956B CN2010101600404A CN201010160040A CN101837956B CN 101837956 B CN101837956 B CN 101837956B CN 2010101600404 A CN2010101600404 A CN 2010101600404A CN 201010160040 A CN201010160040 A CN 201010160040A CN 101837956 B CN101837956 B CN 101837956B
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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
Abstract
The invention discloses an oxidation system for producing hydrogen peroxide in the field of chemical equipment. In the oxidation system, the outlet of a phosphoric acid preparation tank and a hydride source are communicated with the inlet of a hydride pump; the outlet of the hydride pump is communicated with the bottom of an upper tower; the inlet of a compressed air filter is communicated with a compressed air source; the outlet of the compressed air filter is divided into two paths, one path is communicated with the bottom of the upper tower, and the other path is communicated with the bottom of a lower tower; the number of oxidizing solution coolers is two; an oxidizing solution outlet at the top of the upper tower is communicated with the bottom of a middle tower after passing through one oxidizing solution cooler; an oxidizing solution outlet at the top of the middle tower is communicated with the bottom of the lower tower after passing through the other oxidizing solution cooler; and the tail gas at the tops of the middle and upper towers can be condensed for recycling. When the system works, main reaction is performed in the upper and middle towers and complete oxidation reaction is performed in the lower tower, so that hydride can be more fully oxidized and the yield can be improved. The oxidation system is particularly used for producing the hydrogen peroxide.
Description
Technical field
The present invention relates to a kind of production unit of hydrogen peroxide, the production unit of the hydrogenation process during particularly process for prepairng hydrogen peroxide by anthraquinone is produced.
Background technology
At present, the main production method of hydrogen peroxide is anthraquinone, and through the big quantity research improvement of various countries company, this method becomes our times and produces the method that hydrogen peroxide has comparative advantage, and has almost completely replaced electrolytic process.This method be with anthraquinone derivative (mainly being the 2-alkyl-anthraquinone) as support of the catalyst, in the presence of catalyzer, will be dissolved in 2-alkyl-anthraquinone (AQ) hydrogenation in the suitable organic solvent with hydrogen, generate corresponding 2-alkyl hydrogen anthraquinone (HAQ).Behind the HAQ and catalyst separating in the solvent, can carry out oxidation to it with air or oxygen rich gas, generate H2O2, HAQ restores again and is AQ simultaneously.In the process for prepairng hydrogen peroxide by anthraquinone process, what mainly consume is hydrogen, and anthraquinone has been a carrier function, can recycle.Working fluid during reaction mainly is divided into solvent and two parts of working material.The general mixed solvent that uses two kinds of solvent compositions, a kind of solvent mainly as anthraquinone, general at present C9～C11 high boiling point BTX aromatics of using petroleum industry, or select methylnaphthalene for use; Another kind of solvent mainly as the hydrogen anthraquinone, multiselect is with alcohols and ester class, as trioctyl phosphate (TOP), diisobutyl carbinol(DIBC) (DIBC) etc.The selection of anthraquinone is also very important, and selected anthraquinone and hydrogen anthraquinone should have higher solubleness in selected solvent, and keeps chemically stable in hydrogenation repeatedly, oxidising process except that needed chemical reaction takes place as far as possible, and is also cheap and easy to get simultaneously.Make the work carrier at the industrial 2-alkyl-anthraquinone that all adopts at present, wherein using maximum is 2-ethyl-anthraquinone (EAQ).Also can adopt and mix anthraquinone, but mixing anthraquinone preferably has lowest total of the melting point as working material.The catalyzer of anthraquinone use mainly contains two kinds of nickel catalyzator and palladium catalysts.Nickel catalyzator mainly is a Raney's nickel, have active preferably, but it runs into the easy spontaneous combustion of air, easily poisoned by oxygen and hydrogen peroxide, and be difficult to regeneration after losing efficacy, so just greatly limited the use of nickel catalyzator, nickel catalyzator is replaced by noble metal hydrogenation catalysts such as platinum, palladiums gradually, and wherein palladium is particularly commonly used.In order to improve using rate of metal, usually palladium is loaded on the bigger serface carrier, prepare the catalyzer of high degree of dispersion, cause degraded again easily but specific surface area is excessive.
In the prior art, during with process for prepairng hydrogen peroxide by anthraquinone, its oxidation system mainly comprises oxidizing tower, from the hydride of hydrogenation system, in oxidizing tower, carry out oxidizing reaction from the pressurized air of pneupress system and from the phosphoric acid of phosphoric acid configured slot, the hydrogen anthraquinone is oxidized in this process, generate hydrogen peroxide, and the hydrogen anthraquinone is reduced to original 2-ethyl-anthraquinone, and then sends to extracting system and extract.Its weak point is: existing oxidation system oxidization-hydrogenation ratio is lower, and the oxidation of hydride is incomplete, yields poorly, and the simultaneity factor production cycle is stable inadequately.
Summary of the invention
The purpose of this invention is to provide a kind of oxidation system that is used for hydrogen peroxide manufacture, make it can overcome the defective of prior art, hydride is oxidation more fully, to improve productive rate.
The object of the present invention is achieved like this: a kind of oxidation system that is used for hydrogen peroxide manufacture, the oxidizing tower, compressed-air filter, the oxidation liquid gas-liquid separator that comprise the phosphoric acid configured slot, form by Shang Ta, Zhong Ta and following tower, groove, oxidation liquid storage tank in the middle of Oxidized Liquid Cooler, oxidation liquid exhaust gas cooler, the aromatic hydrocarbons; The import that the outlet of described phosphoric acid configured slot is connected the hydrogenation liquid pump with the hydride source, the hydride pump outlet is connected and is gone up tower bottom, compressed air gas source is connected in the compressed-air filter import, the outlet of compressed-air filter is divided into two-way, one the tunnel connects upward tower bottom, and tower bottom is down connected on another road; Oxidized Liquid Cooler is provided with two, tower bottom during the oxidation liquid outlet of last top of tower is connected after one of them Oxidized Liquid Cooler, tower bottom is down connected in the oxidation liquid outlet of middle top of tower after another Oxidized Liquid Cooler, the tail gas of Zhong Ta and last top of tower is groove in the middle of oxidation liquid exhaust gas cooler is connected aromatic hydrocarbons, the oxidation liquid outlet of following top of tower connects oxidation liquid gas-liquid separator, the Zhong Ta bottom is connected in the air outlet at oxidation liquid gas-liquid separator top, the liquid outlet of oxidation liquid gas-liquid separator bottom is connected oxidation liquid storage tank, and the outlet of oxidation liquid storage tank bottom connects extraction workshop section through the oxidation liquid pump; The air outlet at groove top connects device for recovering tail gas in the middle of the aromatic hydrocarbons, and the liquid outlet of groove bottom connects oxidation liquid storage tank in the middle of the aromatic hydrocarbons.
During this device work, hydride enters tower bottom on the oxidizing tower after the prepared phosphoric acid aqueous solution sucks the mixing of hydrogenation liquid pump in phosphoric acid storage tank in advance.Pressurized air as oxygenant is divided into two-way behind air filter; One the tunnel enters tower bottom on the oxidizing tower, and another road enters tower bottom under the oxidizing tower.The air that enters tower bottom with the hydride thorough mixing after in the tower joint and flow to, the hydrogen anthraquinone is oxidized in this process, generate hydrogen peroxide, and the hydrogen anthraquinone is reduced to original 2-ethyl-anthraquinone, the working fluid of this moment promptly is called oxidation liquid.The oxidation liquid that rises to top of tower enters middle tower bottom after one of them Oxidized Liquid Cooler cooling; In middle tower, oxidation liquid from last tower also flows to the secondary air that comes autoxidation liquid gas-liquid separator, this moment, the hydrogen anthraquinone was by further oxidation, the oxidation liquid therefrom oxidation liquid outlet of top of tower leaves, after another Oxidized Liquid Cooler cooling, send into down tower bottom, in following tower, mix rising with fresh air from air filter, remaining hydrogen anthraquinone is oxidized complete in uphill process in the oxidation liquid, the mixture that comes out from following column overhead goes out through oxidation liquid gas-liquid separator separates that gas is laggard goes into oxidation liquid storage tank, by the oxidation liquid pump it is sent into extraction workshop section then; The tail gas of Shang Ta and middle top of tower, its main component is a nitrogen, and be entrained with a small amount of aromatic hydrocarbon steam and remaining oxygen, this part tail gas compiles and enters oxidation liquid exhaust gas cooler, after cooling, enter the middle groove of aromatic hydrocarbons, liquid wherein can be regularly in the middle of the aromatic hydrocarbons groove bottom put into oxidation liquid storage tank, fail the gas of condensation to send into device for recovering tail gas.From above-mentioned working process as can be seen, the present invention can enter the temperature of the oxidation liquid of Zhong Ta and following tower by two Oxidized Liquid Cooler adjustment, make it under optimum temps, oxidizing reaction take place, this device adopts three-tower structure, taken into full account the characteristic of the slow oxidative reaction of hydrogen anthraquinone, structure design in conjunction with oxidizing tower, principal reaction is concentrated in Shang Ta and the middle tower, and the task of complete oxidation is finished by following tower, solved the oxidation incomplete technical barrier that exists in the industry for many years, hydride is oxidation more fully, can improve productive rate; Owing to the complete of oxidation improved output and made system's production cycle more stable, the air utilization is more complete simultaneously.This system-specific is in the production of hydrogen peroxide.
As a further improvement on the present invention, the inner top of described Shang Ta and middle tower is built-in with gas-liquid separation device.Because Shang Ta and middle tower are the major portion of oxidizing reaction, the tail gas of generation is more, and its inside is provided with gas-liquid separation device, can increase the gas-liquid separation interface, further guarantee gas-liquid separation effect, the gas content that can guarantee to enter down in the oxidation liquid in the tower is less, and guaranteeing finally can complete oxidation.
For making reaction to carry out more smoothly, described Shang Ta, Zhong Ta and following tower inner bottom part are respectively equipped with gas distributor.The gas branch spreads device can make oxygen dispersion, the fragmentation that enters in the oxidizing tower, forms small bubbles, with oxidation liquid bigger contact area is arranged, and guarantees to react and can carry out smoothly.
For guaranteeing that Shang Ta and Zhong Ta bear most oxidizing reaction work, the described tower height degree of going up is greater than middle tower height degree, and middle tower height degree is greater than following tower height degree.
Description of drawings
Fig. 1 is a fundamental diagram of the present invention.
Embodiment
As shown in the figure, be a kind of fundamental diagram that is used for the oxidation system of hydrogen peroxide manufacture, oxidizing tower, compressed-air filter X1201, oxidation liquid gas-liquid separator V1202 that this oxidation system comprises phosphoric acid configured slot V1201, is made up of last tower T1201A, middle tower T1201B and following tower T1201C, groove V1203, oxidation liquid storage tank V1204 in the middle of Oxidized Liquid Cooler E1201A and E1201B, oxidation liquid exhaust gas cooler E1202, the aromatic hydrocarbons; The import that the outlet of phosphoric acid configured slot V1201 is connected hydrogenation liquid pump P1101 with the hydride source, the outlet of hydrogenation liquid pump P1101 is connected and is gone up tower T1201A bottom, compressed air gas source is connected in compressed-air filter X1201 import, the outlet of compressed-air filter X1201 is divided into two-way, one the tunnel connects upward tower T1201A bottom, and tower T1201C bottom is down connected on another road; Tower T1201B bottom during the oxidation liquid outlet at last tower T1201A top is connected behind one of them Oxidized Liquid Cooler E1201A, tower T1201C bottom is down connected in the oxidation liquid outlet at middle tower T1201B top behind another Oxidized Liquid Cooler E1201B, the tail gas at middle tower T1201B and last tower T1201A top is groove V1203 in the middle of oxidation liquid exhaust gas cooler E1202 connects aromatic hydrocarbons, the oxidation liquid outlet at following tower T1201C top connects oxidation liquid gas-liquid separator V1202, tower T1201B bottom during the air outlet at oxidation liquid gas-liquid separator V1202 top is connected, the liquid outlet of oxidation liquid gas-liquid separator V1202 bottom is connected oxidation liquid storage tank V1204, the outlet of oxidation liquid storage tank V1204 bottom connects extraction workshop section through oxidation liquid pump P1201, oxidation liquid pump P1201 adopts the setting of two pumps that are arranged in parallel, a job, another can be standby; The air outlet at groove V1203 top connects device for recovering tail gas in the middle of the aromatic hydrocarbons, and the liquid outlet of groove V1203 bottom connects oxidation liquid storage tank V1204 in the middle of the aromatic hydrocarbons.The inner top of last tower T1201A and middle tower T1201B is built-in with gas-liquid separation device; Last tower T1201A, middle tower T1201B and following tower T1201C inner bottom part are respectively equipped with gas distributor; Last tower T1201A height is greater than middle tower T1201B height, and middle tower T1201B height is greater than following tower T1201C height.In this device, oxidation system comprise phosphoric acid configured slot V1201, by on tower T1201A, middle tower T1201B and following tower the T1201C oxidizing tower, compressed-air filter X1201, the oxidation liquid gas-liquid separator V1202 that form, the import of groove V1203, oxidation liquid storage tank V1204 in the middle of Oxidized Liquid Cooler, oxidation liquid exhaust gas cooler E1202, the aromatic hydrocarbons, outlet are provided with corresponding gate valve, pressure controlled valve, level control valve etc. can also be set, to realize automatic adjusting.
During this device work, feed pure water and phosphoric acid in the phosphoric acid configured slot V1201, configure phosphoric acid solution, and after the measuring apparatus metering, after the hydride from hydrogenation system sucks hydrogenation liquid pump P1101 mixing, enter tower T1201A bottom on the oxidizing tower; Pressurized air as oxygenant is divided into two-way behind air filter; One the tunnel enters tower T1201A bottom on the oxidizing tower, and another road enters tower T1201C bottom under the oxidizing tower.The air that enters tower T1201A bottom with the hydride thorough mixing after in last tower T1201A and on the flow direction, the hydrogen anthraquinone is oxidized in this process, generate hydrogen peroxide, and the hydrogen anthraquinone is reduced to original 2-ethyl-anthraquinone, the working fluid of this moment promptly is called oxidation liquid.The oxidation liquid that rises to tower T1201A top is isolated tail gas and oxidation liquid through gas-liquid separation device, and oxidation liquid wherein enters middle tower T1201B bottom after one of them Oxidized Liquid Cooler E1201A cooling; In middle tower T1201B, oxidation liquid from last tower T1201A also flows to the secondary air that comes autoxidation liquid gas-liquid separator V1202, this moment, the hydrogen anthraquinone was by further oxidation, the isolated oxidation liquid in middle tower T1201B top therefrom the oxidation liquid outlet at tower T1201B top leave, after another Oxidized Liquid Cooler E1201B cooling, send into down tower T1201C bottom, in following tower T1201C, mix rising with fresh air from air filter, remaining hydrogen anthraquinone is oxidized complete in uphill process in the oxidation liquid, the mixture that comes out from following tower T1201C cat head enters oxidation liquid storage tank V1204 after oxidation liquid gas-liquid separator V1202 isolates gas, by oxidation liquid pump P1201 it is sent into extraction workshop section then; The tail gas at last tower T1201A and middle tower T1201B top, its main component is a nitrogen, and be entrained with a small amount of aromatic hydrocarbon steam and remaining oxygen, this part tail gas compiles and enters oxidation liquid exhaust gas cooler E1202, after cooling, enter the middle groove V1203 of aromatic hydrocarbons, liquid wherein can regularly be put into oxidation liquid storage tank V1204, recycling from the middle groove V1203 of aromatic hydrocarbons bottom; Fail the gas of condensation and send into device for recovering tail gas.
Through evidence, this device can make the more domestic universal class device of oxidizing process plant efficiency improve more than 20%, and oxidization-hydrogenation ratio can reach 98%, improves more than 5% than general device both at home and abroad, has realized the complete oxidation under the high hydrogenation efficiency.Like this, not only saved facility investment, and owing to the complete of oxidation improved output and made system's production cycle more stable, the air utilization is more complete simultaneously.Its captured the hydrogen peroxide industry for a long time oxidization-hydrogenation ratio low, produce unsettled technical barrier.
The present invention is not limited to the foregoing description, as those skilled in the art, by simple conversion or be equal to the alternative technical scheme identical or close with the present invention that obtain, all falls within the scope of protection of the present invention.
Claims (4)
1. oxidation system that is used for hydrogen peroxide manufacture, it is characterized in that: the oxidizing tower, compressed-air filter, the oxidation liquid gas-liquid separator that comprise the phosphoric acid configured slot, form by Shang Ta, Zhong Ta and following tower, groove, oxidation liquid storage tank in the middle of Oxidized Liquid Cooler, oxidation liquid exhaust gas cooler, the aromatic hydrocarbons; The import that the outlet of described phosphoric acid configured slot is connected the hydrogenation liquid pump with the hydride source, the hydride pump outlet is connected and is gone up tower bottom, compressed air gas source is connected in the compressed-air filter import, the outlet of compressed-air filter is divided into two-way, one the tunnel connects upward tower bottom, and tower bottom is down connected on another road; Oxidized Liquid Cooler is provided with two, tower bottom during the oxidation liquid outlet of last top of tower is connected after one of them Oxidized Liquid Cooler, tower bottom is down connected in the oxidation liquid outlet of middle top of tower after another Oxidized Liquid Cooler, the tail gas of Zhong Ta and last top of tower is groove in the middle of oxidation liquid exhaust gas cooler is connected aromatic hydrocarbons, the oxidation liquid outlet of following top of tower connects oxidation liquid gas-liquid separator, the Zhong Ta bottom is connected in the air outlet at oxidation liquid gas-liquid separator top, the liquid outlet of oxidation liquid gas-liquid separator bottom is connected oxidation liquid storage tank, and the outlet of oxidation liquid storage tank bottom connects extraction workshop section through the oxidation liquid pump; The air outlet at groove top connects device for recovering tail gas in the middle of the aromatic hydrocarbons, and the liquid outlet of groove bottom connects oxidation liquid storage tank in the middle of the aromatic hydrocarbons.
2. the oxidation system that is used for hydrogen peroxide manufacture according to claim 1 is characterized in that: the inner top of described Shang Ta and middle tower is built-in with gas-liquid separation device.
3. the oxidation system that is used for hydrogen peroxide manufacture according to claim 1 and 2 is characterized in that: described Shang Ta, Zhong Ta and following tower inner bottom part are respectively equipped with gas distributor.
4. the oxidation system that is used for hydrogen peroxide manufacture according to claim 1 and 2 is characterized in that: the described tower height degree of going up is greater than middle tower height degree, and middle tower height degree is greater than following tower height degree.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101600404A CN101837956B (en) | 2010-04-29 | 2010-04-29 | Oxidation system for producing hydrogen peroxide |
| PCT/CN2011/072635 WO2011134344A1 (en) | 2010-04-29 | 2011-04-12 | Oxidation system of hydrogen peroxide production |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101600404A CN101837956B (en) | 2010-04-29 | 2010-04-29 | Oxidation system for producing hydrogen peroxide |
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| CN101837956A CN101837956A (en) | 2010-09-22 |
| CN101837956B true CN101837956B (en) | 2011-09-28 |
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| CN2010101600404A Active CN101837956B (en) | 2010-04-29 | 2010-04-29 | Oxidation system for producing hydrogen peroxide |
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| WO (1) | WO2011134344A1 (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837956B (en) * | 2010-04-29 | 2011-09-28 | 扬州惠通化工技术有限公司 | Oxidation system for producing hydrogen peroxide |
| CN101955161B (en) * | 2010-10-15 | 2012-02-22 | 怀化市双阳林化有限公司 | Method for reducing discharge of oxidization raffinate |
| CN105731385B (en) * | 2016-03-29 | 2018-02-09 | 福建永荣科技有限公司 | A kind of hydrogen peroxide oxidation extraction tower and method |
| JP2018135231A (en) * | 2017-02-21 | 2018-08-30 | 三菱瓦斯化学株式会社 | Oxidation tower and hydrogen peroxide production apparatus comprising oxidation tower |
| CN107032303B (en) * | 2017-06-15 | 2023-06-27 | 扬州惠通科技股份有限公司 | Fluidized bed production system and method for hydrogen peroxide |
| CN108751135B (en) * | 2018-07-06 | 2023-09-29 | 浙江工程设计有限公司 | Hydrogen peroxide production facility and extraction processing apparatus based on anthraquinone process |
| CN111137864B (en) * | 2020-01-02 | 2024-04-05 | 黎明化工研究设计院有限责任公司 | Oxidation tower for preparing hydrogen peroxide by anthraquinone process |
| CN111115584B (en) * | 2020-01-02 | 2024-04-05 | 黎明化工研究设计院有限责任公司 | Oxidation tower for preparing hydrogen peroxide by anthraquinone process |
| CN111039262A (en) * | 2020-01-02 | 2020-04-21 | 黎明化工研究设计院有限责任公司 | Oxidation tower for preparing hydrogen peroxide by anthraquinone process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5662878A (en) * | 1996-04-25 | 1997-09-02 | University Of Chicago | Process for the production of hydrogen peroxide |
| CN1721320A (en) * | 2002-09-03 | 2006-01-18 | 中国石油化工股份有限公司巴陵分公司 | Oxidation process for preparing hydrogen peroxide |
| CN201309829Y (en) * | 2008-08-14 | 2009-09-16 | 安徽临泉化工股份有限公司 | Oxidation device for producing hydrogen peroxide by anthraquinone process |
| CN201686491U (en) * | 2010-04-29 | 2010-12-29 | 扬州惠通化工技术有限公司 | Oxidizing system for preparing hydrogen peroxide |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3880596A (en) * | 1971-09-24 | 1975-04-29 | Degussa | Apparatus for the production of hydrogen peroxide |
| FR2730986B1 (en) * | 1995-02-28 | 1997-05-16 | Chemoxal Sa | PLANT FOR THE PRODUCTION OF HYDROGEN PEROXIDE |
| CN101837956B (en) * | 2010-04-29 | 2011-09-28 | 扬州惠通化工技术有限公司 | Oxidation system for producing hydrogen peroxide |
-
2010
- 2010-04-29 CN CN2010101600404A patent/CN101837956B/en active Active
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2011
- 2011-04-12 WO PCT/CN2011/072635 patent/WO2011134344A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5662878A (en) * | 1996-04-25 | 1997-09-02 | University Of Chicago | Process for the production of hydrogen peroxide |
| CN1721320A (en) * | 2002-09-03 | 2006-01-18 | 中国石油化工股份有限公司巴陵分公司 | Oxidation process for preparing hydrogen peroxide |
| CN201309829Y (en) * | 2008-08-14 | 2009-09-16 | 安徽临泉化工股份有限公司 | Oxidation device for producing hydrogen peroxide by anthraquinone process |
| CN201686491U (en) * | 2010-04-29 | 2010-12-29 | 扬州惠通化工技术有限公司 | Oxidizing system for preparing hydrogen peroxide |
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| CN101837956A (en) | 2010-09-22 |
| WO2011134344A1 (en) | 2011-11-03 |
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Address after: 225008 No. 18 Hung Road, Yangzhou Development Zone, Jiangsu, China Patentee after: Yangzhou Huitong chemical Polytron Technologies Inc Address before: 225008 No. 18 Hung Road, Yangzhou Development Zone, Jiangsu, China Patentee before: Open chemical industry technological Co., Ltd. of the favor of Yangzhou |
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