CN201686492U - Hydrogenation system for producing hydrogen peroxide - Google Patents
Hydrogenation system for producing hydrogen peroxide Download PDFInfo
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- CN201686492U CN201686492U CN2010201752648U CN201020175264U CN201686492U CN 201686492 U CN201686492 U CN 201686492U CN 2010201752648 U CN2010201752648 U CN 2010201752648U CN 201020175264 U CN201020175264 U CN 201020175264U CN 201686492 U CN201686492 U CN 201686492U
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Abstract
The utility model discloses a hydrogenation system for producing hydrogen peroxide, which belongs to the field of chemical industry equipment. The system includes a hydrogen gas filter, a working liquid preheater, a hydrogenation tower, a hydrogenated liquid gas-liquid separator, a hydrogenated liquid filter, a hydrogenated liquid reproducing bed, and a hydrogenated liquid storing tank; the hydrogenation tower is divided into an upper tower and a lower tower, an outlet of the upper tower is connected with a top inlet of the lower tower, a hydrogenated liquid cooler is arranged between the upper tower and a lower tower, an inlet of the hydrogenated liquid cooler is connected with a bottom outlet of the upper tower, and an outlet of the hydrogenated liquid cooler is connected with the top inlet of the lower tower. During operation, the working liquid and the raw hydrogen gas are filled into the upper tower, after hydrogenation reaction, a part enters into the lower tower, the other part enters into the hydrogenated liquid cooler and then to the lower tower after cooling for the hydrogenation reaction again, the hydrogenation temperature of the lower tower may be adjusted so as to ensure Pd catalyst to have high activity for a long time, and components of the working liquid may be stabilized. The hydrogenation system is used for producing hydrogen peroxide specially.
Description
Technical field
The utility model 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 hydrogenation system mainly comprises hydrogen filter, working fluid preheater, hydrogenation tower, hydride gas-liquid separator, hydride strainer, hydride Regenerative beds, hydride storage tank; The import of described hydrogen filter connects hydrogen source gas, the outlet of hydrogen filter connects the hydrogen inlet of hydrogenation tower, the import of working fluid preheater links to each other with the working fluid source, the outlet of working fluid preheater connects the working fluid import of hydrogenation tower, the hydride outlet of hydrogenation tower bottom is divided into two-way, one the tunnel connects the hydride gas-liquid separator, one the tunnel through the import of hydride recycle pump connection working fluid preheater, the outlet one tunnel of hydride gas-liquid separator connects the import of hydride strainer, another road connects the regeneration steam condenser, the condensate outlet of regeneration steam condenser connects the phlegma scale tank, and the outlet of phlegma scale tank connects working fluid preparation still; The outlet of hydride strainer is divided into two-way, and one the tunnel connects the hydride storage tank, and another road connects the hydride Regenerative beds, and the outlet of hydride Regenerative beds connects the hydride storage tank, and the outlet of hydride storage tank connects oxidation system through draw-off pump.
During its work, working fluid is pumped into the working fluid preheater through working fluid, enters the hydrogenation tower after the control certain temperature; Raw hydrogen enters the hydrogenation top of tower together with working fluid remove the mechanical impurity that may carry secretly through hydrogen filter after; The hydrogenation tower is filled by the palladium catalyst; Spray and following time through bed top sparger simultaneously at working fluid and hydrogen, 2-ethyl-anthraquinone wherein and hydrogen carry out hydrogenation under the palladium catalysis, generate corresponding 2-ethyl hydrogen anthraquinone and a spot of tetrahydrochysene 2-ethyl-anthraquinone, the working fluid of this moment promptly is called hydride.Hydride enters the hydride gas-liquid separator with the foreign gas of not participating in the hydrogen that reacts at the bottom of the hydrogenation tower, isolated hydrogenation tail gas (mainly carrying partial solvent aromatic hydrocarbons secretly) enters in the phlegma scale tank after the regeneration vapour cooler makes wherein most of aromatic hydrocarbons condensation, this part aromatic hydrocarbons is back into working fluid preparation still, recycling after cleaning, and isolated non-condensable gases can be from phlegma scale tank top flux meter metering back emptying; An isolated hydride part is sent the hydrogenation tower back to through circulation hydrogenation liquid pump in the hydride gas-liquid separator, another part hydride is pressed into the hydride strainer by hydrogen pressure, catalyst and carrier small quantities of powder that elimination washes away out in the hydrogenation tower, hydride after filtering divides two portions: a part accounts for 10% of total amount and enters the hydride Regenerative beds, make the small amount of degradation thing that generates in the hydrogenation process obtain entering the hydride storage tank after the regeneration, another part directly enters the hydride storage tank, relends to help the hydrogenation liquid pump that hydride is sent into oxidation system to carry out oxidation.When hydrogenation efficiency when other adjusting measure does not reach the production control requirement, catalyst just needs regeneration, during regeneration, at first will need regenerated tower joint to switch out, working fluid is wherein put into the hydride gas-liquid separator, enter regenerated Ta Jienei after removing the iron rust that to carry secretly and other impurity with low-pressure steam, knot is gathered organic polymer on catalyst; Inorganic salts objectionable impurities purge falls, and after steam purge finishes, after with nitrogen the moisture in the catalyst bed being dried up, can come into operation again with the hydrogen activation more again.The deficiencies in the prior art part is: the difficult control of temperature in (1) hydrogenation tower, and hydrogenation temperature wears out along with catalyst and improves, and wears out thereby quicken catalyst; When the catalyst working temperature was higher, the work-ing life of catalyzer was shorter; Simultaneously, pay the reaction generation more; (2) anthraquinone degradation polymer and metallic salt have the poly-tendency of common knot at catalyst layer, cause the regeneration period short; (3) the easy degree of depth hydrogenation of anthraquinone; (4) the component poor stability of system works liquid.In addition, the hydride gas-liquid separator separates setting with the hydrogenation tower, causes the pipeline complexity, and cost rises.
The utility model content
The purpose of this utility model provides a kind of hydrogenation system of hydrogen peroxide manufacture, makes its defective that can overcome prior art, makes that the Controllable Temperature in the hydrogenation tower is good, and the regeneration period of catalyst prolongs, the reaction efficiency height.
The purpose of this utility model is achieved in that a kind of hydrogenation system of hydrogen peroxide manufacture, comprises hydrogen filter, working fluid preheater, hydrogenation tower, hydride gas-liquid separator, hydride strainer, hydride Regenerative beds, hydride storage tank; The import of described hydrogen filter connects hydrogen source gas, the outlet of hydrogen filter connects the hydrogen inlet of hydrogenation tower, the import of working fluid preheater links to each other with the working fluid source, the outlet of working fluid preheater connects the working fluid import of hydrogenation tower, the hydrogenation tower bottom connects the hydride gas-liquid separator, simultaneously, connect the import of working fluid preheater through the hydride recycle pump, the outlet one tunnel of hydride gas-liquid separator connects the import of hydride strainer, another road connects the regeneration steam condenser, the condensate outlet of regeneration steam condenser connects the phlegma scale tank, and the outlet of phlegma scale tank connects working fluid preparation still; The outlet of hydride strainer is divided into two-way, and one the tunnel connects the hydride storage tank, and another road connects the hydride Regenerative beds, and the outlet of hydride Regenerative beds connects the hydride storage tank, and the outlet of hydride storage tank connects oxidation system through draw-off pump; Described hydrogenation tower is divided into Shang Ta and Xia Ta, the outlet of last tower links to each other with the top inlet of following tower, also be provided with the hydride water cooler between Shang Ta and the following tower, the import of hydride water cooler connects the outlet of going up tower bottom, and the outlet of hydride water cooler connects the import of top of tower down.
During this device work, working fluid enters the working fluid preheater, enters the hydrogenation tower again after the control certain temperature; Raw hydrogen enters top of tower together with working fluid remove the mechanical impurity that may carry secretly through hydrogen filter after; In last tower, 2-ethyl-anthraquinone and hydrogen carry out hydrogenation under the palladium catalysis, generate corresponding 2-ethyl hydrogen anthraquinone and a spot of tetrahydrochysene 2-ethyl-anthraquinone, the hydride of last tower bottom, a part can enter Xia Ta, another part can enter the hydride condenser, after condensation, enter Xia Ta again, proceeding hydrogenation in the tower down, enter the amount of the hydride in the condenser by adjustment, can change the temperature of the hydride that enters down tower, to guarantee that the long term operation of palladium catalyst is under the higher state of activity.Hydride enters the hydride gas-liquid separator with the foreign gas of not participating in the hydrogen that reacts at the bottom of the hydrogenation tower, isolating the hydrogenation tail gas of carrying partial solvent aromatic hydrocarbons secretly enters in the phlegma scale tank after the regeneration vapour cooler makes wherein most of aromatic hydrocarbons condensation, this part aromatic hydrocarbons is back into working fluid preparation still, recycling after cleaning, and isolated non-condensable gases can be from phlegma scale tank top flux meter metering back emptying; An isolated hydride part is sent the hydrogenation tower back to through circulation hydrogenation liquid pump in the hydride gas-liquid separator, another part hydride is pressed into the hydride strainer by hydrogen pressure, catalyst and carrier small quantities of powder that elimination washes away out in the hydrogenation tower, hydride after filtering divides two portions: a part accounts for 10% of total amount and enters the hydride Regenerative beds, make the small amount of degradation thing that generates in the hydrogenation process obtain entering the hydride storage tank after the regeneration, another part directly enters the hydride storage tank, relends to help the hydrogenation liquid pump that hydride is sent into oxidation system to carry out oxidation.Compared with prior art, the utility model makes the Shang Ta of hydrogenation tower and following tower isolated, carry out temperature regulation by the hydride condenser condenses, its beneficial effect is: (1) has at first been avoided hydrogenation temperature to wear out along with catalyst and has been improved, thereby guarantees that catalyst is unlikely to too fast aging; (2) realize maximally utilising the low temperature active district of catalyst, thereby effectively prolong the work-ing life of noble metal catalyst; (3) the anthraquinone hydrogenation reaction is carried out at a lower temperature, more helps overcoming the generation of paying reaction; (4) hydrogenation fixed bed temperature is avoided being in the highest state operation of total system, thereby effectively land productivity prevents that anthraquinone degradation polymer and metallic salt from the poly-tendency of the common knot of catalyst layer, effectively having prolonged the regeneration period; (5) realize the ingenious combination of two towers up and down, at the active Jie Duan ﹠amp of the different use of catalyst; Different hydrogenation stage is selected more rational catalyst bed temperature of reaction; The liquid spraying amount combines, thereby prevents the degree of depth hydrogenation of anthraquinone effectively; (6) component that can guarantee system works liquid is stablized.This system-specific is in the production of hydrogen peroxide.
For making the utility model compact construction, described hydride gas-liquid separator is arranged on down the bottom of tower, and is connected as a single entity with following tower inner chamber.Can reduce the setting of part pipeline, increase the gas-liquid separation interface, further guarantee gas-liquid separation effect.
For ease of with in the hydrogenation tower and the liquid emptying in the hydride storage tank, described down tower and hydride storage tank bottom are provided with pipeline and are connected working fluid and prepare still.Working fluid is capable of circulation in working fluid configuration still to be utilized again.
Description of drawings
Fig. 1 is the utility model structural representation.
Embodiment
As shown in the figure, be the fundamental diagram of the hydrogenation system of hydrogen peroxide manufacture, this hydrogenation system mainly includes hydrogen filter X1102, working fluid preheater E1101, hydrogenation tower, hydride gas-liquid separator, hydride strainer X1103A/B, hydride Regenerative beds V1103, hydride storage tank V1104; The import of described hydrogen filter X1102 connects hydrogen source gas, the outlet of hydrogen filter X1102 connects the hydrogen inlet of hydrogenation tower, the import of working fluid preheater E1101 links to each other with the working fluid source, the outlet of working fluid preheater E1101 connects the working fluid import of hydrogenation tower, the hydride outlet of hydrogenation tower bottom is connected as a single entity with the hydride gas-liquid separator, the hydrogenation tower bottom connects working fluid preheater E1101 import through hydride recycle pump P1, the outlet one tunnel of hydride gas-liquid separator connects the import of hydride strainer X1103A/B, another road connects regeneration steam condenser E1103, the condensate outlet of regeneration steam condenser E1103 connects phlegma scale tank V1102, and the outlet of phlegma scale tank V1102 connects working fluid preparation still; The outlet of hydride strainer X1103A/B is divided into two-way, one the tunnel connects hydride storage tank V1104, another road connects hydride Regenerative beds V1103, the outlet of hydride Regenerative beds V1103 connects hydride storage tank V1104, the outlet of hydride storage tank V1104 connects oxidation system through draw-off pump P2, P3, draw-off pump P2, P3 are arranged in parallel, and can work independently, and another is standby; Described hydrogenation tower is divided into tower T1101 and following tower T1102, the outlet of last tower T1101 links to each other with the top inlet of following tower T1102, also be provided with hydride water cooler E1102 between last tower T1101 and the following tower T1102, the import of hydride water cooler E1102 connects the outlet of going up tower T1101 bottom, and the outlet of hydride water cooler E1102 connects the import at tower T1102 top down; Described tower T1102 down is provided with pipeline with hydride storage tank V1104 bottom and is connected working fluid preparation still.The import of above-mentioned hydrogen filter X1102, working fluid preheater E1101, hydrogenation tower, hydride gas-liquid separator, hydride strainer X1103A/B, hydride Regenerative beds V1103, hydride storage tank V1104 and outlet all can be provided with corresponding valve, part valve can be level control valve, pressure controlled valve, temperature-sensing valve etc., to control corresponding flow, pressure and temperature.
During work, working fluid enters working fluid preheater E1101, enters the hydrogenation tower again after the control certain temperature; Raw hydrogen enters tower T1101 top together with working fluid remove the mechanical impurity that may carry secretly through hydrogen filter X1102 after; In last tower T1101,2-ethyl-anthraquinone and hydrogen carry out hydrogenation under the palladium catalysis, generate corresponding 2-ethyl hydrogen anthraquinone and a spot of tetrahydrochysene 2-ethyl-anthraquinone, the hydride of last tower T1101 bottom, a part can enter down tower T1102, another part can enter the hydride condenser, after condensation, enter down tower T1102 again, enter the amount of the hydride in the condenser by adjustment, can change the temperature of the hydride that enters down tower T1102, to guarantee that the long term operation of palladium catalyst is under the higher state of activity.Hydride enters the hydride gas-liquid separator with the foreign gas of not participating in the hydrogen that reacts at the bottom of the hydrogenation tower, isolating the hydrogenation tail gas of carrying partial solvent aromatic hydrocarbons secretly enters in the phlegma scale tank V1102 after the regeneration vapour cooler makes wherein most of aromatic hydrocarbons condensation, this part aromatic hydrocarbons is back into working fluid preparation still, recycling after cleaning, and isolated non-condensable gases can be from phlegma scale tank V1102 top flux meter metering back emptying; An isolated hydride part is sent the hydrogenation tower back to through circulation hydrogenation liquid pump in the hydride gas-liquid separator, another part hydride is pressed into hydride strainer X1103A/B by hydrogen pressure, catalyst and carrier small quantities of powder that elimination washes away out in the hydrogenation tower, hydride after filtering divides two portions: a part accounts for 10% of total amount and enters hydride Regenerative beds V1103, make the small amount of degradation thing that generates in the hydrogenation process obtain entering hydride storage tank V1104 after the regeneration, another part directly enters hydride storage tank V1104, relends to help the hydrogenation liquid pump that hydride is sent into oxidation system to carry out oxidation.
The hydrogenation efficiency of this hydrogenation system is stable, Shang Ta and the operation of following tower; Regeneration period, it was simple in structure at 6～12 months, and the palladium catalyst life-span is long, and under reasonable working conditions, catalyst life-span 〉=5 year to guaranteeing that ordinary production is stable and reduce material consumption, have been brought into play very important.
Claims (3)
1. the hydrogenation system of a hydrogen peroxide manufacture comprises hydrogen filter, working fluid preheater, hydrogenation tower, hydride gas-liquid separator, hydride strainer, hydride Regenerative beds, hydride storage tank; The import of described hydrogen filter connects hydrogen source gas, the outlet of hydrogen filter connects the hydrogen inlet of hydrogenation tower, the import of working fluid preheater links to each other with the working fluid source, the outlet of working fluid preheater connects the working fluid import of hydrogenation tower, the hydrogenation tower bottom connects the hydride gas-liquid separator, simultaneously, connect the import of working fluid preheater through the hydride recycle pump, the outlet one tunnel of hydride gas-liquid separator connects the import of hydride strainer, another road connects the regeneration steam condenser, the condensate outlet of regeneration steam condenser connects the phlegma scale tank, and the outlet of phlegma scale tank connects working fluid preparation still; The outlet of hydride strainer is divided into two-way, and one the tunnel connects the hydride storage tank, and another road connects the hydride Regenerative beds, and the outlet of hydride Regenerative beds connects the hydride storage tank, and the outlet of hydride storage tank connects oxidation system through draw-off pump; It is characterized in that: described hydrogenation tower is divided into Shang Ta and Xia Ta, the outlet of last tower links to each other with the top inlet of following tower, also be provided with the hydride water cooler between Shang Ta and the following tower, the import of hydride water cooler connects the outlet of going up tower bottom, and the outlet of hydride water cooler connects the import of top of tower down.
2. the hydrogenation system of hydrogen peroxide manufacture according to claim 1, it is characterized in that: described hydride gas-liquid separator is arranged on down the bottom of tower, and is connected as a single entity with following tower inner chamber.
3. the hydrogenation system of hydrogen peroxide manufacture according to claim 1 and 2 is characterized in that: described tower down and hydride storage tank bottom are provided with pipeline and are connected working fluid and prepare still.
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| CN2010201752648U CN201686492U (en) | 2010-04-29 | 2010-04-29 | Hydrogenation system for producing hydrogen peroxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011134345A1 (en) * | 2010-04-29 | 2011-11-03 | 扬州惠通化工技术有限公司 | Hydrogenating system for producing hydrogen peroxide |
| CN107032305A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | The production system and production method of a kind of hydrogen peroxide |
| CN107032306A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | Fluid bed produces the system and method for hydrogen peroxide |
| CN107032304A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | The hydrogenation apparatus and hydrogenation processes of fluid bed production hydrogen peroxide |
| CN107032303A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | The fluid bed production system and production method of hydrogen peroxide |
| CN107098318A (en) * | 2017-06-15 | 2017-08-29 | 扬州惠通化工科技股份有限公司 | Produce the fluid bed hydrogenation system and hydrogenation processes of hydrogen peroxide |
| CN111977615A (en) * | 2020-07-13 | 2020-11-24 | 中国空分工程有限公司 | Efficient hydrogen peroxide solution production hydrogenation system |
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2010
- 2010-04-29 CN CN2010201752648U patent/CN201686492U/en not_active Expired - Lifetime
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011134345A1 (en) * | 2010-04-29 | 2011-11-03 | 扬州惠通化工技术有限公司 | Hydrogenating system for producing hydrogen peroxide |
| CN107032305A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | The production system and production method of a kind of hydrogen peroxide |
| CN107032306A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | Fluid bed produces the system and method for hydrogen peroxide |
| CN107032304A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | The hydrogenation apparatus and hydrogenation processes of fluid bed production hydrogen peroxide |
| CN107032303A (en) * | 2017-06-15 | 2017-08-11 | 扬州惠通化工科技股份有限公司 | The fluid bed production system and production method of hydrogen peroxide |
| CN107098318A (en) * | 2017-06-15 | 2017-08-29 | 扬州惠通化工科技股份有限公司 | Produce the fluid bed hydrogenation system and hydrogenation processes of hydrogen peroxide |
| CN107032304B (en) * | 2017-06-15 | 2023-06-27 | 扬州惠通科技股份有限公司 | Hydrogenation reaction device and hydrogenation reaction method for producing hydrogen peroxide by fluidized bed |
| 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 |
| CN107032306B (en) * | 2017-06-15 | 2023-07-14 | 扬州惠通科技股份有限公司 | System and method for producing hydrogen peroxide by fluidized bed |
| CN107032305B (en) * | 2017-06-15 | 2023-07-14 | 扬州惠通科技股份有限公司 | Hydrogen peroxide production system and production method |
| CN107098318B (en) * | 2017-06-15 | 2023-07-14 | 扬州惠通科技股份有限公司 | Fluidized bed hydrogenation reaction system and hydrogenation reaction method for producing hydrogen peroxide |
| CN111977615A (en) * | 2020-07-13 | 2020-11-24 | 中国空分工程有限公司 | Efficient hydrogen peroxide solution production hydrogenation system |
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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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Granted publication date: 20101229 |