CN115259098A - Method for continuously producing hydrogen peroxide - Google Patents
Method for continuously producing hydrogen peroxide Download PDFInfo
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- CN115259098A CN115259098A CN202211020114.3A CN202211020114A CN115259098A CN 115259098 A CN115259098 A CN 115259098A CN 202211020114 A CN202211020114 A CN 202211020114A CN 115259098 A CN115259098 A CN 115259098A
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- temperature
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- hydrogen peroxide
- heated warehouses
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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
- C01B15/013—Separation; Purification; Concentration
Abstract
The invention relates to the technical field of hydrogen peroxide production, and discloses a method for continuously producing hydrogen peroxide, which comprises the following steps: firstly, evaporating hydrogen peroxide, then carrying out gas-liquid separation on the hydrogen peroxide, and then rectifying the gas phase obtained in the previous step; finally, the hydrogen peroxide solution can be obtained and recovered after rectification. According to the invention, the heating bin and the liquid storage bin are connected through the liquid conveying pipe, the first heating device and the second heating device are respectively arranged in the liquid conveying pipe and the heating bin, and the solution is respectively heated to the first temperature and the second temperature when being conveyed and heated, so that the solution can be heated to the evaporating temperature more quickly, the solution is evaporated more quickly, and the production efficiency is improved.
Description
Technical Field
The invention relates to the technical field of hydrogen peroxide production, in particular to a method for continuously producing hydrogen peroxide.
Background
The hydrogen peroxide production method is generally an anthraquinone method, in the anthraquinone method production, 2-Ethyl Anthraquinone (EAQ) is used as a carrier to prepare H2O2, heavy aromatic hydrocarbon and trioctyl phosphate (TOP) are used as mixed solvents to prepare solution (hereinafter referred to as working solution) with a certain composition, the working solution and hydrogen enter a hydrogenation tower filled with a palladium catalyst, hydrogenation reaction is carried out under certain pressure and temperature to obtain corresponding 2-ethyl hydrogen anthraquinone (HEAQ) solution (hereinafter referred to as hydrogenation solution), the hydrogenation solution is oxidized by oxygen in the air, the hydrogen anthraquinone in the solution generates anthraquinone and reacts to generate H2O2, pure water is used for extracting the working solution (hereinafter referred to as oxidation solution) containing the H2O2 to obtain an aqueous solution (commonly referred to as hydrogen peroxide) of the H2O2, the aqueous solution of the H2O2 is subjected to heavy aromatic hydrocarbon purification treatment and air purging to obtain an H2O2 product with the concentration of 27.5%, and the organic carbon content is generally 50mg/kg to 200mg/kg.
At present, when the hydrogen peroxide is produced, the solution generally needs to be heated, so that the solution is evaporated, and then the evaporated gas is separated, but the solution is generally directly heated by the current technology when the solution is heated, the solution is easily heated unevenly, so that the evaporation is incomplete, and the subsequent processing is influenced.
Disclosure of Invention
The present invention mainly solves the technical problems of the prior art, and therefore, the inventor provides a method for continuously producing hydrogen peroxide.
In order to achieve the above purpose, the present invention adopts the following technical scheme, and the method for continuously producing hydrogen peroxide comprises the following steps:
s1, evaporating hydrogen peroxide;
s2, carrying out gas-liquid separation on the hydrogen peroxide;
s3, rectifying the gas phase obtained in the previous step;
and S4, rectifying to obtain a hydrogen peroxide solution and recovering.
Preferably, the evaporation of hydrogen peroxide in S1 includes the following contents: at first set up heated warehouses and stock solution storehouse, be connected through the transfer line between heated warehouses and stock solution storehouse, heated warehouses's inside is provided with first heating device, the inside of transfer line is provided with second heating device, inner wall through setting up at the inside second heating device heating transfer line of transfer line, make the inner wall heat to the first temperature, solution will be heated to the first temperature when passing through the transfer line, inside through setting up at heated warehouses inside first heating device heating heated warehouses, make the inside temperature heating of heated warehouses to the second temperature, solution will further be heated to the second temperature and then evaporate in heated warehouses's inside.
Preferably, the gas-liquid separation of hydrogen peroxide in S2 includes the following steps: and (2) introducing the gas obtained by evaporation in the step (S1) into an oxidation tower, wherein a gas-liquid separator and a liquid-gas separator are arranged in the oxidation tower, the gas-liquid separator separates the gas from the oxidation liquid, the gas-liquid separator separates oxidation liquid drops carried in the tail gas, the liquid-gas separator is arranged at an upper seal head of the oxidation tower, and the gas-liquid separator is arranged at the top of the oxidation tower and connected with an air outlet pipe.
Preferably, the rectification of the gas phase obtained in the previous step in S3 includes the following steps: and introducing gas separated by the gas-liquid separator and the liquid-gas separator into the rectifying tower, condensing the gas phase discharged from the upper part of the rectifying tower into condensed water containing less than 0.1% of hydrogen peroxide by using a tower top condenser, allowing one part of the condensed water to enter a condensate collecting tank through a reflux ratio device, and allowing the other part of the condensed water to return to the rectifying tower as reflux.
Preferably, the distillation in S4 to obtain a hydrogen peroxide solution and the recovery includes the following contents: the intermediate product obtained by rectification at the lower part of the rectification tower flows into the storage container and is 60-65% of hydrogen peroxide solution.
Preferably, the second heating devices in S1 are uniformly distributed inside the infusion tube, so that the solution can be uniformly heated during the solution delivery, the first temperature is such that the liquid hydrogen peroxide entering the infusion tube will be completely evaporated when flowing through the infusion tube, and for optimal heat transfer, the first temperature is preferably 30-50 ℃ higher than the boiling temperature of the liquid to be evaporated.
Preferably, the first temperature is 120 ℃ to 140 ℃ and the second temperature is 200 ℃ to 250 ℃, the second temperature being higher than the first temperature.
As preferred, the inside of heated warehouses is provided with temperature-detecting device and automatic water injection device, electric connection between temperature-detecting device and the automatic water injection device, initiative water injection device and external storage water tank connection, and in the evaporation process, temperature-detecting device can detect the inside temperature of heated warehouses, and when the inside temperature of heated warehouses was higher than dangerous temperature, initiative water injection device will carry out the water injection to the inside of heated warehouses, reduces the inside temperature of heated warehouses, avoids solution because of the high explosion of temperature.
As preferred, the conveyer pipe is close to the one end fixed mounting of heated warehouses has atomizer, atomizer can spout solution into the inside of little drop of water to the heated warehouses for area of contact between solution and the heated warehouses increases, and the inside of heated warehouses is provided with agitating unit simultaneously, through carrying the inside back of heated warehouses with solution when the transfer line, stir solution through agitating unit, make the heated warehouses more even to the heat-conduction of solution, and then solution can be faster by the second temperature of being heated, make solution evaporation rate grow.
Advantageous effects
The invention provides a method for continuously producing hydrogen peroxide. The method has the following beneficial effects:
(1) The method for continuously producing the hydrogen peroxide is characterized in that the heating bin and the liquid storage bin are connected through the infusion tube, the first heating device and the second heating device are respectively arranged in the infusion tube and the heating bin, and the solution is firstly heated to the first temperature and the second temperature when the solution is conveyed and heated, so that the solution can be heated to the evaporating temperature more quickly, the solution is evaporated more quickly, and the production efficiency is improved.
(2) The method for continuously producing the hydrogen peroxide has the advantages that the gas-liquid separator and the liquid-gas separator are arranged, so that the separation effect of liquid and gas can be improved, the oxygen-poor air after reaction can be separated from the working solution in time, meanwhile, the working solution carried in the oxidized tail gas is reduced, the equipment pipeline investment is reduced, and the effects of improving the productivity and reducing the investment are achieved.
(3) This method of continuous production hydrogen peroxide, the inside of heated warehouses is provided with temperature-detecting device and automatic water injection device, electric connection between temperature-detecting device and the automatic water injection device, initiative water injection device and external storage water tank connection, in the evaporation process, temperature-detecting device can detect the inside temperature of heated warehouses, when the inside temperature of heated warehouses is higher than dangerous temperature, initiative water injection device will carry out the water injection to the inside of heated warehouses, reduce the inside temperature of heated warehouses, avoid solution because of the high explosion of temperature.
(4) This method of continuous production hydrogen peroxide, the one end fixed mounting that the conveyer pipe is close to the heated warehouses has atomizer, atomizer can spray into the inside of little drop of water to the heated warehouses with solution, make the area of contact increase between solution and the heated warehouses, the inside of heated warehouses is provided with agitating unit simultaneously, through carrying the inside back of heated warehouses with solution when the transfer line, stir solution through agitating unit, make the heated warehouses more even to the heat-conduction of solution, and then solution can be faster by heating to the second temperature, further make solution evaporation rate grow, accelerate production speed.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows: a process for the continuous production of hydrogen peroxide comprising the steps of:
s1, evaporating hydrogen peroxide;
the evaporation of hydrogen peroxide in the S1 comprises the following contents: at first set up heated warehouses and stock solution storehouse, be connected through the transfer line between heated warehouses and stock solution storehouse, heated warehouses's inside is provided with first heating device, the inside of transfer line is provided with second heating device, inner wall through setting up at the inside second heating device heating transfer line of transfer line, make the inner wall heat to the primary temperature, solution will be heated to the primary temperature when the transfer line of process, inside through setting up at heated warehouses inside first heating device heating heated warehouses, make heated warehouses inside temperature heating to the secondary temperature, solution will further be heated to the secondary temperature in heated warehouses's inside and then evaporate.
The second heating means are arranged distributed uniformly within the infusion tube so as to uniformly heat the solution as it is delivered, the first temperature being such that the liquid hydrogen peroxide entering the infusion tube will be completely vaporized as it flows through the infusion tube, the first temperature preferably being 30 ℃ above the boiling temperature of the liquid to be vaporized, the first temperature being 120 ℃ and the second temperature being 200 ℃ above the first temperature for optimum heat transfer.
The inside of heated warehouses is provided with temperature-detecting device and automatic water injection device, electric connection between temperature-detecting device and the automatic water injection device, initiative water injection device and external storage water tank connection, in the evaporation process, temperature-detecting device can detect the inside temperature of heated warehouses, when the inside temperature of heated warehouses is higher than dangerous temperature, initiative water injection device will carry out the water injection to the inside of heated warehouses, reduce the inside temperature of heated warehouses, avoid solution because of the high explosion of temperature.
One end fixed mounting that the conveyer pipe is close to the heated warehouses has atomizer, atomizer can spray into the inside of little drop of water to the heated warehouses with solution, make the area of contact increase between solution and the heated warehouses, the inside of heated warehouses is provided with agitating unit simultaneously, carry the inside back of heated warehouses through when the transfer line with solution, stir solution through agitating unit, it is more even to make the heated warehouses to the heat-conduction of solution, and then solution can be faster by heating to the second temperature, make solution evaporation rate grow.
S2, carrying out gas-liquid separation on the hydrogen peroxide;
and (2) introducing the gas obtained by evaporation in the step (S1) into an oxidation tower, wherein a gas-liquid separator and a liquid-gas separator are arranged in the oxidation tower, the gas-liquid separator separates the gas from the oxidation liquid, the gas-liquid separator separates the oxidation liquid drops carried in the tail gas, the liquid-gas separator is arranged at an upper end socket of the oxidation tower, and the gas-liquid separator is arranged at the top of the oxidation tower and connected with an air outlet pipe.
S3, rectifying the gas phase obtained in the previous step;
and introducing gas separated by the gas-liquid separator and the liquid-gas separator into the rectifying tower, condensing the gas phase discharged from the upper part of the rectifying tower into condensed water containing less than 0.1 percent of hydrogen peroxide by using a tower top condenser, introducing one part of the condensed water into a condensate collecting tank through a reflux ratio device, and returning the other part of the condensed water serving as reflux liquid into the rectifying tower.
S4, rectifying to obtain a hydrogen peroxide solution and recovering;
the intermediate product obtained by rectification at the lower part of the rectification tower flows into the storage container and is 60-65% of hydrogen peroxide solution.
Example two: on the basis of the first embodiment, the method comprises the following steps:
s1, evaporating hydrogen peroxide;
the evaporation of hydrogen peroxide in S1 comprises the following contents: at first set up heated warehouses and stock solution storehouse, be connected through the transfer line between heated warehouses and stock solution storehouse, heated warehouses's inside is provided with first heating device, the inside of transfer line is provided with second heating device, inner wall through setting up at the inside second heating device heating transfer line of transfer line, make the inner wall heat to the primary temperature, solution will be heated to the primary temperature when the transfer line of process, inside through setting up at heated warehouses inside first heating device heating heated warehouses, make heated warehouses inside temperature heating to the secondary temperature, solution will further be heated to the secondary temperature in heated warehouses's inside and then evaporate.
The second heating means are arranged distributed uniformly inside the infusion tube so as to heat the solution uniformly during the delivery thereof, the first temperature being such that the liquid hydrogen peroxide entering the infusion tube will be completely evaporated during the flow through the infusion tube, the first temperature preferably being 50 ℃ higher than the boiling temperature of the liquid to be evaporated, the first temperature being 140 ℃ and the second temperature being 250 ℃ higher than the first temperature for optimum heat transfer.
The inside of heated warehouses is provided with temperature-detecting device and automatic water injection device, electric connection between temperature-detecting device and the automatic water injection device, initiative water injection device and external storage water tank connection, in the evaporation process, temperature-detecting device can detect the inside temperature of heated warehouses, when the inside temperature of heated warehouses is higher than dangerous temperature, initiative water injection device will carry out the water injection to the inside of heated warehouses, reduce the inside temperature of heated warehouses, avoid solution because of the high explosion of temperature.
One end fixed mounting that the conveyer pipe is close to the heated warehouses has atomizer, atomizer can spray into the inside of little drop of water to the heated warehouses with solution, make the area of contact increase between solution and the heated warehouses, the inside of heated warehouses is provided with agitating unit simultaneously, carry the inside back of heated warehouses through when the transfer line with solution, stir solution through agitating unit, it is more even to make the heated warehouses to the heat-conduction of solution, and then solution can be faster by heating to the second temperature, make solution evaporation rate grow.
S2, carrying out gas-liquid separation on the hydrogen peroxide;
and (2) introducing the gas obtained by evaporation in the step (S1) into an oxidation tower, wherein a gas-liquid separator and a liquid-gas separator are arranged in the oxidation tower, the gas-liquid separator separates the gas from the oxidation liquid, the gas-liquid separator separates the oxidation liquid drops carried in the tail gas, the liquid-gas separator is arranged at an upper end socket of the oxidation tower, and the gas-liquid separator is arranged at the top of the oxidation tower and connected with an air outlet pipe.
S3, rectifying the gas phase obtained in the previous step;
and introducing gas separated by the gas-liquid separator and the liquid-gas separator into the rectifying tower, condensing the gas phase discharged from the upper part of the rectifying tower into condensed water containing less than 0.1% of hydrogen peroxide by using a tower top condenser, allowing one part of the condensed water to enter a condensate collecting tank through a reflux ratio device, and allowing the other part of the condensed water to return to the rectifying tower as reflux.
S4, rectifying to obtain a hydrogen peroxide solution and recovering;
the intermediate product obtained by rectification at the lower part of the rectification tower flows into the storage container and is 60-65% of hydrogen peroxide solution.
The working principle of the invention is as follows:
when in use, the utility model is used,
at first set up heated warehouses and stock solution storehouse, be connected through the transfer line between heated warehouses and stock solution storehouse, heated warehouses's inside is provided with first heating device, the inside of transfer line is provided with second heating device, inner wall through setting up at the inside second heating device heating transfer line of transfer line, make the inner wall heat to the first temperature, solution will be heated to the first temperature when passing through the transfer line, inside through setting up at heated warehouses inside first heating device heating heated warehouses, make the inside temperature heating of heated warehouses to the second temperature, solution will further be heated to the second temperature and then evaporate in heated warehouses's inside.
The inside of heated warehouses is provided with temperature-detecting device and automatic water injection device, electric connection between temperature-detecting device and the automatic water injection device, initiative water injection device and external storage water tank connection, in the evaporation process, temperature-detecting device can detect the inside temperature of heated warehouses, when the inside temperature of heated warehouses is higher than dangerous temperature, initiative water injection device will carry out the water injection to the inside of heated warehouses, reduce the inside temperature of heated warehouses, avoid solution because of the high explosion of temperature.
One end fixed mounting that the conveyer pipe is close to the heated warehouses has atomizer, atomizer can spray into the inside of little drop of water to the heated warehouses with solution, make the area of contact increase between solution and the heated warehouses, the inside of heated warehouses is provided with agitating unit simultaneously, carry the inside back of heated warehouses through when the transfer line with solution, stir solution through agitating unit, it is more even to make the heated warehouses to the heat-conduction of solution, and then solution can be faster by heating to the second temperature, make solution evaporation rate grow.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A process for the continuous production of hydrogen peroxide, characterized by: the method comprises the following steps:
s1, evaporating hydrogen peroxide;
s2, carrying out gas-liquid separation on the hydrogen peroxide;
s3, rectifying the gas phase obtained in the previous step;
and S4, rectifying to obtain a hydrogen peroxide solution and recovering.
2. A process for the continuous production of hydrogen peroxide according to claim 1, characterized in that: the evaporation of hydrogen peroxide in the S1 comprises the following contents: at first set up heated warehouses and stock solution storehouse, be connected through the transfer line between heated warehouses and stock solution storehouse, heated warehouses's inside is provided with first heating device, the inside of transfer line is provided with second heating device, inner wall through setting up at the inside second heating device heating transfer line of transfer line, make the inner wall heat to the first temperature, solution will be heated to the first temperature when passing through the transfer line, inside through setting up at heated warehouses inside first heating device heating heated warehouses, make the inside temperature heating of heated warehouses to the second temperature, solution will further be heated to the second temperature and then evaporate in heated warehouses's inside.
3. A process for the continuous production of hydrogen peroxide according to claim 1, characterized in that: the gas-liquid separation of the hydrogen peroxide in the S2 comprises the following contents: and (2) introducing the gas obtained by evaporation in the step (S1) into an oxidation tower, wherein a gas-liquid separator and a liquid-gas separator are arranged in the oxidation tower, the gas-liquid separator separates the gas from the oxidation liquid, the gas-liquid separator separates oxidation liquid drops carried in the tail gas, the liquid-gas separator is arranged at an upper seal head of the oxidation tower, and the gas-liquid separator is arranged at the top of the oxidation tower and connected with an air outlet pipe.
4. A process for the continuous production of hydrogen peroxide according to claim 1, characterized in that: the rectification of the gas phase obtained in the step 3 comprises the following steps: and introducing gas separated by the gas-liquid separator and the liquid-gas separator into the rectifying tower, condensing the gas phase discharged from the upper part of the rectifying tower into condensed water containing less than 0.1% of hydrogen peroxide by using a tower top condenser, allowing one part of the condensed water to enter a condensate collecting tank through a reflux ratio device, and allowing the other part of the condensed water to return to the rectifying tower as reflux.
5. A process for the continuous production of hydrogen peroxide according to claim 1, characterized in that: the step 4 of obtaining the hydrogen peroxide solution after rectification and recovering comprises the following contents: the intermediate product obtained by rectification at the lower part of the rectification tower flows into the storage container and is 60-65% of hydrogen peroxide solution.
6. A process for the continuous production of hydrogen peroxide according to claim 1, characterized in that: the second heating devices in the S1 are uniformly distributed in the infusion tube, so that the solution can be uniformly heated when being delivered, the first temperature is that the liquid hydrogen peroxide entering the infusion tube is completely evaporated when flowing through the infusion tube, and the first temperature is preferably 30-50 ℃ higher than the boiling temperature of the liquid to be evaporated for optimal heat transfer.
7. A process for the continuous production of hydrogen peroxide according to claim 6, characterized in that: the first temperature is 120-140 ℃, and the second temperature is 200-250 ℃, the second temperature being higher than the first temperature.
8. A process for the continuous production of hydrogen peroxide according to claim 2, characterized in that: the inside of heated warehouses is provided with temperature-detecting device and automatic water injection device, electric connection between temperature-detecting device and the automatic water injection device, initiative water injection device and external storage water tank connection, and in the evaporation process, temperature-detecting device can detect the inside temperature of heated warehouses, and when the inside temperature of heated warehouses was higher than dangerous temperature, initiative water injection device will carry out the water injection to the inside of heated warehouses, reduces the inside temperature of heated warehouses, avoids solution because of the high explosion of temperature.
9. A process for the continuous production of hydrogen peroxide according to claim 2, characterized in that: the one end fixed mounting that the conveyer pipe is close to the heated warehouses has atomizer, atomizer can spray into the inside of little drop of water to the heated warehouses with the solution for area of contact between solution and the heated warehouses increases, and the inside of heated warehouses is provided with agitating unit simultaneously, through carrying the inside back of heated warehouses with solution when the transfer line, stir solution through agitating unit, it is more even to make the heated warehouses heat-conduction of solution, and then solution can be faster by heating to the second temperature, make solution evaporation rate grow.
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| CN202211020114.3A CN115259098A (en) | 2022-08-24 | 2022-08-24 | Method for continuously producing hydrogen peroxide |
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| CN202211020114.3A CN115259098A (en) | 2022-08-24 | 2022-08-24 | Method for continuously producing hydrogen peroxide |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103523756A (en) * | 2013-10-23 | 2014-01-22 | 天津大沽化工股份有限公司 | Production method and device of high-concentration hydrogen peroxide |
| CN107185277A (en) * | 2017-06-01 | 2017-09-22 | 黎明化工研究设计院有限责任公司 | A kind of gas-liquid separation device of anthraquinone legal system hydrogen peroxide oxidation tower |
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2022
- 2022-08-24 CN CN202211020114.3A patent/CN115259098A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103523756A (en) * | 2013-10-23 | 2014-01-22 | 天津大沽化工股份有限公司 | Production method and device of high-concentration hydrogen peroxide |
| CN107185277A (en) * | 2017-06-01 | 2017-09-22 | 黎明化工研究设计院有限责任公司 | A kind of gas-liquid separation device of anthraquinone legal system hydrogen peroxide oxidation tower |
Non-Patent Citations (1)
| Title |
|---|
| 王恒通等: "《药厂GMP应知应会》", 中国医药科技出版社, pages: 219 * |
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