CN109019521B - Hydrogen peroxide concentration and purification device and application thereof in hydrogen peroxide concentration and purification - Google Patents
Hydrogen peroxide concentration and purification device and application thereof in hydrogen peroxide concentration and purification Download PDFInfo
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- CN109019521B CN109019521B CN201811288333.3A CN201811288333A CN109019521B CN 109019521 B CN109019521 B CN 109019521B CN 201811288333 A CN201811288333 A CN 201811288333A CN 109019521 B CN109019521 B CN 109019521B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/22—Evaporating by bringing a thin layer of the liquid into contact with a heated surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0045—Vacuum condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a hydrogen peroxide concentration and purification device and application thereof in hydrogen peroxide concentration and purification, which mainly comprises a purification tower (1), a falling film evaporator (2) and a rectifying tower (3), wherein a crude and dilute hydrogen peroxide pipeline is connected with the upper part of the purification tower, and an aromatic hydrocarbon pipeline is connected with the lower part of the purification tower; the hydrogen peroxide outlet at the bottom of the purifying tower is connected with the hydrogen peroxide inlet of the falling film evaporator, the hydrogen peroxide outlet at the lower part of the falling film evaporator is connected with the lower part of the rectifying tower, the hydrogen peroxide outlet at the bottom of the falling film evaporator is connected with the upper part of the purifying tower, the gas phase outlet at the top of the rectifying tower is connected with the condenser (10) at the top of the rectifying tower, the gas phase outlet of the condenser at the top of the rectifying tower is connected with the vacuum pump (11), and the hydrogen peroxide outlet at the bottom of the rectifying tower is connected with the high-purity hydrogen peroxide cooler (8). In the invention, as the adsorption tower is not used, part of the hydrogen peroxide after concentration is returned to the purification tower. Therefore, waste liquid and waste adsorbent generated in the adsorption process are reduced, and meanwhile, the effective components of the working solution are recovered, so that the consumption is reduced, and the safety performance of the device is improved.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and relates to a hydrogen peroxide concentration and purification device and application thereof in industrial production, in particular to application in hydrogen peroxide concentration and purification.
Background
Hydrogen peroxide is an important inorganic chemical raw material and is widely applied to various fields of papermaking, textile, chemical synthesis, military industry, electronics, food processing, medicine, cosmetics, environmental protection, metallurgy and the like. The hydrogen peroxide is decomposed to produce water and oxygen, and has no secondary pollution to the environment, and is a green chemical. At present, the anthraquinone method is generally adopted for producing hydrogen peroxide at home and abroad. The anthraquinone method for producing hydrogen peroxide uses anthraquinone derivative as working carrier, and uses hydrogen gas to hydrogenate anthraquinone derivative dissolved in organic solvent under the action of catalyst so as to produce correspondent hydroanthraquinone. Then, hydro-anthraquinone oxidizes to produce hydrogen peroxide and anthraquinone derivatives. Finally, extracting hydrogen peroxide in the organic solvent with water to obtain hydrogen peroxide water solution with a certain concentration as a product, and recycling working solution containing anthraquinone derivative and the organic solvent. Among them, the efficiency of the anthraquinone hydrogenation process directly determines the yield and concentration of hydrogen peroxide, and has decisive significance for the production of the whole hydrogen peroxide.
Along with the expansion of the application field of hydrogen peroxide, the requirements on hydrogen peroxide are higher and higher in many application fields such as caprolactam and propylene oxide production, and high concentration and high purity are required. The hydrogen peroxide is concentrated and purified, and the extracted crude hydrogen peroxide is subjected to a purification tower and then is subjected to an adsorption tower to continuously remove organic compounds, so that the TOC (total carbon) content is reduced. Because the adsorption tower is adopted, the adsorption quantity reaches saturation in a period of operation, the adsorption tower needs to be regenerated, methanol, alkali and the like are needed in the regeneration process, and a large amount of waste liquid and waste water are generated. Meanwhile, the adsorbent needs to be replaced when running for a certain time, so that dangerous solid wastes are generated; more importantly, the potential safety hazard exists during the treatment of the adsorption tower.
In order to overcome the defects, the invention provides a hydrogen peroxide concentration and purification device which does not need to pass through an adsorption tower.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a hydrogen peroxide concentration and purification device, which omits an adsorption tower in the prior art and reduces the consumption of hydrogen peroxide working solution. Simultaneously, the discharge amount of waste liquid, waste water and dangerous solid waste is reduced, and more importantly, the safety of the device is improved.
The technical scheme of the invention is as follows:
the hydrogen peroxide concentration and purification device mainly comprises a purification tower, a falling film evaporator and a rectifying tower, wherein a crude dilute hydrogen peroxide pipeline is connected with the upper part of the purification tower, and an aromatic hydrocarbon pipeline is connected with the lower part of the purification tower; the hydrogen peroxide outlet at the bottom of the purifying tower is connected with the hydrogen peroxide inlet of the falling film evaporator, the hydrogen peroxide outlet at the lower part of the falling film evaporator is connected with the lower part of the rectifying tower, the hydrogen peroxide outlet at the bottom of the falling film evaporator is connected with the upper part of the purifying tower, the gas phase outlet at the top of the rectifying tower is connected with the condenser, the gas phase outlet of the condenser is connected with the vacuum pump, and the hydrogen peroxide outlet at the bottom of the rectifying tower is connected with the cooler.
The hydrogen peroxide concentration and purification device is characterized in that a hydrogen peroxide outlet at the bottom of the purification tower is connected with a coalescer, passes through the coalescer and is connected with a preheater inlet, and the preheater outlet is connected with a hydrogen peroxide inlet of the falling film evaporator.
The hydrogen peroxide concentration and purification device is characterized in that a hydrogen peroxide outlet at the bottom of the falling film evaporator is connected with a circulating cooler through a centrifugal pump, and the outlet of the circulating cooler and a crude and thin hydrogen peroxide inlet pipeline of the purification tower are connected with the upper part of the purification tower together.
And the outlet centrifugal pump of the falling film evaporator is also connected with the feed pipeline of the falling film evaporator.
The hydrogen peroxide concentration and purification device is characterized in that a steam outlet pipeline of the rectifying tower is connected with a steam jet pump, the steam jet pump is used as a heat source of a falling film evaporator, and the falling film evaporator is used for heating the diluted hydrogen peroxide to concentrate the diluted hydrogen peroxide.
The falling film evaporator can also directly use steam as a heat source.
The hydrogen peroxide concentration and purification device is characterized in that after the noncondensable gas in the rectifying tower is cooled by the cooler in the rectifying tower, a gas phase outlet pipeline is connected with an inlet of a condenser at the top of the rectifying tower, an outlet of the condenser at the top of the rectifying tower is connected with a vacuum pump, and the noncondensable gas is discharged through the vacuum pump.
And the hydrogen peroxide concentration and purification device is characterized in that an aromatic hydrocarbon pipeline at the purification tower item is connected with the distillation device.
The application of the hydrogen peroxide concentration and purification device in the production of high-concentration and high-purity hydrogen peroxide is as follows:
crude dilute hydrogen peroxide with the weight concentration of 25-45% from the extraction process is introduced into the purifying tower from the upper part of the purifying tower, and aromatic hydrocarbon is introduced into the purifying tower from the lower part of the purifying tower; hydrogen peroxide after aromatic hydrocarbon extraction enters a coalescer from an outlet at the bottom of the purifying column, aromatic hydrocarbon is separated in the coalescer, the separated aromatic hydrocarbon enters a preheater for heating, the heated hydrogen peroxide enters a falling film evaporator for continuous heating, the concentration of hydrogen peroxide at the bottom of the falling film evaporator is about 50-70%, the concentration of hydrogen peroxide at the middle lower part is 18-30%, and the hydrogen peroxide at the lower part enters a rectifying column; the hydrogen peroxide with the concentration of 50-70% at the bottom of the falling film evaporator enters a circulating cooler for cooling through part of hydrogen peroxide of a circulating pump, then enters a purifying tower from the upper part of the purifying tower, and the rest hydrogen peroxide returns to an inlet of the falling film evaporator; the hydrogen peroxide from the falling film evaporator is rectified in a rectifying tower, and the hydrogen peroxide is concentrated to obtain high-purity hydrogen peroxide with the weight concentration of 50-70%, wherein the total carbon (TOC) amount is 10-50ppm (weight).
The theoretical plate number of the purifying tower is 3-15, and the weight ratio of aromatic hydrocarbon to crude hydrogen peroxide is 0.01-0.10. The temperature of the purifying tower is 15-45 ℃ and the operating pressure is normal.
The temperature of the falling film evaporator is 55-60 ℃, and the operating pressure is-0.092 to-0.095 MPa (gauge pressure); the weight ratio of the hydrogen peroxide returned to the purification tower from the bottom of the falling film evaporator to the high-purity hydrogen peroxide extracted from the rectifying tower is 1:1-5.
The operating temperature of the top of the rectifying tower is 38-45 ℃, and the operating pressure is-0.092 to-0.095 MPa (gauge pressure).
The steam evaporated in the rectifying tower is pressurized by an evaporation jet pump and then used as a heat source of the falling film evaporator, and the evaporation jet pump uses medium-pressure steam.
The non-condensable gas of the rectifying tower is cooled by a cooler in the rectifying tower, enters a condenser at the top of the rectifying tower for condensation, and then enters a vacuum pump for discharge.
The aromatic hydrocarbon extracted by the purifying tower can be treated by a distillation device, and the aromatic hydrocarbon can be recycled after TOC is removed; or for the configuration of working fluids.
Compared with the prior art, the hydrogen peroxide concentration and purification device provided by the invention has the advantages that the number of adsorption towers is reduced, and the safety performance of the device is improved. Because of the presence of the adsorption process, regeneration of the adsorbent is required, and methanol, alkali, etc. are required in the regeneration process, resulting in a large amount of waste liquid and wastewater. Meanwhile, the adsorbent needs to be replaced at a certain time, so that dangerous solid waste is generated; more importantly, the potential safety hazard exists during the treatment of the adsorption tower.
In the invention, because the adsorption process is not used, part of the concentrated hydrogen peroxide is returned to the purification tower, and the total carbon in the hydrogen peroxide is removed by utilizing the aromatic hydrocarbon extraction technology, and because the total carbon removed in the adsorption process contains more than 50% of the effective components of the ethyl anthraquinone and the tetrahydroethyl anthraquinone in the working solution, the effective components are extracted by aromatic hydrocarbon to obtain the working solution, and the consumption of the ethyl anthraquinone in the hydrogen peroxide production can be reduced.
The total carbon impurities of the hydrogen peroxide can be removed during the regeneration of the working solution, so that the investment is reduced, the product purity is improved, technical grade hydrogen peroxide is not produced, and the yield of high-purity grade hydrogen peroxide is improved.
Drawings
FIG. 1 shows a hydrogen peroxide concentration and purification device of the invention
In the figure: 1-purifying tower, 2-falling film evaporator, 3-rectifying tower, 4-coalescer, 5-preheater, 6-evaporating jet pump, 7-centrifugal pump, 8-high-purity hydrogen peroxide cooler, 10-rectifying tower top condenser, 11-vacuum pump and 13-circulating cooler
FIG. 2-concentration and purification device for hydrogen peroxide
In the figure: 1-purifying tower, 2-falling film evaporator, 3-rectifying tower, 4-coalescer, 5-preheater, 6-steam jet pump, 7-centrifugal pump, 8-high-purity hydrogen peroxide cooler, 9-technical hydrogen peroxide cooler, 10-rectifying tower top condenser, 11-vacuum pump, 12-adsorbing tower
SM-medium pressure steam SCM-steam condensate RWS-circulating water supply RWR-circulating backwater.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
example 1
The hydrogen peroxide concentration and purification device shown in the attached figure 1 mainly comprises a purification tower 1, a coalescer 4, a preheater 5, a falling film evaporator 2, a rectifying tower 3, a steam jet pump 6, a centrifugal pump 7, a circulating cooler 13, a rectifying tower top condenser 10, a vacuum pump 11 and a high-purity hydrogen peroxide cooler 8.
The concentration of the crude hydrogen peroxide sent by the extraction process is 25-45%, TOC is 200-800ppm, the crude hydrogen peroxide enters a purifying tower at the upper part of the tower, aromatic hydrocarbon enters the purifying tower from the lower part of the tower, the theoretical plate number of the purifying tower is 13, and the weight ratio of the aromatic hydrocarbon to the crude hydrogen peroxide is 0.01-0.10. The temperature of the purifying tower is 15-45 ℃ and the operating pressure is normal.
After passing through the purification tower, the TOC of hydrogen peroxide from the lower part of the purification tower is 100-350ppm, organic matters are separated by entering a coalescer, then the organic matters are sent to a preheater to be preheated to 33-38 ℃, then sent to a falling film evaporator to be heated, the heating temperature is 75-80 ℃, and medium-pressure steam is used for driving an evaporation jet pump steam as a heat source; delivering hydrogen peroxide with the concentration of 18-30% and TOC of 80-100ppm at the lower part of the falling film evaporator into a rectifying tower for rectifying; hydrogen peroxide with the concentration of about 50-60% and TOC of 20-50ppm is extracted from the bottom of the falling film evaporator, is cooled by a circulating cooler, returns to a crude hydrogen peroxide feeding pipe to be mixed with the crude hydrogen peroxide, enters a purifying tower, and has the temperature of 55-60 ℃ and the operating pressure of-0.092 to-0.095 MPa (gauge pressure). The weight ratio of the hydrogen peroxide returned to the purification tower from the bottom of the falling film evaporator to the high-purity hydrogen peroxide extracted from the rectifying tower is 1:1-5.
Rectifying and concentrating in a rectifying tower, pressurizing the concentrated steam by an evaporation jet pump, heating the steam by a falling film evaporator, rectifying and concentrating to obtain high-purity hydrogen peroxide with the concentration of 50-60% and the TOC content of 20-30ppm, cooling in a cooler, and delivering to a user for use. The operating temperature of the top of the rectifying tower is 38-45 ℃, and the operating pressure is-0.092 to-0.095 MPa (gauge pressure).
The implementation result shows that compared with the prior art, the method can reduce 0.71 kg/ton of waste liquid and 0.04 kg/ton of waste adsorbent, and can also reduce the consumption of ethyl anthraquinone by 5-15%. Meanwhile, the yield of the high-purity grade hydrogen peroxide is increased, and the technical grade hydrogen peroxide is not by-produced.
Example 2
The concentration of the crude hydrogen peroxide sent by the extraction procedure is 25 percent, TOC is 200-800ppm, the crude hydrogen peroxide enters a purifying tower at the upper part of the tower, aromatic hydrocarbon enters the purifying tower from the lower part of the tower, the theoretical plate number of the purifying tower is 15, and the weight ratio of the aromatic hydrocarbon to the crude hydrogen peroxide is 0.03-0.05. The temperature of the purifying tower is 20-40 ℃ and the operating pressure is normal.
After passing through the purification tower, the TOC of hydrogen peroxide from the lower part of the purification tower is 100-350ppm, organic matters are separated by entering a coalescer, then the organic matters are sent to a preheater to be preheated to 33-38 ℃, then sent to a falling film evaporator to be heated, the heating temperature is 75-80 ℃, and medium-pressure steam is used for driving an evaporation jet pump steam as a heat source; delivering hydrogen peroxide with the concentration of 18-30% and TOC of 80-100ppm at the lower part of the falling film evaporator into a rectifying tower for rectifying; hydrogen peroxide with the concentration of about 50-60% and TOC of 20-50ppm is extracted from the bottom of the falling film evaporator, is cooled by a circulating cooler, returns to a crude hydrogen peroxide feeding pipe to be mixed with the crude hydrogen peroxide, enters a purifying tower, and has the temperature of 55-60 ℃ and the operating pressure of-0.092 to-0.095 MPa (gauge pressure). The weight ratio of the hydrogen peroxide returned to the purification tower from the bottom of the falling film evaporator to the high-purity hydrogen peroxide extracted from the rectifying tower is 1:1-5.
Rectifying and concentrating in a rectifying tower, pressurizing the concentrated steam by an evaporation jet pump, heating the steam by a falling film evaporator, rectifying and concentrating to obtain high-purity hydrogen peroxide with the concentration of 50-70% and the TOC content of 10-20ppm, cooling in a cooler, and delivering to a user for use. The operating temperature of the top of the rectifying tower is 40-45 ℃, and the operating pressure is-0.092 to-0.095 MPa (gauge pressure).
The implementation result shows that compared with the prior art, the method can reduce 0.71 kg/ton of waste liquid and 0.04 kg/ton of waste adsorbent, and can also reduce the consumption of ethyl anthraquinone by 5-15%. Meanwhile, the yield of the high-purity grade hydrogen peroxide is increased, and the technical grade hydrogen peroxide is not by-produced.
Example 3
The concentration of the crude hydrogen peroxide sent by the extraction procedure is 45 percent, TOC is 200-800ppm, the crude hydrogen peroxide enters a purifying tower at the upper part of the tower, aromatic hydrocarbon enters the purifying tower from the lower part of the tower, the theoretical plate number of the purifying tower is 8, and the weight ratio of the aromatic hydrocarbon to the crude hydrogen peroxide is 0.03-0.05. The temperature of the purifying tower is 15-40 ℃ and the operating pressure is normal pressure.
After passing through the purification tower, the TOC of hydrogen peroxide from the lower part of the purification tower is 100-350ppm, organic matters are separated by entering a coalescer, then the organic matters are sent to a preheater to be preheated to 33-38 ℃, then sent to a falling film evaporator to be heated, the heating temperature is 75-80 ℃, and medium-pressure steam is used for driving an evaporation jet pump steam as a heat source; delivering hydrogen peroxide with the concentration of 18-30% and TOC of 80-100ppm at the lower part of the falling film evaporator into a rectifying tower for rectifying; hydrogen peroxide with the concentration of about 50-60% and TOC of 20-50ppm is extracted from the bottom of the falling film evaporator, is cooled by a circulating cooler, returns to a crude hydrogen peroxide feeding pipe to be mixed with the crude hydrogen peroxide, enters a purifying tower, and has the temperature of 55-60 ℃ and the operating pressure of-0.092 to-0.095 MPa (gauge pressure). The weight ratio of the hydrogen peroxide returned to the purification tower from the bottom of the falling film evaporator to the high-purity hydrogen peroxide extracted from the rectifying tower is 1:1-5.
Rectifying and concentrating in a rectifying tower, pressurizing the concentrated steam by an evaporation jet pump, heating the steam by a falling film evaporator, rectifying and concentrating to obtain high-purity hydrogen peroxide with the concentration of 50-70% and the TOC content of 30-50ppm, cooling in a cooler, and delivering to a user for use. The operating temperature of the top of the rectifying tower is 40-45 ℃, and the operating pressure is-0.092 to-0.095 MPa (gauge pressure).
The implementation result shows that compared with the prior art, the method can reduce 0.71 kg/ton of waste liquid and 0.04 kg/ton of waste adsorbent, and can also reduce the consumption of ethyl anthraquinone by 5-15%. Meanwhile, the yield of the high-purity grade hydrogen peroxide is increased, and the technical grade hydrogen peroxide is not by-produced.
Comparative example
The prior hydrogen peroxide concentration and purification device shown in figure 2 mainly comprises a purification tower 1, a coalescer 4, an adsorption tower 12, a preheater 5, a falling film evaporator 2, a centrifugal pump 7, a rectifying tower 3, a steam jet pump 6, a high-purity hydrogen peroxide cooler 8, a technical grade hydrogen peroxide cooler 9, a rectifying tower top condenser 10 and a vacuum pump 11.
The concentration of the crude hydrogen peroxide sent by the extraction process is 25-45%, TOC is 200-800ppm, the crude hydrogen peroxide enters a purifying tower at the upper part of the tower, aromatic hydrocarbon enters the purifying tower from the lower part of the tower, the theoretical plate number of the purifying tower is 13, and the weight ratio of the aromatic hydrocarbon to the crude hydrogen peroxide is 0.03-0.05. The temperature of the purifying tower is 20-40 ℃ and the operating pressure is normal.
After passing through the purifying tower, the TOC of hydrogen peroxide coming out of the lower part of the purifying tower is 100-350ppm, and after organic matters are separated out by the coalescer, the organic matters are sent to the adsorption tower for adsorption and decarbonization, and the TOC content is less than 60ppm.
After decarbonizing by an adsorption tower, delivering dilute hydrogen peroxide to a preheater for preheating to 33-38 ℃, then delivering the dilute hydrogen peroxide to a falling film evaporator for heating at 75-80 ℃, and using medium-pressure steam to drive evaporation jet pump steam as a heat source; hydrogen peroxide with the concentration of 18-30% and the TOC of 80-100ppm at the lower part of the falling film evaporator is fed into a rectifying tower for rectification; extracting technical grade hydrogen peroxide with the concentration of about 60 percent and the TOC of 20-50ppm from the bottom of the falling film evaporator, and cooling the technical grade hydrogen peroxide by a cooler to obtain a product; the ratio of the hydrogen peroxide extracted from the lower part to the hydrogen peroxide extracted from the bottom is 3:1. The temperature of the falling film evaporator is 55-60 ℃, and the operating pressure is-0.092 to-0.095 MPa (gauge pressure).
Rectifying and concentrating in a rectifying tower, pressurizing the concentrated steam by an evaporation jet pump, heating the steam by a falling film evaporator, rectifying and concentrating to obtain high-purity hydrogen peroxide with the concentration of 50-60% and the TOC content of 10-50ppm, cooling in a cooler, and delivering to a user for use. The operating temperature of the top of the rectifying tower is 40-45 ℃, and the operating pressure is-0.092 to-0.095 MPa (gauge pressure).
Because the adsorption decarburization technology is used, the adsorption tower needs to be regenerated by using methanol and alkali after running for 800 hours, and organic waste liquid is produced by regeneration, and meanwhile, the adsorbent needs to be replaced after a certain number of times. One ton of hydrogen peroxide (27.5% folded) is produced, 0.71kg of regenerated waste liquid (folded continuous) and 0.04kg of waste adsorbent (folded continuous) are produced.
Claims (9)
1. The hydrogen peroxide concentration and purification device mainly comprises a purification tower (1), a falling film evaporator (2) and a rectifying tower (3), wherein a crude and thin hydrogen peroxide pipeline is connected with the upper part of the purification tower, and an aromatic hydrocarbon pipeline is connected with the lower part of the purification tower; the hydrogen peroxide outlet at the bottom of the purifying tower is connected with the hydrogen peroxide inlet of the falling film evaporator, the hydrogen peroxide outlet at the lower part of the falling film evaporator is connected with the lower part of the rectifying tower, the hydrogen peroxide outlet at the bottom of the falling film evaporator is connected with the upper part of the purifying tower, the gas phase outlet at the top of the rectifying tower is connected with the condenser (10) at the top of the rectifying tower, the gas phase outlet of the condenser at the top of the rectifying tower is connected with the vacuum pump (11), the hydrogen peroxide outlet at the bottom of the rectifying tower is connected with the high-purity hydrogen peroxide cooler (8), the hydrogen peroxide outlet at the bottom of the falling film evaporator is connected with the circulating cooler (12) through the centrifugal pump (7), and the outlet of the circulating cooler is connected with the crude dilute hydrogen peroxide inlet pipeline of the purifying tower at the upper part of the purifying tower.
2. The hydrogen peroxide concentration and purification device according to claim 1, wherein the hydrogen peroxide outlet at the bottom of the purification tower is connected with the coalescer (4), passes through the coalescer (4) and is connected with the inlet of the preheater (5), and the outlet of the preheater is connected with the hydrogen peroxide inlet of the falling film evaporator.
3. The hydrogen peroxide concentration and purification device according to claim 1, wherein the outlet of the centrifugal pump is further connected with a feed line of the falling film evaporator.
4. The hydrogen peroxide concentration and purification device according to claim 1, wherein a rectifying tower steam outlet pipeline is connected with a steam jet pump (6).
5. The hydrogen peroxide concentration and purification device according to claim 1, wherein the aromatic hydrocarbon pipeline at the top of the purification tower is connected with the distillation device.
6. The hydrogen peroxide concentration and purification device according to claim 1, wherein after the noncondensable gas in the rectifying tower is cooled by the in-tower cooler, a gas phase outlet pipeline is connected with an inlet of a condenser at the top of the rectifying tower, an outlet of the condenser at the top of the rectifying tower is connected with a vacuum pump, and the noncondensable gas is discharged by the vacuum pump.
7. Use of the hydrogen peroxide concentration and purification device according to any one of claims 1-6 in hydrogen peroxide concentration and purification, wherein crude and diluted hydrogen peroxide with the weight concentration of 25-45% from the extraction process is introduced into a purification tower from the upper part of the purification tower, and aromatic hydrocarbon is introduced into the lower part of the purification tower; hydrogen peroxide after aromatic hydrocarbon extraction enters a coalescer from an outlet at the bottom of the purifying tower, aromatic hydrocarbon is separated in the coalescer, the separated aromatic hydrocarbon enters a preheater for heating, the heated hydrogen peroxide enters a falling film evaporator for heating, the hydrogen peroxide with the concentration of 50-70% at the bottom of the falling film evaporator, the concentration of hydrogen peroxide at the middle lower part is 18-30%, and the hydrogen peroxide at the lower part enters a rectifying tower; the hydrogen peroxide with the concentration of 50-70% at the bottom of the falling film evaporator enters a circulating cooler to be cooled after passing through a circulating pump, then enters a purifying tower from the upper part of the purifying tower, and the rest hydrogen peroxide returns to an inlet of the falling film evaporator; the hydrogen peroxide from the falling film evaporator is rectified in a rectifying tower, and the hydrogen peroxide is concentrated to obtain high-purity hydrogen peroxide with the weight concentration of 50-70%, wherein the TOC weight content is 10-50ppm.
8. The hydrogen peroxide concentration and purification device for hydrogen peroxide concentration and purification, according to claim 7, wherein the theoretical plate number of the purification tower is 3-15, and the weight ratio of aromatic hydrocarbon to crude hydrogen peroxide is 0.01-0.10; the temperature of the purifying tower is 15-45 ℃ and the operating pressure is normal pressure; the temperature of the falling film evaporator is 55-60 ℃, the operating pressure gauge pressure is-0.092 to-0.095 MPa, and the weight ratio of the hydrogen peroxide returned from the bottom of the falling film evaporator to the purification tower to the high-purity hydrogen peroxide extracted from the rectifying tower is 1:1-5; the operating temperature of the top of the rectifying tower is 38-45 ℃, and the operating pressure gauge pressure is minus 0.092 to minus 0.095MPa.
9. The application of the hydrogen peroxide concentration and purification device in hydrogen peroxide concentration and purification as claimed in claim 7, wherein the aromatic hydrocarbon is treated by a distillation device after extraction in the purification tower, and the aromatic hydrocarbon is recycled or used for preparing working solution after TOC removal.
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| CN113912019A (en) * | 2021-11-29 | 2022-01-11 | 湖南双阳高科化工有限公司 | Production method of electronic grade hydrogen peroxide aqueous solution |
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| WO2003022737A1 (en) * | 2001-09-07 | 2003-03-20 | Basf Aktiengesellschaft | Method for the preparation of an aqueous hydrogen peroxide solution from a direct synthesis |
| JP2008087992A (en) * | 2006-09-29 | 2008-04-17 | Mitsubishi Gas Chem Co Inc | Method for producing hydrogen peroxide by anthraquinone process |
| CN102757019A (en) * | 2012-06-14 | 2012-10-31 | 天津大学 | System and method for concentrating and purifying hydrogen peroxide |
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| TW305821B (en) * | 1993-09-13 | 1997-05-21 | Mitsubishi Gas Chemical Co | |
| CN102161475A (en) * | 2009-11-02 | 2011-08-24 | 郑国玉 | Concentration method in production of hydrogen peroxide by anthraquinone method |
| DE102010039748A1 (en) * | 2010-08-25 | 2012-03-01 | Evonik Degussa Gmbh | Process for concentrating aqueous hydrogen peroxide solution |
| CN103657121B (en) * | 2012-09-17 | 2015-11-25 | 中国石油化工股份有限公司 | A kind of renovation process of extracting, rectifying and separating phenylethylene solvent for use |
| PL403721A1 (en) * | 2013-04-30 | 2014-11-10 | Instytut Lotnictwa | Method for preparing hydrogen peroxide, in particular HTP class for uses in the drive systems for the vacuum distillation |
| CN209098188U (en) * | 2018-10-31 | 2019-07-12 | 湖南百利工程科技股份有限公司 | A kind of hydrogen peroxide concentration purifying plant |
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|---|---|---|---|---|
| JPH08310803A (en) * | 1995-05-18 | 1996-11-26 | Mitsubishi Gas Chem Co Inc | Production of refined hydrogen peroxide |
| WO2003022737A1 (en) * | 2001-09-07 | 2003-03-20 | Basf Aktiengesellschaft | Method for the preparation of an aqueous hydrogen peroxide solution from a direct synthesis |
| JP2008087992A (en) * | 2006-09-29 | 2008-04-17 | Mitsubishi Gas Chem Co Inc | Method for producing hydrogen peroxide by anthraquinone process |
| CN102757019A (en) * | 2012-06-14 | 2012-10-31 | 天津大学 | System and method for concentrating and purifying hydrogen peroxide |
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