CN109200744B - Method for treating tail gas in hydrogen peroxide production process - Google Patents
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- CN109200744B CN109200744B CN201710521924.XA CN201710521924A CN109200744B CN 109200744 B CN109200744 B CN 109200744B CN 201710521924 A CN201710521924 A CN 201710521924A CN 109200744 B CN109200744 B CN 109200744B
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
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- B01D2257/7027—Aromatic hydrocarbons
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Abstract
The tail gas treatment method in the hydrogen peroxide production process comprises the steps of condensing hydrogen peroxide oxidized tail gas to 5-30 ℃, introducing the hydrogen peroxide oxidized tail gas into an adsorption resin column, adsorbing aromatic hydrocarbon by using adsorption resin, and purifying the hydrogen peroxide tail gas; the adsorption resin is soaked in toluene, methyl isobutyl ketone and distilled water separately before use. The invention modifies the adsorption resin, sequentially soaks the adsorption resin with toluene and methyl isobutyl ketone, and soaks the adsorption resin with water by sectional partial pressure, thereby not only improving the specific surface, pore volume and pore diameter of the adsorption resin, but also improving the stability of the adsorption resin; the adsorbent is used for the hydrogen peroxide tail gas purification process, and has the advantages of good purification effect, high strength, long service cycle, simple operation and low energy consumption.
Description
Technical Field
The invention relates to a method for treating tail gas in a hydrogen peroxide production process, and relates to a method for separating and recovering aromatic hydrocarbon in the tail gas.
Background
The tail gas from the anthraquinone process to produce hydrogen peroxide comes from an oxidation tower, and the aromatic hydrocarbon content in the tail gas reaches 20g/m after the tail gas is condensed (10-20 ℃)3-30g/m3. The aromatic hydrocarbon has strong volatility and is easy to run and damage along with gas phase, and the aromatic hydrocarbon belongs to benzene substances, so the environmental pollution is serious if the aromatic hydrocarbon is not recovered in time. The general treatment method is that the tail gas is firstly condensed by a heat exchanger to most of aromatic hydrocarbon gas, then the pressure of the oxidized tail gas is used as power, the temperature is cooled by an expansion unit, the heavy aromatic hydrocarbon in the tail gas is further condensed and recovered, and the heavy aromatic hydrocarbon is directly discharged after being adsorbed by activated carbon fibers.
Because the liquid drop diameter of the liquid aromatic hydrocarbon carried in the tail gas is very small, usually 1um-l0um, the common condensation-adsorption is adopted to adsorb the aromatic hydrocarbon in the tail gas, besides the gas aromatic hydrocarbon to be adsorbed, the aromatic hydrocarbon in the small drop form also needs to be adsorbed, thus greatly increasing the load of an adsorption device.
To solve the above problemsIn the problem, patent CN1483503A discloses a method for purifying and recovering aromatic hydrocarbons in tail gas of a hydrogen peroxide production device, which uses a pretreated activated carbon catalyst as an adsorbent to remove aromatic hydrocarbons in the tail gas, and uses superheated steam or N2Heating at 120-400 deg.c for desorption.
Patents CN106139824A and CN204550425A disclose a hydrogen peroxide oxidized tail gas recycling device, which comprises an absorption tower, a rich liquid tank, a stripping tower, a separator, a recovery tank, a rectifying tower and a refining tank, which are connected in sequence through pipelines; the device is also provided with a barren liquor tank, a discharge hole of the barren liquor tank is connected to the absorption tower, the stripping tower and the rectifying tower are provided with feed inlets which are connected to the barren liquor tank through pipelines, the top of the absorption tower is provided with an emptying pipeline, the top of the absorption tower is provided with an adsorption tank, and carbon fibers are filled in the adsorption tank.
In patent CN1973958A, it is described that two adsorption beds filled with adsorbent are used to alternately adsorb and desorb organic matters in tail gas, and the desorption gas uses compressed air or nitrogen to regenerate adsorbent, and then uses existing cooler, absorption tower, spray tower and other equipment to recover aromatic hydrocarbon.
Patent CN102008862A discloses a recovery device and a recovery method for aromatic hydrocarbon in tail gas in hydrogen peroxide production process, the method adopts a condensation mode to condense most of aromatic hydrocarbon, then adopts a gas-liquid removing device to remove aromatic hydrocarbon liquid drops in tail gas, and then further absorbs aromatic hydrocarbon by an adsorption device to reach relevant emission standards.
Patents CN106139789A and CN204543898A disclose a device for increasing recovery rate of aromatic hydrocarbons in hydrogen peroxide oxidized tail gas, which includes a first-stage condenser, an intermediate separation tank, a second-stage condenser, a cyclone separator, and an oil-water separator.
Patent CN202700289A discloses a device for treating tail gas generated by hydrogen peroxide oxidation, which comprises a tank body arranged outside a membrane filter, a tail gas inlet arranged on the left side edge of the lower part of the tank body, and a tail gas outlet arranged on the upper part of the tank body, wherein the tail gas inlet is used for collecting and filtering liquid drops in a gas state.
The tail gas treatment device mentioned in the above documents generally has the problems of high operating cost, complex flow, high energy consumption, unsatisfactory staticizing treatment effect and the like, so that aromatic hydrocarbons in the tail gas are fully recovered in a proper mode, the discharged tail gas is stably discharged up to the standard, and the tail gas treatment device has important significance for reducing the production cost and protecting the environment.
Disclosure of Invention
In order to solve the problems of complex treatment process, high cost and substandard tail gas purification effect of a tail gas purification treatment method generated in the hydrogen peroxide production process in the prior art, the invention provides the tail gas purification treatment method, which treats the adsorption resin by a specific means, and the treated adsorption resin performs adsorption separation on the tail gas, so that aromatic hydrocarbon in the tail gas is fully recovered, and the discharged tail gas reaches the standard.
In order to achieve the technical purpose, the invention adopts the following technical means:
the invention provides a method for treating tail gas in a hydrogen peroxide production process, which comprises the following steps: condensing the tail gas to 5-30 ℃, introducing an adsorption resin column for separation, recovering aromatic hydrocarbons in the tail gas, and purifying the tail gas;
the adsorbent resin filled in the adsorbent resin column is purified in the following way before use:
firstly, soaking the mixture in toluene for 8 to 24 hours at the temperature of between 50 and 130 ℃; then soaking the mixture for 4 to 24 hours at the temperature of between 50 and 120 ℃ by using methyl isobutyl ketone, and then soaking the mixture in three stages by using distilled water with the oxygen content of less than or equal to 10 mg/L: the first stage treatment conditions are that the pressure is 0.5MPa to 1.0MPa, the temperature is 65 ℃ to 80 ℃, and the soaking time is 8h to 12 h; the second stage treatment conditions are that the pressure is 0.9MPa to 1.0MPa, the temperature is 85 ℃ to 100 ℃, and the soaking time is 12h to 24 h; the third stage treatment conditions are that the pressure is 1.0MPa to 1.5MPa, the temperature is 120 ℃ to 130 ℃, and the soaking time is 12h to 24 h; and (3) simultaneously introducing inert gas or nitrogen into the three stages, and finally washing and drying.
In the treatment method, in the process of soaking the adsorption resin, the volume ratio of the toluene or the methyl isobutyl ketone to the adsorption resin is 5-10: 1; preferably 5-8: 1, most preferably 5-6: 1.
In the treatment method, the temperature of soaking in toluene is preferably 80-120 ℃, and the soaking time is preferably 10-16 h. The soaking temperature of the methyl isobutyl ketone is preferably 60-80 ℃, and the soaking time is preferably 6-12 h.
In the above treatment method, the oxygen content of the distilled water used for soaking the adsorption resin is preferably not more than 5mg/L, more preferably not more than 3mg/L (in the conditions of 20 ℃ and 100 kPa).
In the above treatment method, it is further preferable that the flow rates of the inert gas or the nitrogen gas are 20m each in the three stages of the soaking of the adsorption resin in distilled water3/h～50m3/h、10m3/h～25m3H and 5m3/h～10m3/h。
In the treatment method, the temperature of the tail gas introduced into the adsorption resin column is 5-30 ℃, preferably 5-25 ℃, and more preferably 5-15 ℃.
In the above treatment method, the operation pressure of the adsorption resin column is controlled to be 0.05MPa to 0.5MPa, preferably 0.1MPa to 0.5MPa, and most preferably 0.1MPa to 0.2 MPa.
In the treatment method, the feeding volume airspeed of the hydrogen peroxide oxidized tail gas introduced into the adsorption resin column is 5m3/h～25m3H, preferably 5m3/h～15m3H, most preferably 5m3/h～10m3/h。
In the above treatment method, it will be understood by those skilled in the art that the adsorbent resin is a conventional adsorbent resin, which is well known to those skilled in the art, and can be made by the prior art or commercially available, such as LSA-5BG type adsorbent resin produced by Xian Langxi New materials Ltd used in the present invention.
Compared with the prior art, the hydrogen peroxide tail gas purification method has the following advantages:
the invention modifies the adsorption resin, sequentially soaks the adsorption resin with toluene and methyl isobutyl ketone, and soaks the adsorption resin with water by sectional partial pressure, thereby not only improving the specific surface, pore volume and pore diameter of the adsorption resin, but also improving the stability of the adsorption resin; the adsorbent is used for the purification process of the hydrogen peroxide oxidized tail gas, and has the advantages of good purification effect, high strength, low operation cost and the like.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
FIG. 1 is a flow chart of a specific process for treating tail gas in the hydrogen peroxide production process used in the example;
FIG. 2 is a schematic view of an adsorption column;
wherein, 1, a first-stage condenser, 2, an eluent tank, 3, an adsorption column, 4, a delivery pump, 5, a valve, 6, a waste eluent tank, 31, a resin charging port; 32. a purified tail gas outlet; 33. an eluent inlet; 34. adsorbing a resin column cylinder; 35. an adsorbent resin; 36. an adsorbent resin discharge port; 37. an eluent outlet; 38. and a tail gas inlet.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
In the following embodiments, the process flow apparatus shown in fig. 1 is used to treat the hydrogen peroxide oxidation tail gas, as shown in fig. 1 and 2, the tail gas is condensed to 5-30 ℃ by the primary condenser 1, and enters the lower part of the adsorption column 3 through the valve 5 from the tail gas inlet 38, the adsorption column 3 has a resin charging port 31, a purified tail gas outlet 32, an eluent inlet 33, an adsorption resin column cylinder 34, the other end of the adsorption resin column cylinder 34 is provided with the tail gas inlet 38, and the side surface of the adsorption resin column cylinder 34 is provided with an adsorption resin discharging port 36 and an eluent outlet 37. Hydrogen peroxide oxidized tail gas flows in the adsorption resin 35, is directly emptied through a purified tail gas outlet 32 after being purified by the adsorption resin, then the eluent in the eluent tank 2 is input into the adsorption resin column 3 by using the delivery pump 4 to elute aromatic hydrocarbon in the resin, and the eluted aromatic hydrocarbon and the eluent enter the waste eluent tank 6 through an eluent outlet 37. When the resin no longer has the capacity to adsorb aromatic hydrocarbons or the adsorption capacity is not sufficient to require replacement, the resin is discharged from the adsorbent resin discharge port 36.
The adsorption resins adopted in the embodiment of the invention are LSA-5BG type and XDA-1 type produced by Xian blue Xiao New materials GmbH, DA201 type and DA201-B type produced by Zheng Zhou Duoji science and technology GmbH, which are respectively numbered as L1, L2, L3 and L4, and the specific properties are shown in Table 1.
TABLE 1
Example 1
Soaking the adsorption resin L1 in toluene at 60 ℃ for 24h, filtering, and soaking in methyl isobutyl ketone at 50 ℃ for 20h, wherein the volume ratio of toluene or methyl isobutyl ketone to adsorption resin is 10: and 1, filtering, washing and drying for later use. 500mL of the above-treated resin was put into deoxygenated water having an oxygen content of 3mg/L at a rate of 20 m/hr3Introducing nitrogen at a flow rate, and soaking for 12h at a pressure of 0.6MPa and a temperature of 65 ℃; the nitrogen flow rate was then adjusted to 15m3Soaking for 18 hours at 90 ℃ under the pressure of 1.0 MPa; the nitrogen flow rate was adjusted to 5m3And h, soaking for 24h under the conditions that the pressure is increased to 1.5MPa and the temperature is increased to 120 ℃, and washing and drying after the treatment are finished to obtain the modified adsorption ion exchange resin GL 1.
Example 2
The adsorbent resin L2 was modified by the same procedure as in example 1 to obtain adsorbent resin GL 2.
Example 3
The adsorbent resin L3 was modified by the same procedure as in example 1 to obtain adsorbent resin GL 3.
Example 4
The adsorbent resin L4 was modified by the same procedure as in example 1 to obtain adsorbent resin GL 4.
The pore structures of L1-L4 and GL1-GL4 before and after modification were measured by a 2400 adsorption apparatus, and the results are shown in Table 2.
TABLE 2
The strength of the adsorption resin before and after modification was determined according to the method of the national standard GB/T12598-2001, and the test results are shown in Table 3.
TABLE 3
Example 5
The adsorption columns were loaded with the adsorption resins L1-L4 and GL1-GL4 before and after modification, and applied to the hydrogen peroxide oxidation tail gas purification process in the process flow of FIG. 1, and the results are shown in Table 4.
Table 4.
As can be seen from table 4, when the modified adsorption resin is used to treat the hydrogen peroxide oxidized tail gas, the content of aromatic hydrocarbons in the treated tail gas is lower, which shows that the hydrogen peroxide oxidized tail gas purification method of the present invention has a significant effect on aromatic hydrocarbons in the tail gas.
Claims (14)
1. The method for treating tail gas in the hydrogen peroxide production process comprises the following steps: condensing the tail gas to 5-30 ℃, introducing an adsorption resin column for separation, recovering aromatic hydrocarbons in the tail gas, and purifying the tail gas;
the adsorbent resin filled in the adsorbent resin column is purified in the following way before use:
firstly, soaking the mixture in toluene for 8 to 24 hours at the temperature of between 50 and 130 ℃; then soaking the mixture for 4 to 24 hours at the temperature of between 50 and 120 ℃ by using methyl isobutyl ketone, and then soaking the mixture in three stages by using distilled water with the oxygen content of less than or equal to 10 mg/L: the first stage treatment conditions are that the pressure is 0.5MPa to 1.0MPa, the temperature is 65 ℃ to 80 ℃, and the soaking time is 8h to 12 h; the second stage treatment conditions are that the pressure is 0.9MPa to 1.0MPa, the temperature is 85 ℃ to 100 ℃, and the soaking time is 12h to 24 h; the third stage treatment conditions are that the pressure is 1.0MPa to 1.5MPa, the temperature is 120 ℃ to 130 ℃, and the soaking time is 12h to 24 h; introducing inert gas or nitrogen into the three stages at the same time, and finally washing and drying;
the adsorbent resin is selected from one of LSA-5BG type adsorbent resin, XDA-1 type adsorbent resin, DA201 type adsorbent resin and DA201-B type adsorbent resin.
2. The treatment method according to claim 1, wherein during the soaking treatment of the adsorption resin, the volume ratio of the toluene or the methyl isobutyl ketone to the adsorption resin is 5-10: 1.
3. the treatment method according to claim 2, wherein the temperature for soaking in toluene is 80 ℃ to 120 ℃, and the soaking time is 10h to 16 h.
4. The treatment method according to claim 2, wherein the temperature of the soaking with the methyl isobutyl ketone is 60 ℃ to 80 ℃, and the soaking time is 6h to 12 h.
5. The process according to claim 1, wherein the flow rates of the inert gas or nitrogen gas introduced into the adsorption resin in the three stages of the distilled water soaking are 20m each3/h～50m3/h、10m3/h～25m3H and 5m3/h～10m3/h。
6. The process of claim 1 wherein the temperature of the off-gas introduced into the adsorbent resin column is 5 ℃ to 30 ℃.
7. The treatment method according to claim 6, wherein the temperature of the tail gas introduced into the adsorption resin column is 5 ℃ to 25 ℃.
8. The treatment method according to claim 7, wherein the temperature of the tail gas introduced into the adsorption resin column is 5 ℃ to 15 ℃.
9. The treatment method according to claim 1, wherein the operation pressure of the adsorption resin column is controlled to be 0.05MPa to 0.5 MPa.
10. The treatment method according to claim 9, wherein the operation pressure of the adsorption resin column is controlled to be 0.1 to 0.5 MPa.
11. The treatment method according to claim 10, wherein the operation pressure of the adsorption resin column is controlled to be 0.1 to 0.2 MPa.
12. The treatment method according to claim 1, wherein the feed volume space velocity of the hydrogen peroxide oxidized tail gas introduced into the adsorption resin column is 5m3/h～25m3/h。
13. The treatment method according to claim 12, wherein the feed volume space velocity of the hydrogen peroxide oxidized tail gas introduced into the adsorption resin column is 5m3/h～15m3/h。
14. The treatment method according to claim 13, wherein the feed volume space velocity of the hydrogen peroxide oxidized tail gas introduced into the adsorption resin column is 5m3/h～10m3/h。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202700289U (en) * | 2012-01-19 | 2013-01-30 | 江苏理文化工有限公司 | Device for processing hydrogen peroxide oxidation tail gas |
| CN205613244U (en) * | 2016-05-05 | 2016-10-05 | 江苏建康职业学院 | Chemical production tail gas recovery processing device |
| CN106669376A (en) * | 2015-11-09 | 2017-05-17 | 中国石油化工股份有限公司 | Method for using butane oxidation tail gas |
| CN106674003A (en) * | 2015-11-09 | 2017-05-17 | 中国石油化工股份有限公司 | Method for preparing cyclopentanol by hydrating cyclopentene |
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| US7416581B2 (en) * | 2004-09-03 | 2008-08-26 | Point Source Solutions, Inc. | Air-permeable filtration media, methods of manufacture and methods of use |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202700289U (en) * | 2012-01-19 | 2013-01-30 | 江苏理文化工有限公司 | Device for processing hydrogen peroxide oxidation tail gas |
| CN106669376A (en) * | 2015-11-09 | 2017-05-17 | 中国石油化工股份有限公司 | Method for using butane oxidation tail gas |
| CN106674003A (en) * | 2015-11-09 | 2017-05-17 | 中国石油化工股份有限公司 | Method for preparing cyclopentanol by hydrating cyclopentene |
| CN205613244U (en) * | 2016-05-05 | 2016-10-05 | 江苏建康职业学院 | Chemical production tail gas recovery processing device |
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