CN111437691A - Organic waste gas treatment method for producing hydrogen peroxide by anthraquinone process - Google Patents
Organic waste gas treatment method for producing hydrogen peroxide by anthraquinone process Download PDFInfo
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- 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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- 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
- B01D53/04—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 with stationary adsorbents
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Abstract
The invention belongs to the technical field of chemical production, and particularly relates to an organic waste gas treatment method for producing hydrogen peroxide by an anthraquinone process, which comprises the steps of enabling organic waste gas controlled by the pressure of an emptying system to pass through a primary cooler and a primary separator, and cooling to 28-32 ℃ by using circulating water; then continuously passing through a secondary cooler and a secondary separator, and cooling to 3-7 ℃; then introducing the mixture into an activated carbon adsorption system for further treatment, and recycling the separated organic solvent; the invention reduces the temperature of the discharged organic waste gas from 50 ℃ to about 5 ℃, and can reduce the content of heavy aromatic hydrocarbon to 12 percent (the content is about 1700 mg/m)3) (ii) a Then the organic waste gas is reduced to 120mg/m by a two-stage or multi-stage active carbon adsorption system3Realizing the standard discharge of VOCs; in addition, the treatment method can recover a large amount of aromatic hydrocarbon and reduce the production cost.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a method for treating organic waste gas generated in hydrogen peroxide production by an anthraquinone process.
Background
With the progress of science and technology, the quality of life of people is improved, and the requirement on environmental protection is higher and higher. The environmental pollution is mainly caused by three wastes formed in the industrial production process and the life of people; particularly, petrochemical enterprises can emit a large amount of waste gas in the production process, wherein the emission of volatile organic waste gas is regarded as the second main type of atmospheric pollutants, and is second only to atmospheric particulate matters. With the emphasis of the country on environmental protection and the increase of the environmental protection treatment, the organic waste gas generated in the production process must be treated by enterprises and discharged after reaching the standard, but the organic waste gas is generally directly discharged into the atmosphere after being simply treated by the traditional chemical enterprises in the production process, and the VOCs (volatile organic compounds) can not reach 120mg/m or less3The emission standard of (2) causes serious atmospheric pollution.
In the prior art, the anthraquinone method is the most important method for producing hydrogen peroxide, and the process comprises the steps of preparing a working solution from alkyl anthraquinone and an organic solvent, introducing hydrogen for hydrogenation under the conditions that the pressure is 0.30MPa, the temperature is 55-65 ℃ and a catalyst exists, performing countercurrent oxidation with air (or oxygen) at 40-44 ℃, and preparing a hydrogen peroxide aqueous solution product with the mass fraction of 20-30% through extraction, regeneration, refining and concentration. In the process of producing hydrogen peroxide by the anthraquinone method, if organic waste gas cannot be reasonably treated, the atmosphere can be polluted.
For example, chinese patent publication No. CN108057309A essentially discloses a recycling apparatus for organic waste gas, which is characterized in that: the organic waste gas is pretreated firstly and is subjected to two-stage treatment by an activated carbon fiber box, so that the recovery amount of organic solvents in the organic waste gas is improved, but the up-to-standard discharge of VOCs in the organic waste gas is not realized; meanwhile, the device only has four processes of adsorption, desorption, cooling and drying, and particularly can blow out part of organic solvent steam remained in the activated carbon after steam desorption from the air when a fan is dried and exhausted, so that emission detection data is influenced, and meanwhile, the field has smell.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the organic waste gas treatment method for producing the hydrogen peroxide by the anthraquinone method, which treats organized and unorganized organic waste gas in the hydrogen peroxide production process by the anthraquinone method, realizes standard emission of VOCs and reduces environmental pollution.
In order to achieve the purpose, the invention adopts the following technical scheme:
an organic waste gas treatment method for producing hydrogen peroxide by an anthraquinone process comprises the steps of enabling organic waste gas controlled by pressure of an emptying system to pass through a primary cooler and a primary separator, and cooling to 28-32 ℃ by using circulating water;
then continuously passing through a secondary cooler and a secondary separator, and cooling to 3-7 ℃;
then the organic solvent is introduced into an activated carbon adsorption system for further treatment, and the separated organic solvent is recycled.
In a further technical scheme, the method for treating the organic waste gas further comprises the following steps: the unorganized emptying gas of each storage tank in the system for producing hydrogen peroxide by the anthraquinone method passes through a pipeline, is cooled, condensed and separated by a cooler and a separating tank, and is pumped into the activated carbon adsorption system by a vortex gas pump for treatment.
In a further technical scheme, the activated carbon adsorption system comprises at least three activated carbon adsorption tanks, and a cooler, a separation tank, a metering tank, a fan, a vortex air pump, a control valve and a DCS control system which are matched with the activated carbon adsorption tanks;
every two activated carbon adsorption tanks are connected through a valve and a pipeline to form a primary and secondary adsorption process, organic solvent in the organic waste gas is discharged after being adsorbed by the activated carbon adsorption tanks, the activated carbon adsorption tanks adsorbing the organic solvent are subjected to steam desorption, condenser condensation and separation tank separation to obtain the organic solvent for recovery, and the desorbed water is led to a sewage station for treatment.
In a further technical scheme, after the activated carbon adsorption tank undergoes steam desorption, the activated carbon adsorption tank is firstly vacuumized by a vortex air pump through a cooler, part of organic solvent steam is cooled and recovered, internal circulation drying is carried out on the activated carbon adsorption tank through a fan through the cooler, and then air is sent into the activated carbon adsorption tank through the fan to cool and dry the activated carbon adsorption tank.
Compared with the prior art, the invention has the following technical effects:
the organic waste gas treatment method for producing hydrogen peroxide by anthraquinone process provided by the invention reduces the temperature of the emptied organic waste gas from 50 ℃ to about 5 ℃, and can reduce the content of heavy aromatic hydrocarbon to 12% (the content is about 1700 mg/m)3) (ii) a Then the organic waste gas is reduced to 120mg/m by a two-stage or multi-stage active carbon adsorption system3Realizing the standard discharge of VOCs; in addition, the treatment method can recover a large amount of aromatic hydrocarbon and reduce the production cost.
Drawings
FIG. 1 is a flow chart of the organic waste gas treatment method for producing hydrogen peroxide by an anthraquinone process;
FIG. 2 is a schematic view of an activated carbon adsorption system provided by the present invention;
FIG. 3 is a flow chart of the adsorption and steam desorption condensation process of the activated carbon adsorption tank of the present invention;
FIG. 4 is a flow chart of the vacuum-pumping and fan-drying process of the activated carbon adsorption tank of the present invention;
the reference numbers in the figures illustrate: 1-a first activated carbon adsorption tank, 2-a second activated carbon adsorption tank, 3-a third activated carbon adsorption tank, 4-a cooler, 5-a blower, 6-a vortex air pump, 7-a separation tank, 8-a metering tank, 11-a first air release valve, 21-a second air release valve, 31-a third air release valve, 12-a first joint inlet valve, 22-a second joint inlet valve, 32-a third joint inlet valve, 13-a first steam outlet valve, 23-a second steam outlet valve, 33-a third steam outlet valve, 14-a first joint outlet valve, 24-a second joint outlet valve, 34-a third joint outlet valve, 15-a first outlet valve, 25-a second outlet valve, 35-a third outlet valve, 16-a first drying valve, 26-a second drying valve, 36-a third drying valve, 17-a first steam inlet valve, 27-a second steam inlet valve, 37-a third steam inlet valve, 41-a tail gas main valve, 42-an emptying valve, 43-a condensing valve, 44-an internal drying valve, 45-an external drying valve, 46-a liquid discharge valve, 47-a vacuum valve and 48-an exhaust valve.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified by combining the specific drawings.
As shown in figure 1, the invention provides an organic waste gas treatment method for producing hydrogen peroxide by an anthraquinone process, which comprises the steps of enabling organic waste gas controlled by the pressure of an emptying system to pass through a primary cooler and a primary separator, and cooling to 28-32 ℃ by using circulating water; then continuously passing through a secondary cooler and a secondary separator, and cooling to 3-7 ℃; then introducing the mixture into an activated carbon adsorption system for further treatment; and recycling the separated organic solvent.
Specifically, for example, the oxidation tail gas at about 50 ℃ in the system for producing hydrogen peroxide by the anthraquinone method passes through a primary cooler by system pressure, is cooled to about 30 ℃ by circulating water, and part of organic solvent in the oxidation tail gas is cooled, condensed and separated by a primary separator; then, the oxidized tail gas at about 30 ℃ continuously passes through a secondary cooler, the temperature is reduced to about 5 ℃ by low-temperature water or an expansion refrigerating unit, and then the organic solvent in the oxidized tail gas is further cooled, condensed and separated out through a secondary separator; introducing the treated oxidation tail gas into an active carbon adsorption system for further treatment; by the treatment method, the organic solvent of the oxidation tail gas is fully separated, and the requirement of standard emission is met; and the separated organic solvent can be recycled.
In the invention, in order to improve the separation effect on the organic solvent, internals such as a diaphragm separator, a stainless steel wire mesh demister and the like are arranged in the primary cooler; and the secondary cooler is internally provided with internals such as a stainless steel wire mesh demister, a high-efficiency separation filter element and the like.
In the technical scheme provided by the invention, aiming at the characteristic that the organic waste gas in the hydrogen peroxide produced by the anthraquinone method is heavy aromatic hydrocarbon (the main component is C9 trimethylbenzene), the content of the heavy aromatic hydrocarbon can be reduced to 12 percent (the content is about 1700 mg/m) by reducing the vented organic waste gas from 50 ℃ to about 5 ℃ by a fractional condensation separation method according to the relation curve of the content of the aromatic hydrocarbon and the temperature3) (ii) a Then the organic waste gas is reduced to 120mg/m by a two-stage or multi-stage active carbon adsorption system3In the following, the following description is given,the discharge of VOCs reaching the standard is realized; in addition, by the treatment method, a large amount of aromatic hydrocarbon can be recovered, and the production cost is reduced; on the other hand, the method provided by the invention can realize automation and has the advantages of simple operation, low operation cost, high purification efficiency, safety and economy.
The treatment method provided by the invention also comprises the step of enabling unorganized vent gas of each storage tank in the system for producing hydrogen peroxide by the anthraquinone method to pass through a pipeline, cooling, condensing and separating the vent gas by a cooler and a separating tank, and then pumping the vent gas into the activated carbon adsorption system for treatment by a vortex gas pump. That is, the treatment method provided by the invention can be compatible with the treatment of the unorganized air of each storage tank, and realizes the synchronous treatment of the unorganized air of the organized storage tank and each storage tank.
FIG. 2 is a schematic view of an activated carbon adsorption system according to the present invention; the active carbon adsorption system comprises three active carbon adsorption tanks, and a cooler 4, a separation tank 7, a metering tank 8, a fan 5, a vortex air pump 6, a control valve and a DCS control system which are matched with the active carbon adsorption tanks; the three activated carbon adsorption tanks are respectively a first activated carbon adsorption tank 1, a second activated carbon adsorption tank 2 and a third activated carbon adsorption tank 3;
a tail gas main valve 41 is arranged on an input pipe of the activated carbon adsorption system, the other end of the tail gas main valve 41 is connected to the air inlet end at the bottom of the first activated carbon adsorption tank 1 through a first air release valve 11, is connected to the air inlet end at the bottom of the second activated carbon adsorption tank 2 through a second air release valve 21, and is connected to the air inlet end at the bottom of the third activated carbon adsorption tank 3 through a third air release valve 31;
the outlet duct of the first activated carbon adsorption tank 1 is divided into three paths: one path is discharged through a first discharge valve 14 and then communicated to the air inlet end at the bottom of the first activated carbon adsorption tank 1 through a first inlet valve 12, communicated to the air inlet end at the bottom of the second activated carbon adsorption tank 2 through a second inlet valve 22, and communicated to the air inlet end at the bottom of the third activated carbon adsorption tank 3 through a third inlet valve 32; one path is discharged through a first air outlet valve 15; one path is connected to the cooler 4 through the first drying valve 16, and is connected to the input pipe of the activated carbon adsorption system through the vacuum valve 47 and the vortex air pump 6;
the outlet duct of the second activated carbon adsorption tank 2 is divided into three paths: one path is discharged through a second coupling outlet valve 24 and then communicated to the air inlet end at the bottom of the first activated carbon adsorption tank 1 through a first coupling inlet valve 12, communicated to the air inlet end at the bottom of the second activated carbon adsorption tank 2 through a second coupling inlet valve 22 and communicated to the air inlet end at the bottom of the third activated carbon adsorption tank 3 through a third coupling inlet valve 32; one path is discharged through a second air outlet valve 25; one path is connected to the cooler 4 through the second drying valve 26, and is connected to the input pipe of the activated carbon adsorption system through the vacuum valve 47 and the vortex air pump 6;
the outlet duct of the third activated carbon adsorption tank 3 is divided into three paths: one path is discharged through a third discharge valve 34 and then communicated to the air inlet end at the bottom of the first activated carbon adsorption tank 1 through a first inlet valve 12, communicated to the air inlet end at the bottom of the second activated carbon adsorption tank 2 through a second inlet valve 22 and communicated to the air inlet end at the bottom of the third activated carbon adsorption tank 3 through a third inlet valve 32; one path is discharged through a third air outlet valve 35; one path is connected to the cooler 4 through a third drying valve 36, and is connected to an input pipe of the activated carbon adsorption system through a vacuum valve 47 and a vortex air pump 6;
the air outlet end of the cooler 4 is divided into two paths: one path is discharged through a condensing valve 43, and is communicated to the air inlet end at the bottom of the first activated carbon adsorption tank 1 through a first steam outlet valve 13, communicated to the air inlet end at the bottom of the second activated carbon adsorption tank 2 through a second steam outlet valve 23, and communicated to the air inlet end at the bottom of the third activated carbon adsorption tank 3 through a third steam outlet valve 33;
one path is communicated to the air inlet end of the fan 5 through an external drying valve 45; the air outlet end of the fan 5 is discharged through an internal drying valve 44; then respectively communicated to the air inlet end at the bottom of the first active carbon adsorption tank 1 through a first steam outlet valve 13, communicated to the air inlet end at the bottom of the second active carbon adsorption tank 2 through a second steam outlet valve 23, and communicated to the air inlet end at the bottom of the third active carbon adsorption tank 3 through a third steam outlet valve 33;
the liquid outlet end of the cooler 4 is connected to a separation tank 7 through a liquid outlet valve 46, and the separation tank 7 is connected to a metering tank 8 through a pipeline;
the separation tank 7 and the metering tank 8 are respectively communicated to the air inlet end of the vortex air pump 6 through an exhaust valve 48 and a vacuum valve 47;
the first activated carbon adsorption tank 1 is connected with a steam pipeline with a first steam inlet valve 17, the second activated carbon adsorption tank 2 is connected with a steam pipeline with a second steam inlet valve 27, and the third activated carbon adsorption tank 3 is connected with a steam pipeline with a third steam inlet valve 37;
the input pipe of the active carbon adsorption system is also connected with a pipeline with an air release valve 42.
Specifically, in a process flow of the present invention, a series flow is formed between the first activated carbon adsorption tank 1 and the second activated carbon adsorption tank 2 through the control of a pipeline and a valve, i.e. a first-stage and second-stage adsorption system is realized, organic waste gas passes through the tail gas main valve 41, enters the first activated carbon adsorption tank 1 through the first deflation valve 11, is discharged through the first discharge valve 14, enters the second activated carbon adsorption tank 2 through the second inlet valve 22, and is then discharged through the second outlet valve 25, such that the organic solvent in the organic waste gas is subjected to activated carbon adsorption treatment and then reaches the emission standard.
Simultaneously, the third activated carbon adsorption tank 3 begins to perform steam desorption: specifically, steam enters the third activated carbon adsorption tank 3 through the third steam inlet valve 37, steam desorption analysis is carried out on activated carbon in the third activated carbon adsorption tank 3, steam after analysis is discharged through the third steam outlet valve 33, the steam is condensed in the cooler 4 through the condensing valve 43, condensed condensate enters the separation tank 7 through the liquid discharge valve 46, and separated organic solvent enters the metering tank 8 through a pipeline and is recycled through the pipeline. Meanwhile, the air discharged from the cooler 4, the separation tank 7 and the metering tank 8 passes through the vacuum valve 47 and the exhaust valve 48, and is discharged to the tail gas total treatment through the vortex air pump 6.
When the steam desorption and analysis of the third activated carbon adsorption tank 3 are finished, vacuumizing is started: a small amount of aromatic hydrocarbon and steam in the third activated carbon adsorption tank 3 pass through a third steam outlet valve 33, a condensing valve 43, a cooler 4 for condensation and a vacuum valve 47, and are discharged to the tail gas total treatment through a vortex air pump 6; the condensate is discharged into the separation tank 7 through a drain valve.
Drying in a fan in a circulating manner: air enters the third activated carbon adsorption tank 3 through the fan 5, the inner drying valve 44 and the third steam outlet valve 33 for drying, is discharged from the third drying valve 36, is condensed through the cooler 4, returns to the inlet of the fan 5 through the outer drying valve 45 for internal circulation drying, and is discharged into the separation tank 7 through the liquid discharge valve.
Drying by external circulation of a fan: air enters the third activated carbon adsorption tank 3 through the fan 5, the inner drying valve 44 and the third steam outlet valve 33 for drying and cooling, and is discharged through the third air outlet valve 35.
After the third activated carbon adsorption tank 3 is dried and cooled, the second activated carbon adsorption tank 2 and the third activated carbon adsorption tank 3 form a series flow through the control of a pipeline and a valve, namely, a one-stage two-stage adsorption system is realized, organic waste gas enters the second activated carbon adsorption tank 2 through a second air release valve 21 and is discharged through a second discharge valve 24 until a third inlet valve 32 enters the third activated carbon adsorption tank 3, and then is discharged through a third air outlet valve 35. Meanwhile, the first activated carbon adsorption tank 1 starts to be subjected to steam desorption condensation, vacuum pumping, fan internal circulation drying and fan external circulation drying; the operation is circulated in such a way.
In the invention, the organic solvent is separated from the activated carbon adsorption tank for adsorbing the organic solvent through steam desorption and desorption, condenser condensation and a separation tank for recycling, and desorption water is led to a sewage station for treatment. Fig. 3 is a flow chart showing the adsorption and steam desorption condensation process of the activated carbon adsorption tank in the activated carbon adsorption system of the present invention.
In a specific embodiment of the invention, the active carbon adsorption system is controlled by a DSC system, and is fully automatically monitored and controlled, and the DSC control system is set to be normally stopped, reset and suddenly stopped; the device is provided with a safety interlock system, an emergency emptying system and an emergency emptying system, and is capable of automatically circulating and operating, and simple and easy to operate.
Fig. 4 is a flow chart showing a process of vacuum-pumping and fan-drying in the activated carbon adsorption system according to the present invention, wherein the process specifically includes three operation procedures of vacuum-pumping, fan internal circulation drying and fan external drying; because a large amount of water and a small amount of organic solvent steam remain in the activated carbon after each steam desorption, the adsorption effect of the activated carbon is seriously influenced; in addition, the temperature of the activated carbon after steam desorption is generally above 100 ℃, and the adsorption effect of the activated carbon is also seriously influenced, therefore, in the invention, after the activated carbon adsorption tank undergoes steam desorption, the activated adsorption tank is firstly vacuumized by a vortex air pump 6 through a cooler 4, part of organic solvent steam is cooled and recovered, then internal circulation drying is carried out through the cooler 4 by a fan 5, and further a large amount of water and a small amount of organic solvent steam remained in the activated carbon are circularly cooled, condensed and recovered; then air is sent in through a fan 5 to cool and dry the activated carbon adsorption tank.
According to the invention, the internal circulation drying of the fan is carried out before the external drying of the fan, so that the problems that the emission detection data is influenced and the odor appears on site when the external drying of the fan is carried out are effectively prevented; through the final drying step outside the fan, the temperature is reduced to below 35 ℃ when organic waste gas is adsorbed in the next period, and the adsorption effect is ensured.
In the invention, after the activated carbon adsorption tanks are dried and cooled by the fan, the activated carbon adsorption tanks are connected in series with one of the activated carbon adsorption tanks for continuous cyclic use, and the other activated carbon adsorption tank is used for steam desorption, so that the non-stop operation of the activated carbon adsorption system is realized, and the treatment efficiency of the organic waste gas is improved.
The treatment method provided by the invention realizes the effective treatment of the discharged air with an organization in the system for producing hydrogen peroxide by an anthraquinone method and without an organization in each storage tank, and has the advantages of high automation degree, simple operation, low operation cost, high purification efficiency, safety and economy.
The foregoing shows and describes the general principles, essential features, and inventive features of this invention. 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 (4)
1. A treatment method of organic waste gas generated in the production of hydrogen peroxide by an anthraquinone process is characterized by comprising the steps of enabling the organic waste gas subjected to pressure control by an emptying system to pass through a primary cooler and a primary separator, and cooling to 28-32 ℃ by using circulating water;
then continuously passing through a secondary cooler and a secondary separator, and cooling to 3-7 ℃;
then the organic solvent is introduced into an activated carbon adsorption system for further treatment, and the separated organic solvent is recycled.
2. The method of claim 1, further comprising: the unorganized emptying gas of each storage tank in the system for producing hydrogen peroxide by the anthraquinone method passes through a pipeline, is cooled, condensed and separated by a cooler and a separating tank, and is pumped into the activated carbon adsorption system by a vortex gas pump for treatment.
3. The method of claim 1, wherein the activated carbon adsorption system comprises at least three activated carbon adsorption tanks and a cooler, a separation tank, a metering tank, a fan, a vortex air pump, a control valve and a DCS control system which are matched with the activated carbon adsorption tanks;
every two activated carbon adsorption tanks are connected through a valve and a pipeline to form a primary and secondary adsorption process, organic solvent in the organic waste gas is discharged after being adsorbed by the activated carbon adsorption tanks, the activated carbon adsorption tanks adsorbing the organic solvent are subjected to steam desorption, condenser condensation and separation tank separation to obtain the organic solvent for recovery, and the desorbed water is led to a sewage station for treatment.
4. The method as claimed in claim 3, wherein after the activated carbon adsorption tank undergoes steam desorption, the activated carbon adsorption tank is firstly vacuumized by a vortex air pump through a cooler to cool and recover part of the organic solvent steam, then internal circulation drying is carried out through the cooler by a fan, and then air is sent through the fan to cool and dry the activated carbon adsorption tank.
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| CN114225626A (en) * | 2021-11-26 | 2022-03-25 | 安徽金禾实业股份有限公司 | Analysis method of carbon fiber tail gas absorption unit in hydrogen peroxide production |
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