CN111773749A - Vacuum concentration system for dilute sulfuric acid - Google Patents

Vacuum concentration system for dilute sulfuric acid Download PDF

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Publication number
CN111773749A
CN111773749A CN202010669857.8A CN202010669857A CN111773749A CN 111773749 A CN111773749 A CN 111773749A CN 202010669857 A CN202010669857 A CN 202010669857A CN 111773749 A CN111773749 A CN 111773749A
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sulfuric acid
washing tower
tower
dilute sulfuric
phase
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CN111773749B (en
Inventor
罗芳
王炳强
王永康
王守满
王蒙
吴丹丹
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Qingdao Haiwan Group Co ltd
Qingdao Haiwan Specialty Chemicals Co ltd
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Qingdao Haiwan Group Co ltd
Qingdao Haiwan Specialty Chemicals Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/30Accessories for evaporators ; Constructional details thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/69Sulfur trioxide; Sulfuric acid
    • C01B17/88Concentration of sulfuric acid
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/69Sulfur trioxide; Sulfuric acid
    • C01B17/90Separation; Purification
    • C01B17/905Removal of organic impurities
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treating Waste Gases (AREA)

Abstract

The invention discloses a dilute sulfuric acid vacuum concentration system, which comprises a concentration kettle, a washing tower and a spray tower, wherein the washing tower and the spray tower are sequentially connected with a gas phase outlet of the concentration kettle; the washing tower is provided with a first circulating pipeline to realize the circulating spraying of the liquid-phase dilute sulfuric acid in the washing tower; the spray tower is provided with a second circulating pipeline to realize condensation of the gas phase introduced into the spray tower from the washing tower; the second circulating pipeline is connected with the first circulating pipeline and used as water replenishing of the first circulating pipeline to keep the content of dilute sulfuric acid in the circulating liquid constant. In the vacuum concentration system provided by the invention, the operation temperature of the washing tower is higher than the melting point of the organic matters contained in the waste acid, so that the materials in the washing tower only exist in a gas phase and a liquid phase, and the condition that the washing tower and a process pipeline are blocked after the organic matters with high freezing points are condensed into solid due to entrainment of mist is avoided.

Description

Vacuum concentration system for dilute sulfuric acid
Technical Field
The invention belongs to the technical field of dilute sulfuric acid vacuum concentration, and particularly relates to a dilute sulfuric acid vacuum concentration system.
Background
In the chemical industry, sulfuric acid is generally used as a reaction raw material or medium, but more industrial waste acid is generally generated after the reaction, and the environmental burden is greatly increased. Therefore, various methods for recovering industrial waste acid have been developed in the prior art, wherein the "vacuum concentration method" is a mature, safe, reliable, energy-saving, environment-friendly and most widely used method in the dilute sulfuric acid recovery technology, but for dilute sulfuric acid containing soluble and high-freezing-point organic matters, organic matters are often condensed in the process of concentrating gas phase condensation, so that blockage of a washing tower, a condenser and related pipelines is caused, and thus, the industrial problem is still existed.
At present, although some anti-blocking methods such as a pre-adsorption method are proposed successively, the method reduces the content of organic matters in dilute sulfuric acid, but the method has incomplete removal of the organic matters, can only slightly improve the concentration process, does not fundamentally eliminate the blocking phenomenon, and adopts ion resin adsorption in some schemes, thereby increasing the treatment cost; the other method is a pre-concentration method, belongs to the field of pretreatment, and can only treat dilute sulfuric acid containing low-boiling-point organic matters, and cannot effectively treat mixed waste acid containing higher boiling points or wider boiling ranges.
The chinese patent with application number 200810025334.9 discloses a dilute sulfuric acid vacuum process containing high freezing point organic matter, adding organic reaction raw materials into the spray liquid of a washing tower to reduce the freezing point of the mixture of dilute sulfuric acid and organic matter, but the raw materials of the method are mostly dangerous chemicals of class a and class b, the requirement for safety is higher, the plant design level needs to be increased, the process cost is improved, and the applicability to the organic matter with the freezing point more than 80 ℃ is poor.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide a dilute sulfuric acid vacuum concentration system, wherein the operation temperature of a washing tower is higher than the melting point of organic matters dissolved in waste acid, so that the materials in the washing tower only exist in a gas phase and a liquid phase in the gas phase condensation process, and the phenomenon that the organic matters with high freezing points block a process pipeline is avoided.
In order to solve the technical problems, the invention adopts the technical scheme that:
the invention provides a dilute sulfuric acid vacuum concentration system, which comprises a concentration kettle, a washing tower and a spray tower, wherein the washing tower and the spray tower are sequentially connected with a gas phase outlet of the concentration kettle; the washing tower is provided with a first circulating pipeline to realize the circulating spraying of the liquid-phase dilute sulfuric acid in the washing tower; the spray tower is provided with a second circulating pipeline to realize condensation of the gas phase introduced into the spray tower from the washing tower; the second circulating pipeline is connected with the first circulating pipeline and used as water replenishing of the first circulating pipeline to keep the content of dilute sulfuric acid in the circulating liquid constant.
In the scheme, the vacuum concentration system provided by the invention adopts a double-tower structure with a washing tower and a spray tower separated from each other, and aims to ensure that organic matters in sulfuric acid steam generated by concentration do not have a solid phase state in the washing tower by increasing the temperature of the washing tower, so that the solid phase organic matters are prevented from blocking related pipelines of the washing tower. Meanwhile, the spray tower can further absorb the gas phase overflowing from the washing tower, and the solid-phase substance in the solid-liquid mixed phase is timely treated by the phase splitting device arranged at the bottom of the spray tower, so that the blockage phenomenon of a process pipeline related to spraying is avoided. Under the premise, the first circulation pipeline and the second circulation pipeline can increase the circulating absorption efficiency of the sulfuric acid steam so as to achieve the optimal vacuum concentration effect and pipeline blockage prevention effect.
The further scheme of the invention is as follows: the system is connected with a vacuum unit to enable the concentration kettle, the washing tower and the spray tower to be in a vacuum state, and the pressure of the vacuum system is 12 kPa.
In the scheme, the pressure of the vacuum system with constant absolute pressure is applied to partial components in the system, so that the control of the temperature in the components is realized by adjusting the material composition in the components, and the system is stable and efficient to operate. The components in the system in a vacuum state are not limited to the concentration tank, the washing tower and the spray tower.
The further scheme of the invention is as follows: and continuously heating the raw material dilute sulfuric acid by steam in the concentration kettle to obtain high-concentration finished acid, and simultaneously sending the generated sulfuric acid steam to a washing tower through a gas phase outlet of the concentration kettle.
In the scheme, considering that the freezing point of organic matters contained in the raw material dilute sulfuric acid is possibly higher, the temperature for heating the steam is set to be 182 ℃, and the solid-phase precipitation of the organic matters is avoided. Further, the concentration of the high concentration product acid is about 88%.
The further scheme of the invention is as follows: the system ensures that the operation temperature of the washing tower is constant and is higher than the melting point of organic matters contained in the sulfuric acid steam by controlling the concentration of dilute sulfuric acid in the washing tower and the pressure of a vacuum system, so that the sulfuric acid steam sent into the washing tower is in a gas-liquid two-phase state.
In the scheme, under the condition that the vacuum degree of a system in the washing tower is constant, the operation temperature in the washing tower can be regulated and controlled by changing the composition of the liquid-phase dilute sulfuric acid, when the concentration of the dilute sulfuric acid is within a certain range, the operation temperature is constant and is higher than the melting point of organic matters contained in the sulfuric acid vapor, so that the sulfuric acid vapor in the washing tower does not have a solid phase state after phase separation. To illustrate the above more clearly, here are exemplified: when the melting point of organic matters contained in the sulfuric acid steam is 70-100 ℃, the vacuum pressure of the system is 12kPa, the circulating amount of the first circulating pipeline is adjusted, so that the concentration of the dilute sulfuric acid is maintained at 70-80%, the temperature in the washing tower is maintained within the range of 105-110 ℃, the organic matters are liquefied, and the sulfuric acid steam is in a gas-liquid two-phase state.
The further scheme of the invention is as follows: and the liquid-phase material obtained after the sulfuric acid steam is separated by the washing tower is sent to the top of the washing tower from the bottom of the washing tower through the first circulating pipeline to realize circulating spraying so as to maintain the concentration range of the liquid-phase dilute sulfuric acid in the washing tower.
The further scheme of the invention is as follows: and the gas-phase material separated by the sulfuric acid steam through the washing tower overflows to the spray tower from the top of the washing tower, and organic matters contained in the gas-phase material are absorbed and condensed by the spray liquid.
In the scheme, the spraying amount of the spraying tower can be calculated by the temperature and the concentration evaporation amount. For example, the heat load when water vapor is condensed to 40 ℃ under the condition of the vacuum system pressure of 12kPa is calculated, and then the circulating spray amount of the spray tower is further calculated according to the calculated heat load.
The further scheme of the invention is as follows: the bottom of the spray tower is provided with a phase splitting tank and a waste water tank which are connected in sequence, the spray liquid absorbs condensed solid-liquid phase flowing out from the bottom of the spray tower to the phase splitting tank for phase splitting, wherein the liquid phase overflows to the waste water tank, and is sent back to the washing tower and/or the spray tower for cyclic spraying through a second circulating pipeline as water supplement after being cooled by the first condenser.
In the scheme, the phase separation tank is used for separating substances in a solid-liquid mixed phase, and the solid-phase substances are deposited at the bottom of the tank and are periodically removed. And the liquid phase overflows from the top of the phase separation tank to a wastewater tank, and is condensed and cooled to be used as spray liquid to be sent back to the washing tower and/or the spray tower.
The further scheme of the invention is as follows: the top of the spray tower is also provided with a non-condensable gas outlet, and the non-condensable gas outlet is sequentially connected with a second condenser and a vacuum buffer steam drum so as to discharge non-condensable waste gas out of a boundary region.
In the above scheme, the non-condensable gas refers to a gas which cannot be liquefied through condensation under the current working condition. When non-condensable gas exists in a process system, the tower pressure is increased, the energy consumption is increased, and the like, so that a certain discharge mode needs to be designed.
The further scheme of the invention is as follows: the non-condensable gas generated by the spray tower is sucked into a second condenser by vacuum to be continuously cooled, and the temperature of a non-condensable gas outlet of the second condenser is less than 40 ℃.
In the above scheme, the discharged noncondensable gas easily takes away the liquefied gas, so that certain temperature and vacuum degree setting are adopted to avoid the occurrence of the condition.
The further scheme of the invention is as follows: and a water outlet is also arranged between the waste water tank and the first condenser so as to discharge redundant water out of the boundary area.
Among the above-mentioned scheme, because all there is 12kPa vacuum system pressure in a plurality of parts in the system for the water boiling point in the scrubbing tower descends, exists with the vapor form under the higher operating temperature of scrubbing tower, and this can make the spray column produce a large amount of condensate water, thereby leads to the water in the second circulation pipeline constantly to increase, consequently needs the liquid level interlock through the waste water jar to control the outlet of district, and unnecessary water is drained to the intermittent type.
The further scheme of the invention is as follows: and the high-concentration finished acid is pumped out of a boundary area by a pump after being subjected to three-stage condensation to 40 ℃.
The further scheme of the invention is as follows: the connection part of the second circulation pipeline and the first circulation pipeline is provided with an adjusting valve, the system can adjust the conduction direction or the opening degree of the adjusting valve according to the temperature and the concentration evaporation capacity of the washing tower, water in the second circulation pipeline is sent into the first circulation pipeline, or the connection between the second circulation pipeline and the first circulation pipeline is closed, so that the condensed water in the waste water tank is only used as spray liquid of the spray tower. The second circulation pipeline is communicated with the first circulation pipeline in a one-way mode through the regulating valve.
After adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the washing tower of the vacuum concentration system provided by the invention is provided with the temperature control device, the operating temperature of the washing tower is higher than the melting point of organic matters contained in sulfuric acid steam, so that the materials in the washing tower only exist in a gas phase and a liquid phase, and the condition that the organic matters with high freezing points block a process pipeline is avoided;
2. the spray tower of the vacuum concentration system provided by the invention can further absorb the gas phase overflowing from the washing tower, and the solid-phase substance in the solid-liquid mixed phase is timely treated by the phase splitting device arranged at the bottom of the spray tower, so that the blockage phenomenon of a process pipeline related to spraying is avoided;
3. the vacuum concentration system provided by the invention is provided with the first circulation pipeline aiming at the washing tower and the second circulation pipeline for respectively returning materials to the washing tower and the spray tower, so that the circulating absorption efficiency of sulfuric acid steam can be increased, and the optimal vacuum concentration effect can be achieved.
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention, are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without limiting the invention to the right. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a schematic process flow diagram of a dilute sulfuric acid vacuum concentration system provided by the present invention;
FIG. 2 is a schematic process flow diagram of a dilute sulfuric acid vacuum concentration system provided in example 3 of the present invention.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
As shown in fig. 1, the present invention provides a dilute sulfuric acid vacuum concentration system, wherein the operation temperature of the scrubber is higher than the melting point of the organic matters contained in the waste acid, so as to ensure that the materials in the scrubber exist only in gas phase and liquid phase, thereby avoiding the situation that the organic matters with high freezing point block the process pipeline.
Example 1
In the embodiment, a dilute sulfuric acid vacuum concentration system is provided, which comprises a concentration kettle, and a washing tower and a spray tower which are sequentially connected with a gas phase outlet of the concentration kettle; the washing tower is provided with a first circulating pipeline to realize the circulating spraying of the liquid-phase dilute sulfuric acid in the washing tower; the spray tower is provided with a second circulating pipeline to realize condensation of the gas phase introduced into the spray tower from the washing tower; the second circulating pipeline is connected with the first circulating pipeline and used as water replenishing of the first circulating pipeline to keep the content of dilute sulfuric acid in the circulating liquid constant.
In this embodiment, the vacuum concentration system provided by the invention adopts a double-tower structure in which the washing tower and the spray tower are separated, and aims to prevent organic matters in the sulfuric acid steam generated by concentration from generating a solid phase state in the washing tower by increasing the temperature of the washing tower, thereby preventing the solid phase organic matters from blocking related pipelines of the washing tower. Meanwhile, the spray tower can further absorb the gas phase overflowing from the washing tower, and the solid-phase substance in the solid-liquid mixed phase is timely treated by the phase splitting device arranged at the bottom of the spray tower, so that the blockage phenomenon of a process pipeline related to spraying is avoided. Under the premise, the first circulation pipeline and the second circulation pipeline can increase the circulating absorption efficiency of the sulfuric acid steam so as to achieve the optimal vacuum concentration effect and pipeline blockage prevention effect.
In this embodiment, the system is connected to a vacuum unit, so that a vacuum state is formed in the concentration kettle, the washing tower and the spray tower, and the system pressure of the vacuum state is 12kPa absolute.
In this embodiment, the vacuum system pressure of invariable absolute pressure is exerted to some subassemblies in the system, is convenient for constitute through the material in the adjustment subassembly and realizes the control to the temperature in the subassembly, makes the operation of system stable high-efficient. The components in the system in a vacuum state are not limited to the concentration tank, the washing tower and the spray tower.
In this embodiment, the raw dilute sulfuric acid is continuously heated by the steam in the concentration kettle to obtain a high-concentration finished acid, and the generated sulfuric acid steam is sent to the washing tower through the gas phase outlet of the concentration kettle.
In this example, considering that the freezing point of the organic matter contained in the raw material dilute sulfuric acid may be high, the temperature for intermittent steam heating is set to 182 ℃, and the solid phase precipitation of the organic matter is avoided. Further, the concentration of the high concentration product acid is about 88%.
In this embodiment, the system controls the dilute sulfuric acid concentration in the scrubber and the vacuum system pressure to keep the operating temperature of the scrubber constant and higher than the melting point of the organic compounds in the sulfuric acid vapor, so that the sulfuric acid vapor fed into the scrubber is in a gas-liquid two-phase state.
In this embodiment, under the condition that the vacuum degree of the system in the scrubber is constant, the control of the operating temperature in the scrubber can be realized by changing the concentration of the liquid-phase dilute sulfuric acid, and when the concentration of the dilute sulfuric acid is within a certain range, the operating temperature is constant and is higher than the melting point of organic matters contained in the sulfuric acid vapor, so that the sulfuric acid vapor in the scrubber does not have a solid-phase state after phase separation. To illustrate the above more clearly, here are exemplified: when the melting point of organic matters contained in the sulfuric acid steam is 70-100 ℃, the vacuum pressure of the system is 12kPa, the circulating amount of the first circulating pipeline is adjusted, so that the concentration of the dilute sulfuric acid is maintained at 70-80%, the temperature in the washing tower is maintained within the range of 105-110 ℃, the organic matters are liquefied, and the sulfuric acid steam is in a gas-liquid two-phase state.
In this embodiment, the liquid-phase material obtained by separating the sulfuric acid vapor by the washing tower is sent from the bottom of the washing tower to the top of the washing tower through the first circulation pipeline to realize circulation spraying, so as to maintain the concentration range of the liquid-phase dilute sulfuric acid in the washing tower.
In this embodiment, the gas-phase material obtained by separating the sulfuric acid vapor by the washing tower overflows to the spraying tower from the top of the washing tower, and organic matters contained in the gas-phase material are absorbed and condensed by the spraying liquid.
In this embodiment, the spraying amount of the spraying tower can be calculated from the temperature and the concentration evaporation amount. For example, the heat load when water vapor is condensed to 40 ℃ under the condition of the vacuum system pressure of 12kPa is calculated, and then the circulating spray amount of the spray tower is further calculated according to the calculated heat load.
In this embodiment, the bottom of the spray tower is equipped with consecutive phase splitting jar and waste water tank, quilt spray the solid-liquid phase that the liquid absorption condenses and flow out to phase splitting jar from the bottom of the spray tower and carry out the phase splitting, and wherein the liquid phase spills over to the waste water tank, after the cooling through first condenser, and the realization that circulates and sprays is sent back to scrubbing tower and/or spray column as the moisturizing through second circulation pipeline.
In this embodiment, the phase separation tank separates the solid-liquid mixed phase substance, deposits the solid-phase substance on the tank bottom, and periodically removes the solid-phase substance. And the liquid phase overflows from the top of the phase separation tank to a wastewater tank, and is condensed and cooled to be used as spray liquid to be sent back to the washing tower and/or the spray tower.
In this embodiment, the spray column top still is equipped with noncondensable gas export, noncondensable gas export links to each other with second condenser and vacuum buffer steam pocket in proper order to will not congeal waste gas discharge boundary region.
In this embodiment, the non-condensable gas is a gas that cannot be liquefied by condensation under the current working condition. When non-condensable gas exists in a process system, the tower pressure is increased, the energy consumption is increased, and the like, so that a certain discharge mode needs to be designed.
In this embodiment, the non-condensable gas generated by the spray tower is sucked into the second condenser by vacuum to be continuously cooled, and the temperature of the non-condensable gas outlet of the second condenser is less than 40 ℃.
In this embodiment, the discharge noncondensable gas is taken away the liquefied gas easily, consequently adopts certain temperature and vacuum degree setting to avoid this condition to take place.
In this embodiment, a water outlet is further provided between the wastewater tank and the first condenser to discharge excess water to the boundary area.
In this embodiment, because there is 12kPa of vacuum system pressure in all in a plurality of parts in the system for the boiling point of water in the scrubbing tower descends, exists with the vapor form under the higher operating temperature of scrubbing tower, and this can make the spray column produce a large amount of condensate water, thereby leads to the water in the second circulation pipeline to constantly increase, consequently needs the liquid level interlock control of waste water jar to go out the outlet in district, and unnecessary water is discharged to the interval.
The following contents specifically illustrate the process of dilute sulfuric acid vacuum concentration provided by the present invention:
the raw material dilute sulfuric acid is sucked into a concentration kettle through flow control, the raw material is intermittently heated to 182 ℃ by steam in the kettle and then concentrated to 88 percent, the obtained finished product sulfuric acid overflows from the outlet of the kettle, is subjected to three-stage condensation to 40 ℃, and is pumped out of a boundary area by a pump for subsequent treatment.
Meanwhile, the gas phase generated in the concentration kettle is sprayed by a circulating pump of the washing tower to form gas-liquid separation, and the content of sulfuric acid in the gas-phase sulfuric acid steam can be controlled in the process; further, gas-phase materials overflowing from the top of the washing tower enter the spray tower and are sprayed and cooled by the second circulating pipeline, organic matters with high solidifying points are condensed at the bottom of the spray tower, liquid-solid mixed phases containing the organic matters flow out of the bottom of the spray tower to the phase separation tank for phase separation, liquid phases in the phase separation tank overflow to the waste water tank and are recycled as spray liquid after being cooled, and solid phases at the bottom of the phase separation tank are periodically discharged and removed.
In addition, the spray tower is also provided with a non-condensable gas outlet, the non-condensable gas is continuously cooled by a vacuum suction condenser and then is discharged out of a boundary area through a vacuum buffer steam drum, and the vacuum is obtained by a vacuum unit.
Example 2
This embodiment is a further improvement on embodiment 1, and is different from embodiment 1 in that:
in this embodiment, an adjusting valve is disposed at a connection position of the second circulation pipeline and the first circulation pipeline, and the system can adjust the conduction direction or the opening degree of the adjusting valve according to the temperature and the concentration evaporation capacity of the washing tower, so as to send water in the second circulation pipeline into the first circulation pipeline, or close the connection between the second circulation pipeline and the first circulation pipeline, so that the condensed water in the wastewater tank is only used as the spray liquid of the spray tower. The second circulation pipeline is communicated with the first circulation pipeline in a one-way mode through the regulating valve.
Other embodiments of this example are the same as example 1.
Example 3
As shown in fig. 2, this embodiment is a further improvement on embodiment 1, and is different from embodiment 1 in that:
and a gas phase balance pipeline connected with a raw material dilute sulfuric acid feeding port of the concentration kettle is also arranged at the bottom of the washing tower, and when the concentration of the liquid-phase dilute sulfuric acid in the washing tower is increased, part of the liquid-phase sulfuric acid is discharged out of the washing tower system so as to maintain the concentration of the dilute sulfuric acid in the washing tower and the operation temperature of the washing tower. The discharged liquid phase sulfuric acid is returned to a raw material dilute sulfuric acid feeding port of the concentration kettle so as to increase the yield of finished acid.
Other embodiments of this example are the same as example 1.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. A dilute sulphuric acid vacuum concentration system is characterized by comprising a concentration kettle, a washing tower and a spray tower, wherein the washing tower and the spray tower are sequentially connected with a gas phase outlet of the concentration kettle; the washing tower is provided with a first circulating pipeline to realize the circulating spraying of the liquid-phase dilute sulfuric acid in the washing tower; the spray tower is provided with a second circulating pipeline to realize condensation of the gas phase introduced into the spray tower from the washing tower; the second circulating pipeline is connected with the first circulating pipeline and used as water replenishing of the first circulating pipeline to keep the content of dilute sulfuric acid in the circulating liquid constant.
2. The dilute sulfuric acid vacuum concentration system according to claim 1, wherein a vacuum unit is connected to the system, so that a vacuum state is formed in the concentration kettle, the washing tower and the spray tower, and the pressure of the vacuum system is 12 kPa.
3. The dilute sulfuric acid vacuum concentration system according to claim 2, wherein raw dilute sulfuric acid is continuously heated by steam in the concentration kettle to obtain high-concentration finished acid, and simultaneously, generated sulfuric acid steam is sent to the washing tower through a gas phase outlet of the concentration kettle; and the high-concentration finished acid is pumped out of a boundary area by a pump after being subjected to three-stage condensation to 40 ℃.
4. The dilute sulfuric acid vacuum concentration system as claimed in claim 2, wherein the system controls the dilute sulfuric acid concentration in the washing tower and the vacuum system pressure to make the operation temperature of the washing tower constant and higher than the melting point of the organic matters contained in the sulfuric acid vapor carried by entrainment of mist, so that the sulfuric acid vapor fed into the washing tower is in a gas-liquid two-phase state.
5. The dilute sulfuric acid vacuum concentration system according to claim 4, wherein the liquid phase material obtained after the sulfuric acid vapor is separated by the washing tower is sent from the bottom of the washing tower to the top of the washing tower through the first circulating pipeline to realize circulating spraying so as to maintain the concentration range of the liquid phase dilute sulfuric acid in the washing tower.
6. The dilute sulfuric acid vacuum concentration system according to claim 4, wherein the gas phase material after the sulfuric acid vapor is separated by the washing tower overflows to the spray tower from the top of the washing tower, and organic matters contained in the gas phase material are quenched and condensed by the spray liquid.
7. The dilute sulfuric acid vacuum concentration system according to claim 6, wherein a phase separation tank and a waste water tank are arranged at the bottom of the spray tower and are connected in sequence, the solid-liquid phase absorbed and condensed by the spray liquid flows out from the bottom of the spray tower to the phase separation tank for phase separation, the liquid phase overflows to the waste water tank, and after the temperature is reduced by the first condenser, the liquid phase is returned to the washing tower and/or the spray tower as the water supplement through the second circulation pipeline to realize the circulating spray.
8. The dilute sulfuric acid vacuum concentration system according to claim 1, wherein the top of the spray tower is further provided with a non-condensable gas outlet, and the non-condensable gas outlet is sequentially connected with the second condenser and the vacuum buffer steam drum so as to discharge non-condensable waste gas out of the battery limits.
9. The dilute sulfuric acid vacuum concentration system according to claim 8, wherein the non-condensable gas generated by the spray tower is sucked into the second condenser by vacuum to be continuously cooled, and the non-condensable gas outlet temperature of the second condenser is less than 40 ℃.
10. The dilute sulfuric acid vacuum concentration system of claim 7, wherein a drain port is further provided between the wastewater tank and the first condenser to drain excess water out of the battery limits.
CN202010669857.8A 2020-07-13 2020-07-13 Vacuum concentration system for dilute sulfuric acid Active CN111773749B (en)

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