CN221440395U - Dilute nitric acid waste liquid treatment device - Google Patents
Dilute nitric acid waste liquid treatment device Download PDFInfo
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- CN221440395U CN221440395U CN202322825573.5U CN202322825573U CN221440395U CN 221440395 U CN221440395 U CN 221440395U CN 202322825573 U CN202322825573 U CN 202322825573U CN 221440395 U CN221440395 U CN 221440395U
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- nitric acid
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- condenser
- discharge port
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 89
- 239000007788 liquid Substances 0.000 title claims abstract description 49
- 239000002699 waste material Substances 0.000 title claims abstract description 26
- 230000018044 dehydration Effects 0.000 claims abstract description 43
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 43
- 239000000779 smoke Substances 0.000 claims abstract description 16
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 230000001105 regulatory effect Effects 0.000 claims description 26
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000003517 fume Substances 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 abstract 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000002912 waste gas Substances 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluic acid Chemical compound CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012840 feeding operation Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Treating Waste Gases (AREA)
Abstract
The utility model provides a dilute nitric acid waste liquid treatment device, which comprises a reboiler, a dehydration tower, a tower top condenser, a condensate intermediate tank, an evaporator, a nitric acid condenser, a nitric acid recovery tank and a nitric acid smoke treatment device; the discharge port at the upper part of the reboiler is connected with the feed port at the lower part of the dehydration tower, and the feed port at the bottom is connected with the discharge port at the bottom of the dehydration tower; the discharge port at the top of the dehydration tower is connected with the feed port of the tower top condenser; the middle part of the dehydration tower is provided with a feed inlet, and the discharge outlet at the bottom is also connected with the feed inlet of the evaporator; the discharge port at the bottom of the evaporator discharges distilled waste liquid, and the discharge port at the upper part of the evaporator is connected with the inlet of the nitric acid condenser; the discharge port at the bottom of the nitric acid condenser is connected with the feed inlet at the top of the recovery nitric acid tank, and the discharge port at the lower part of the tower top condenser is connected with the feed inlet at the top of the condensate intermediate tank. According to the utility model, the dilute nitric acid with the mass concentration of more than or equal to 30% is obtained, the dilute nitric acid can meet the in-situ use requirement, and the tail gas is discharged up to the standard.
Description
Technical Field
The utility model belongs to the technical field of environmental treatment, and particularly relates to a dilute nitric acid waste liquid treatment and resource utilization production device.
Background
In the process of producing the medical intermediate p-nitrobenzoic acid by a nitric acid oxidation method, process wastewater is produced, wherein the process wastewater contains 10-15% of dilute nitric acid and 0.5-3% of organic impurities, and the nitric acid content is high, organic matters are difficult to degrade, and cannot be removed by alkali neutralization treatment, so that secondary pollution is caused, and the large-scale production of the p-methylbenzoic acid is limited.
Disclosure of Invention
In order to solve the problems, the invention discloses a dilute nitric acid waste liquid recycling treatment device, which is characterized in that after part of water is removed from the waste liquid, nitric acid is evaporated to obtain recovered nitric acid with use value, tail gas is discharged up to standard, the treatment capacity of the device is high, the operation cost is low, and the environmental effect and economic benefit are remarkably applicable to the requirement of large-scale production.
A nitrogen oxide waste gas treatment production device comprises a reboiler, a dehydration tower, a tower top condenser, a condensate intermediate tank, an evaporator, a nitric acid condenser, a nitric acid recovery tank and a nitric acid smoke treatment device; the discharge port at the upper part of the reboiler is connected with the feed port at the lower part of the dehydration tower, and the feed port at the bottom is connected with the discharge port at the bottom of the dehydration tower; the discharge port at the top of the dehydration tower is connected with the feed port of the tower top condenser; the middle part of the dehydration tower is provided with a feed inlet, and the discharge outlet at the bottom is also connected with the feed inlet of the evaporator; the discharge port at the bottom of the evaporator discharges distilled waste liquid, and the discharge port at the upper part of the evaporator is connected with the inlet of the nitric acid condenser; the discharge port at the bottom of the nitric acid condenser is connected with the feed port at the top of the recovery nitric acid tank, and the discharge port at the lower part of the tower top condenser is connected with the feed port at the top of the condensate intermediate tank; the discharge port at the bottom of the condensate intermediate tank is divided into two discharge pipelines; one of the discharge pipelines is connected with a condensate conveying pump II; the outlet of the condensate delivery pump II is connected with a nitrate smoke treatment device, and a flow regulating valve I is arranged on a connecting pipeline; the other discharging pipeline is connected with the condensate collecting tank through the condensate conveying pump I.
Further, a nitric acid concentration meter and a flow regulating valve L1 are arranged on a pipeline, wherein a discharge hole at the bottom of the dehydration tower is connected with a feed hole of the evaporator, and the flow regulating valve L1 is controlled by liquid level regulation of the bottom of the dehydration tower.
Further, a steam pressure regulating valve P1 is arranged on a heating steam inlet pipe of the reboiler.
Furthermore, the dehydration tower is internally provided with ceramic structured packing, and the top of the tower is internally provided with an internal reflux device.
Further, a first air outlet is formed in the side surface of the lower part of the tower top condenser, a second air outlet is formed in the top of the condensate intermediate tank, a third air outlet is formed in the side surface of the lower part of the nitric acid condenser, and a fourth air outlet is formed in the top of the recovered nitric acid tank; the first air outlet, the second air outlet, the third air outlet and the fourth air outlet are all connected with a nitric acid smoke treatment device in a concentrated manner through pipelines, and absorption liquid generated by the nitric acid smoke treatment device returns to the pipeline in front of a feeding flow regulating valve of the dehydration tower; and the waste gas generated in all the processes is collected and enters a nitric acid smoke treatment device for condensation water absorption treatment and then is discharged after reaching the standard.
Further, a feeding flow regulating valve F1 is arranged on a feeding pipe connected with a feeding port of the dehydration tower.
Further, a flow regulating valve L2 is arranged on a discharge pipeline of the first condensate conveying pump, and the flow regulating valve L2 is controlled by liquid level regulation of the condensate intermediate tank.
The production process of the device comprises the following steps:
The dilute nitric acid waste liquid is continuously pumped into the middle part of the dehydration tower and enters the dehydration tower, the temperature is raised by a reboiler, the nitric acid content in the condensate water extracted from the tower top is lower than 0.5% by controlling the temperature and the reflux ratio of the top of the dehydration tower, one part of the condensate water is used as water for a nitric acid smoke treatment device, and the other part of the condensate water is sent to a biochemical treatment system for treatment. The nitric acid content in tower bottom liquid extracted from the tower bottom is controlled to be 30-32% by adjusting the temperature of the tower bottom of the dehydration tower, the tower bottom liquid enters an evaporator, the recovered nitric acid with the mass concentration of more than 30% is obtained in the evaporator through evaporation and condensation treatment, and the evaporation residual liquid is mainly organic impurities and is further treated after being collected. Waste gas generated in all the processes is collected and enters a nitric acid smoke treatment device for condensate absorption treatment and then is discharged after reaching standards, and absorption liquid returns to dilute nitric acid waste liquid to realize cyclic treatment.
The utility model has the beneficial effects that: the water is removed in the dehydration tower by utilizing the rectification separation principle, so that the nitric acid concentration in the waste liquid is increased to 30-32%, and then dilute nitric acid with the mass concentration of more than or equal to 30% is obtained by evaporation by utilizing the characteristics of nitric acid and water, and is recycled. And the waste gas containing nitrogen oxides generated in the operation process is subjected to absorption treatment, and the obtained absorption liquid is returned to the dilute nitric acid waste liquid, so that the cyclic treatment is realized, and the waste gas reaches the emission standard.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
list of reference numerals:
Wherein 1-reboiler; 2-a dehydration tower; 3A-a condensate delivery pump I; 3B-a condensate delivery pump II; 4. a tower top condenser; 5. a condensate intermediate tank; 6. an evaporator; 7. a nitric acid condenser; 8. recovering the nitric acid tank; 9. and a nitric acid fume treatment device.
Detailed Description
The present invention is further illustrated in the following drawings and detailed description, which are to be understood as being merely illustrative of the invention and not limiting the scope of the invention. It should be noted that the words "front", "rear", "left", "right", "upper" and "lower" used in the following description refer to directions in the drawings, and the words "inner" and "outer" refer to directions toward or away from, respectively, the geometric center of a particular component.
As shown in fig. 1, the apparatus for treating and producing nitrogen oxide waste gas in this embodiment comprises a reboiler 1, a dehydration tower 2, a tower top condenser 4, a condensate intermediate tank 5, an evaporator 6, a nitric acid condenser 7, a recovered nitric acid tank 8 and a nitric acid smoke treatment device 9; the discharge port at the upper part of the reboiler 1 is connected with the feed port at the lower part of the dehydration tower 2, and the feed port at the bottom is connected with the discharge port at the bottom of the dehydration tower 2; a steam pressure regulating valve P1 is arranged on a heating steam inlet pipe of the reboiler 1.
The discharge port at the top of the dehydration tower 2 is connected with the feed port of the tower top condenser 4; the middle part of the dehydration tower 2 is provided with a feed inlet, and the discharge outlet at the bottom is also connected with the feed inlet of the evaporator 6; the pipeline that the discharge gate in the bottom of the dehydration tower 2 is connected with the feed inlet of the evaporator is provided with a nitric acid concentration meter and a flow regulating valve L1, and the flow regulating valve L1 is controlled by the liquid level regulation of the tower kettle of the dehydration tower 2. A feeding flow regulating valve F1 is arranged on a feeding pipe connected with a feeding port of the dehydration tower 2.
The discharge port at the bottom of the evaporator 6 discharges distilled waste liquid, and the discharge port at the upper part is connected with the inlet of the nitric acid condenser 7; the discharge port at the bottom of the nitric acid condenser 7 is connected with the feed port at the top of the nitric acid recovery tank 8, and the discharge port at the lower part of the overhead condenser 4 is connected with the feed port at the top of the condensate intermediate tank 5; the discharge port at the bottom of the condensate intermediate tank 5 is divided into two discharge pipelines; one of the discharge pipelines is connected with a condensate conveying pump II 3B; the outlet of the condensate conveying pump II 3B is connected with a nitrate fume treatment device 9, and a flow regulating valve F2 is arranged on the connecting pipeline; the other discharging pipeline is connected with a condensate collection tank through a condensate conveying pump I3A; a flow regulating valve L2 is arranged on the discharge pipeline of the first condensate conveying pump 3A, and the flow regulating valve L2 is controlled by the liquid level regulation of the condensate intermediate tank 5.
Wherein the dehydration tower 2 is internally provided with ceramic structured packing and the top part in the tower is provided with an internal reflux device.
The side surface of the lower part of the tower top condenser 4 is provided with a first air outlet, the top of the condensate intermediate tank 5 is provided with a second air outlet, the side surface of the lower part of the nitric acid condenser 7 is provided with a third air outlet, and the top of the recovery nitric acid tank 8 is provided with a fourth air outlet; the first air outlet, the second air outlet, the third air outlet and the fourth air outlet are all connected with the nitric acid smoke treatment device 9 in a concentrated way through pipelines, and absorption liquid generated by the nitric acid smoke treatment device 9 returns to the feeding pipeline of the dehydration tower 2 through the pipelines.
Wherein 1-reboiler; 2-a dehydration tower; 3A-a condensate delivery pump I; 3B-a condensate delivery pump II; 4. a tower top condenser; 5. a condensate intermediate tank; 6. an evaporator; 7. a nitric acid condenser; 8. recovering the nitric acid tank; 9. and a nitric acid fume treatment device.
Before the device operates, the nitrate fume treatment device 9 is started, and then the feeding operation is started. Opening a flow control regulating valve F1, setting a flow control value at 1500kg/h, pumping dilute nitric acid waste liquid from the middle part of a dehydration tower 2 with continuous stable flow, opening a steam inlet valve and a steam outlet valve of a reboiler 1, controlling a steam inlet pressure regulating valve P1 at 0.4MPa for heating and raising the temperature, and controlling the temperature of the top of the tower to be 100+/-1 ℃ and the reflux ratio to be 1.2+/-0.2. Under the condition, the nitric acid content in the condensed water condensed by the tower top condenser 4 is lower than 0.5 percent. When the liquid level of the condensate intermediate tank 5 rises to 50%, the condensate conveying pump I3A is started, the outlet flow regulating valve L2 is started, and the liquid level of the condensate intermediate tank is stably controlled to be 50-60%. And simultaneously controlling the temperature of the tower kettle to be 108+/-1 ℃, wherein the nitric acid content in the tower kettle liquid reaches over 32 percent, and when the liquid level of the tower kettle rises to 70 percent, starting a flow regulating valve L1 to convey the tower kettle liquid to the evaporator, and maintaining the process parameters of 60-80 percent of the liquid level of the tower kettle, 108+/-1 ℃ of the temperature of the tower kettle, 100+/-1 ℃ of the temperature of the tower top, 1.2 of the reflux ratio and the like to be stable, so that the dehydration tower is in a stable running state.
The mass concentration of nitric acid in tower bottom liquid entering the evaporator 6 is stabilized to be more than 32%, when the liquid level in the evaporator 6 rises to 60%, a steam inlet valve and a steam outlet valve of a heater are opened, the steam inlet pressure regulating valve P2 is controlled to be 0.4MPa for heating and heating, when the temperature of the evaporator rises to 116-120 ℃, nitric acid steam enters a nitric acid condenser for cooling to be recovered nitric acid with the concentration higher than 30%, and the recovered nitric acid enters a recovered nitric acid tank. And a small amount of evaporated waste liquid is discharged from a discharge hole at the bottom of the evaporator at fixed time, and is subjected to concentrated incineration treatment.
And opening a flow regulating valve F2, setting flow parameters according to the operation requirement of the smoke treatment device, and starting a condensate conveying pump 3B to pump condensate to the smoke treatment device, so that the whole production device is in a stable and automatic operation state.
The beneficial effects of this embodiment are: the set of dilute nitric acid waste liquid treatment device can recycle recovered nitric acid obtained by dehydrating and evaporating the dilute nitric acid waste liquid into a production process, and the tower kettle residual liquid in the evaporation process is rich in organic impurities and can be subjected to concentrated incineration treatment. The content of nitrogen oxides in the waste gas is lower than the emission requirement of industrial waste gas, the resource utilization of dilute nitric acid waste liquid is realized, the equipment investment is low, the treatment effect is good, and the method belongs to the green chemical technology. High automation degree, low operation cost and obvious economic and environmental benefits.
The technical means disclosed by the scheme of the invention is not limited to the technical means disclosed by the embodiment, and also comprises the technical scheme formed by any combination of the technical features.
Claims (7)
1. A dilute nitric acid waste liquid treatment device is characterized in that: comprises a reboiler (1), a dehydration tower (2), a tower top condenser (4), a condensate intermediate tank (5), an evaporator (6), a nitric acid condenser (7), a recovered nitric acid tank (8) and a nitric acid smoke treatment device (9); the discharge port at the upper part of the reboiler (1) is connected with the feed port at the lower part of the dehydration tower (2), and the feed port at the bottom is connected with the discharge port at the bottom of the dehydration tower (2); a discharge port at the top of the dehydrating tower (2) is connected with a feed port of a tower top condenser (4); the middle part of the dehydration tower (2) is provided with a feed inlet, and the discharge outlet at the bottom is also connected with the feed inlet of the evaporator (6); the discharge port at the bottom of the evaporator (6) discharges distilled waste liquid, and the discharge port at the upper part is connected with the inlet of the nitric acid condenser (7); the discharge port at the bottom of the nitric acid condenser (7) is connected with the feed port at the top of the nitric acid recovery tank (8), and the discharge port at the lower part of the overhead condenser (4) is connected with the feed port at the top of the condensate intermediate tank (5); the discharge port at the bottom of the condensate intermediate tank (5) is divided into two discharge pipelines; one of the discharge pipelines is connected with a condensate conveying pump II (3B); the outlet of the condensate conveying pump II (3B) is connected with a nitrate fume treatment device (9), and a first flow regulating valve (F2) is arranged on a connecting pipeline; the other discharging pipeline is connected with the condensate collection tank through a condensate conveying pump I (3A).
2. The dilute nitric acid waste liquid treatment device according to claim 1, wherein: the pipeline that the discharge gate of dehydration tower (2) bottom is connected with the evaporimeter feed inlet is last to be installed nitric acid concentration meter and flow control valve L1, and this flow control valve L1 is by dehydration tower (2) tower cauldron liquid level regulation control.
3. The dilute nitric acid waste liquid treatment device according to claim 1, wherein: a steam pressure regulating valve P1 is arranged on a heating steam inlet pipeline of the reboiler (1).
4. The dilute nitric acid waste liquid treatment device according to claim 1, wherein: the dehydration tower (2) is internally provided with ceramic structured packing, and the top of the tower is internally provided with an internal reflux device.
5. The dilute nitric acid waste liquid treatment device according to claim 1, wherein: the side surface of the lower part of the tower top condenser (4) is provided with a first air outlet, the top of the condensate intermediate tank (5) is provided with a second air outlet, the side surface of the lower part of the nitric acid condenser (7) is provided with a third air outlet, and the top of the recovery nitric acid tank (8) is provided with a fourth air outlet; the first air outlet, the second air outlet, the third air outlet and the fourth air outlet are all connected with the nitric acid smoke treatment device (9) in a concentrated way through pipelines, and absorption liquid generated by the nitric acid smoke treatment device (9) returns to a feeding pipeline of the dehydration tower (2) through the pipelines.
6. The dilute nitric acid waste liquid treatment device according to claim 1, wherein: a feeding flow regulating valve F1 is arranged on a feeding pipe connected with a feeding port of the dehydration tower (2).
7. The dilute nitric acid waste liquid treatment device according to claim 1, wherein: a flow regulating valve L2 is arranged on a discharge pipeline of the first condensate conveying pump (3A), and the flow regulating valve L2 is controlled by liquid level regulation of a condensate intermediate tank (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322825573.5U CN221440395U (en) | 2023-10-20 | 2023-10-20 | Dilute nitric acid waste liquid treatment device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322825573.5U CN221440395U (en) | 2023-10-20 | 2023-10-20 | Dilute nitric acid waste liquid treatment device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN221440395U true CN221440395U (en) | 2024-07-30 |
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ID=92069310
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202322825573.5U Active CN221440395U (en) | 2023-10-20 | 2023-10-20 | Dilute nitric acid waste liquid treatment device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN221440395U (en) |
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2023
- 2023-10-20 CN CN202322825573.5U patent/CN221440395U/en active Active
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