CN112370939A - Ammonia gas recovery method in ammonium molybdate crystallization process - Google Patents
Ammonia gas recovery method in ammonium molybdate crystallization process Download PDFInfo
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- CN112370939A CN112370939A CN202011079748.7A CN202011079748A CN112370939A CN 112370939 A CN112370939 A CN 112370939A CN 202011079748 A CN202011079748 A CN 202011079748A CN 112370939 A CN112370939 A CN 112370939A
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- absorption
- ammonia
- ammonium molybdate
- tail gas
- spray header
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—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 absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/406—Ammonia
Abstract
The invention discloses an ammonia recovery method in an ammonium molybdate crystallization process, which adopts ammonium molybdate buffer solution as absorption liquid to absorb ammonia by three-stage spraying, and specifically comprises the following steps: step 1, primary spraying and ammonia absorption, step 2, secondary and tertiary spraying and ammonia absorption, and step 3, ammonium molybdate solution treatment. The ammonia absorption amount of the invention is large, ammonia-containing tail gas with different concentrations can be processed, ammonium molybdate entrained in the tail gas can be completely recovered, ammonia gas can be recovered and reused, and the problems of ammonia gas pollution and secondary pollution are not generated.
Description
Technical Field
The invention belongs to the technical field of molybdenum powder metallurgy, and relates to a method for recovering ammonia gas in an ammonium molybdate crystallization process.
Background
In the domestic molybdenum hydrometallurgy production process, liquid ammonia is used for preparing an analytical agent for production, ammonium molybdate products are prepared by crystallization through methods such as evaporation and the like, and tail gas NH is generated in the process3. The ammonia gas is water-soluble colorless and alkaline irritant gas, which not only pollutes the atmosphere, but also can cause eutrophication after being dissolved in water, thereby polluting water sources and causing environmental pollution. At present, ammonia gas is treated by adopting a spraying method, and treating liquid enters wastewater, so that the ammonia content in the wastewater exceeds the standard, and secondary pollution is formed. The new technology of the biological filter tower is suitable for treating ammonia in wastewater; the incineration technology is only applied to high ammonia concentration in some petrochemical industries, and ammonia combustion heat energy is required to be provided, so that carbon dioxide and the like are generated and discharged. In a word, the existing waste gas treatment has low efficiency and long time consumption, and reduces the production efficiency.
Disclosure of Invention
The invention aims to provide a method for recovering ammonia gas in the crystallization process of ammonium molybdate, which can treat tail gas containing ammonia with different concentrations, can completely recover the ammonium molybdate entrained in the tail gas, can recover and reuse the ammonia gas, and does not generate the problems of ammonia gas pollution and secondary pollution.
The technical scheme adopted by the invention is that the ammonia recovery method in the ammonium molybdate crystallization process specifically comprises the following steps:
step 1, carrying out dust collection and ammonia absorption on ammonia tail gas carrying ammonium molybdate through a primary spray header, wherein the ammonium molybdate carrying ammonia tail gas is sprayed and absorbed, the ammonia tail gas falls into an absorption pool I along with spraying absorption liquid, one part of the ammonia tail gas is sprayed and absorbed, the other part of the ammonia tail gas which is not absorbed falls into the absorption pool I along with the spraying absorption liquid, and the other part of the ammonia tail gas flows to the secondary spray header;
2, dividing the ammonia tail gas flowing to the secondary spray header into two parts, spraying and absorbing one part of the ammonia tail gas, allowing the sprayed and absorbed liquid to enter an absorption tank II, allowing the other part of unabsorbed ammonia tail gas to flow to the tertiary spray header, absorbing the ammonia tail gas flowing to the tertiary spray header by using absorption liquid sprayed by the tertiary spray header, and allowing the ammonia tail gas to enter the absorption tank II, wherein the generated tail gas is directly discharged;
The present invention is also characterized in that,
and the absorption liquid sprayed out of the first-stage spray header, the second-stage spray header and the third-stage spray header is ammonium molybdate buffer solution.
The ammonium molybdate buffer solution is ammonium molybdate ammonia immersion liquid, ammonium molybdate ammonia mother liquor or other ammonium molybdate solutions.
One side of the upper end of the absorption tank I is provided with a feed inlet, one side of the lower end of the absorption tank I is provided with a sewage discharge outlet A, the top of the absorption tank I is provided with a molybdenum trioxide adding port, and a stirring device is arranged in the absorption tank I.
And a PH meter and a pressure sensor are arranged in the absorption pool II.
The absorption tank I is communicated with the absorption tank II through a connecting pipe, and one side of the absorption tank II, which is far away from the absorption tank I, is provided with a sewage discharge outlet B and a discharge outlet respectively.
The connecting pipe is in an asymmetric V-shaped or U-shaped structure.
The pipeline that the connecting pipe connects absorption cell I one side is longer, and the pipeline that the connecting pipe connects absorption cell II one side is shorter.
The invention has the following beneficial effects:
(1) the invention adopts the ammonium molybdate buffer solution with the subacidity as the ammonia absorption solution, the absorption capacity of the ammonium molybdate buffer solution is larger than that of pure water, and when the specific gravity of the ammonium molybdate buffer solution is more than or equal to 1.15g/cm3Can be used as the raw material for ammonium molybdate crystallization to prepare ammonium molybdate.
(2) The invention can treat tail gas containing ammonia with different concentrations, the ammonium molybdate in the tail gas can be completely recovered, the ammonia gas can be recovered and reused, and the problems of ammonia gas pollution and secondary pollution are not generated.
(3) The method adopts the ammonium molybdate meta-acid buffer solution to recover the ammonia tail gas, is environment-friendly, and realizes the comprehensive utilization of resources.
(4) The invention adopts dynamic measurement and control, has simple operation process, easy realization of automatic control and strong technological adaptability, and is also suitable for recycling ammonia gas in the crystallization process of ammonium tungstate, ammonium rhenate and the like.
Drawings
FIG. 1 is a flow diagram of a method for ammonia recovery during ammonium molybdate crystallization in accordance with the present invention.
In the figure, 1 is a first-stage spray header, 2 is a second-stage spray header, 3 is a third-stage spray header, 4 is an absorption tank I, 5 is an absorption tank II, 6 is a feed inlet, 7 is a sewage discharge outlet A, 8 is a molybdenum trioxide addition port, 9 is a stirring device, 10 is a PH meter, 11 is a pressure sensor, 12 is a connecting pipe, 13 is a sewage discharge outlet B, 14 is a discharge outlet.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention discloses a method for recovering ammonia gas in the crystallization process of ammonium molybdate, which comprises the following steps:
step 1, primary spraying, dust collecting and ammonia absorbing;
the ammonia tail gas that will smuggle ammonium molybdate secretly gathers dust through one-level shower head 1 and inhales ammonia, and at this moment, smuggle ammonium molybdate secretly and be sprayed and absorb, fall into absorption cell I along with spraying the absorption liquid, and ammonia tail gas is divided into two parts, and partly ammonia tail gas is sprayed and is absorbed, falls into absorption cell I4 along with spraying the absorption liquid for absorption liquid specific gravity in the absorption cell I increases, and the pH value increases. The other part of unabsorbed ammonia tail gas flows to a secondary spray header;
the ammonium molybdate buffer solution is ammonium molybdate ammonia immersion liquid, ammonium molybdate ammonia mother liquor or other ammonium molybdate solutions.
Step 2, secondary and tertiary spraying and absorbing ammonia;
the ammonia tail gas flowing to the secondary spray header 2 is divided into two parts, one part is sprayed and absorbed, the sprayed and absorbed liquid enters the absorption tank II, the other part of unabsorbed ammonia tail gas flows to the tertiary spray header, the ammonia tail gas flowing to the tertiary spray header 3 is absorbed by the absorption liquid sprayed out by the tertiary spray header 3 and then enters the absorption tank II5, the PH value of the absorption liquid is further increased, and the generated tail gas is directly discharged;
and (4) after three-stage spraying ammonia absorption, continuously reacting the ammonia tail gas with the absorption liquid, and increasing the pH value of the solution to obtain a new ammonium molybdate solution. The ion change is:
since the absorption cell I4 is communicated with the absorption cell II5, when the pH value of the solution in the absorption cell II5 reaches neutral and the specific gravity is higher<1.15g/cm3In the meantime, molybdenum trioxide was added to the absorption cell I4, and the molybdenum trioxide was uniformly stirred by the stirring device 9 to dissolve the molybdenum trioxide in the absorption liquid in the absorption cell I4, and the PH values of the absorption liquids in the absorption cell I4 and the absorption cell II5 were reduced to 6.0 or less, and the ionization was changed:
specific gravity of new absorption liquid<1.15g/cm3The method can be repeatedly applied to the ammonia tail gas absorption in the step 1 and the step 2; when the specific gravity of the absorption liquid is more than or equal to 1.15g/cm3Can be used as ammonium molybdate crystallization raw material to prepare ammonium molybdate products, thereby realizing comprehensive utilization of resources.
The steps 2 and 3
Can be that
Or one or more of other molybdenum oxy polymer anions.
The absorption liquid sprayed out of the first-stage spray header 1, the second-stage spray header 2 and the third-stage spray header 3 is ammonium molybdate buffer liquid.
A feed inlet 6 is formed in one side of the upper end of the absorption tank I4, a sewage discharge outlet A7 is formed in one side of the lower end of the absorption tank I4, a molybdenum trioxide addition port 8 is formed in the top of the absorption tank I4, and a stirring device 9 is arranged in the absorption tank I4.
The stirring device 9 is a conventional device. The feed inlet 6 is used for introducing absorption liquid, the molybdenum trioxide adding port 8 is used for adding molybdenum trioxide, and the stirring device 9 is used for dissolving or reacting and stirring molybdenum trioxide and ammonium molybdate.
An on-line pH meter 10 and a pressure sensor 11 are arranged in the absorption tank II 5. The PH meter 10 dynamically tests the PH value of the absorption liquid on line, and the pressure sensor 11 dynamically tests the specific gravity of the absorption liquid on line.
The absorption tank I4 is communicated with the absorption tank II5 through a connecting pipe 12, and one side of the absorption tank II5, which is far away from the absorption tank I4, is respectively provided with a sewage discharge port B13 and a discharge port 14. The discharge port 14 is used for discharging the absorption liquid.
The connecting tube 12 is of an asymmetric V-shaped or U-shaped configuration. The pipe on the side of the connection pipe 12 connected to the absorption cell I4 is long, and the pipe on the side of the connection pipe 12 connected to the absorption cell II5 is short.
The connecting pipe 12 is inverted when being installed and is lower than the liquid level of the absorption liquid, so that the absorption liquids in the absorption tank I and the absorption tank II which are communicated with each other are uniformly mixed; and a pipeline on one side of the absorption tank I is longer, so that undissolved substances are prevented from entering the absorption tank II due to stirring.
Drain A7 and drain B13 were used for equipment cleaning.
Example 1
The pH value of 5.5 and the specific gravity of 1.05g/cm are introduced from the feed inlet 6 of the absorption tank I43The ammonium molybdate ammonia leaching solution is used as an ammonia tail gas absorption solution. During tail gas absorption, firstly, dust is collected and ammonia is absorbed from ammonia tail gas generated by ammonium molybdate crystallization through a primary spray header 1, an absorption liquid with a pH value of 5.5 is sprayed to absorb the tail gas, ammonium molybdate and part of ammonia are carried back to an absorption tank I4, the specific gravity of the solution is increased, and the pH value is increased; subsequently, ammonia is absorbed through the second-level spray header 2, the sprayed absorption liquid absorbs ammonia and enters the absorption tank II, the ammonia is absorbed through the third-level spray header 3, the sprayed absorption liquid absorbs ammonia and enters the absorption tank II, tail gas reaches the national emission standard of ammonia tail gas, the tail gas is directly discharged into the atmosphere, the ammonia is absorbed by the absorption liquid and enters the absorption tank II5, and the pH value of the absorption liquid is further increased. A connecting pipe 12 is arranged between the absorption pool I4 and the absorption pool II5, and the connecting pipe 12 is in an asymmetric V shape and is arranged upside down. The absorption liquid in the absorption tank I4 and the absorption tank II5 are communicated with each other, so that the absorption liquid in the two tanks can be uniformly mixed. In the ammonia gas recovery process, when the pH value of the absorption liquid reaches 7.2 and the pressure is sensedSpecific gravity of less than 1.15g/cm measured by the instrument3In the process, high-purity molybdenum trioxide is added into the solution through a molybdenum trioxide adding port 8 and stirred to reduce the pH value to 5.5, and the new absorption liquid can be repeatedly applied to ammonia tail gas absorption; the absorption is repeatedly circulated, and when the specific gravity of the absorption liquid measured by the pressure sensor is 1.15g/cm3And in the process, the ammonium molybdate crystal is discharged through a discharge hole of the absorption pool II5 and used as an ammonium molybdate crystal raw material for preparing an ammonium molybdate product, so that the comprehensive utilization of resources is realized.
Example 2
The pH value of the mixture is 6.0 and the specific gravity of the mixture is 1.03g/cm through the feed inlet 6 of the absorption tank I43The ammonium molybdate mother liquor is used as an ammonia tail gas absorption liquid. During tail gas absorption, firstly, dust is collected and ammonia is absorbed from ammonia tail gas generated by ammonium molybdate crystallization through a primary spray header 1, an absorption liquid with a pH value of 5.5 is sprayed to absorb the tail gas, ammonium molybdate and part of ammonia are carried back to an absorption tank I4, the specific gravity of the solution is increased, and the pH value is increased; and then ammonia is absorbed by the secondary spray header 2, the sprayed absorption liquid absorbs ammonia and returns to the absorption tank II5, the ammonia is absorbed by the tertiary spray header 3, the sprayed absorption liquid absorbs ammonia and returns to the absorption tank II5, the tail gas reaches the national emission standard of ammonia tail gas and is directly discharged into the atmosphere, the ammonia is absorbed by the absorption liquid and enters the absorption tank II5, and the pH value of the ammonium molybdate mother liquor is further increased. A connecting pipe 12 is arranged between the absorption pool I4 and the absorption pool II5, and the connecting pipe 12 is in an asymmetric U shape and is arranged upside down. The absorption liquid in the absorption tank I4 and the absorption tank II5 are communicated with each other, so that the absorption liquid in the two tanks can be uniformly mixed. In the ammonia gas recovery process, when the pH value of the absorption liquid reaches 7.1 and the specific gravity measured by a pressure sensor is less than 1.15g/cm3In the process, high-purity molybdenum trioxide is added into the absorption tank I4 through a molybdenum trioxide adding port 8 and stirred to reduce the pH value of the absorption liquid to 6.0, and the new absorption liquid can be repeatedly applied to ammonia tail gas absorption; the absorption is repeatedly circulated, and when the specific gravity of the absorption liquid measured by the pressure sensor is 1.15g/cm3During the process, the ammonium molybdate crystal is discharged through a discharge hole 14 of the absorption pool II5 and used as an ammonium molybdate crystal raw material for preparing an ammonium molybdate product, so that the comprehensive utilization of resources is realized.
Example 3
The pH value of 5.6 and the specific gravity of 1.02g/cm are introduced from a feed inlet 6 of an absorption tank I43The ammonium tetramolybdate solution is used as ammonia tail gas absorption liquid. When tail gas is absorbed, firstlyAmmonia tail gas generated by ammonium molybdate crystallization is subjected to dust collection and ammonia absorption by a primary spray header 1, an absorption liquid with a pH value of 5.0 is sprayed to absorb the ammonia and part of ammonia in the tail gas and returns to an absorption tank I4, the specific gravity of the absorption liquid is increased, and the pH value is increased; and then ammonia is absorbed by the second-level spray header 2, the sprayed absorption liquid absorbs ammonia and returns to the absorption tank II5, the ammonia is absorbed by the third-level spray header, the sprayed absorption liquid absorbs ammonia and returns to the absorption tank II5, the tail gas reaches the national emission standard of ammonia tail gas and is directly discharged into the atmosphere, the ammonia is absorbed by the absorption liquid and returns to the tank II5, and the pH value of the absorption liquid is further increased. A connecting pipe 12 is arranged between the absorption pool I4 and the absorption pool II5, and the connecting pipe 12 is in an asymmetric V shape and is arranged upside down. The absorption liquid in the absorption tank I4 and the absorption tank II5 are communicated with each other, so that the absorption liquid in the two tanks can be uniformly mixed. In the ammonia gas recovery process, when the pH value of the absorption liquid reaches 7.0 and the specific gravity measured by a pressure sensor is less than 1.15g/cm3In the process, high-purity molybdenum trioxide is added into the absorption tank I4 through a molybdenum trioxide adding port 8, the pH value is reduced to 5.8 by stirring, and the new absorption liquid can be repeatedly applied to ammonia tail gas absorption; the absorption is repeatedly circulated, and when the specific gravity of the absorption liquid measured by the pressure sensor is 1.15g/cm3And in the process, the ammonium molybdate crystal is discharged through a discharge hole 14 in the absorption pool II and used as an ammonium molybdate crystal raw material for preparing an ammonium molybdate product, so that the comprehensive utilization of resources is realized.
Claims (8)
1. A method for recovering ammonia gas in the crystallization process of ammonium molybdate is characterized in that: the method specifically comprises the following steps:
step 1, carrying out dust collection and ammonia absorption on ammonia tail gas carrying ammonium molybdate through a primary spray header, wherein the ammonium molybdate carrying ammonia tail gas is sprayed and absorbed, the ammonia tail gas falls into an absorption pool I along with spraying absorption liquid, one part of the ammonia tail gas is sprayed and absorbed, the other part of the ammonia tail gas which is not absorbed falls into the absorption pool I along with the spraying absorption liquid, and the other part of the ammonia tail gas flows to the secondary spray header;
2, the ammonia tail gas flowing to the secondary spray header is divided into two parts, one part is sprayed and absorbed, the ammonia tail gas enters an absorption tank II along with spraying absorption liquid, the other part of unabsorbed ammonia tail gas flows to the tertiary spray header, the ammonia tail gas flowing to the tertiary spray header is absorbed by absorption liquid sprayed by the tertiary spray header and then enters the absorption tank II, and the generated tail gas is directly discharged;
step 3, because the absorption cell I is communicated with the absorption cell II, when the PH value of the solution in the absorption cell II reaches neutral and the specific gravity of the solution reaches<1.15g/cm3When the pH value of the absorption liquid in the absorption cell I and the absorption cell II is reduced to below 6.0 and the specific gravity is reduced, molybdenum trioxide is added into the absorption cell I<1.15g/cm3In the process, the absorption liquid in the absorption cell I and the absorption cell II can be repeatedly applied to the ammonia tail gas absorption in the step 1 and the step 2; when the specific gravity of the absorption liquid is more than or equal to 1.15g/cm3Can be used as ammonium molybdate crystallization raw material to prepare ammonium molybdate products, thereby realizing comprehensive utilization of resources.
2. The method for recovering ammonia gas in the crystallization process of ammonium molybdate according to claim 1, characterized in that: and the absorption liquid sprayed out of the first-stage spray header, the second-stage spray header and the third-stage spray header is ammonium molybdate buffer solution.
3. The method for recovering ammonia gas in the crystallization process of ammonium molybdate according to claim 2, characterized in that: the ammonium molybdate buffer solution is ammonium molybdate ammonia immersion liquid, ammonium molybdate ammonia mother liquor or other ammonium molybdate solutions.
4. The method for recovering ammonia gas in the crystallization process of ammonium molybdate according to claim 1, characterized in that: a feeding hole is formed in one side of the upper end of the absorption tank I, a sewage discharge port A is formed in one side of the lower end of the absorption tank I, a molybdenum trioxide adding port is formed in the top of the absorption tank I, and a stirring device is arranged in the absorption tank I.
5. The method for recovering ammonia gas in the crystallization process of ammonium molybdate according to claim 1, characterized in that: and a PH meter and a pressure sensor are arranged in the absorption pool II.
6. The method for recovering ammonia gas in the crystallization process of ammonium molybdate according to claim 1, characterized in that: the absorption tank I is communicated with the absorption tank II through a connecting pipe, and one side of the absorption tank II, which is far away from the absorption tank I, is provided with a sewage discharge outlet B and a discharge outlet respectively.
7. The method for recovering ammonia gas in the crystallization process of ammonium molybdate according to claim 6, characterized in that: the connecting pipe is of an asymmetric V-shaped or U-shaped structure.
8. The method for recovering ammonia gas in the crystallization process of ammonium molybdate according to claim 7, characterized in that: the pipeline that the connecting pipe is connected absorption tank I one side is longer, and the pipeline that the connecting pipe is connected absorption tank II one side is shorter.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1074486A (en) * | 1992-01-18 | 1993-07-21 | 戴元宁 | The chemical sorting method of wulfenite |
| US20060088461A1 (en) * | 2004-07-22 | 2006-04-27 | Innovene Usa Llc | Process for recovery and recycle of ammonia from a vapor stream |
| CN104370305A (en) * | 2014-10-23 | 2015-02-25 | 陕西华陆化工环保有限公司 | Method for producing ammonium molybdate |
| CN109665562A (en) * | 2019-01-31 | 2019-04-23 | 成都虹波钼业有限责任公司 | A kind of device and method preparing ammonium molybdate using molybdic acid |
| CN210631924U (en) * | 2019-04-11 | 2020-05-29 | 实联化工(江苏)有限公司 | Ammonia-containing tail gas recovery processing device |
-
2020
- 2020-10-10 CN CN202011079748.7A patent/CN112370939A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1074486A (en) * | 1992-01-18 | 1993-07-21 | 戴元宁 | The chemical sorting method of wulfenite |
| US20060088461A1 (en) * | 2004-07-22 | 2006-04-27 | Innovene Usa Llc | Process for recovery and recycle of ammonia from a vapor stream |
| CN104370305A (en) * | 2014-10-23 | 2015-02-25 | 陕西华陆化工环保有限公司 | Method for producing ammonium molybdate |
| CN109665562A (en) * | 2019-01-31 | 2019-04-23 | 成都虹波钼业有限责任公司 | A kind of device and method preparing ammonium molybdate using molybdic acid |
| CN210631924U (en) * | 2019-04-11 | 2020-05-29 | 实联化工(江苏)有限公司 | Ammonia-containing tail gas recovery processing device |
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