CN110438507A - A kind of alkali etching ammonia water recovery system - Google Patents
A kind of alkali etching ammonia water recovery system Download PDFInfo
- Publication number
- CN110438507A CN110438507A CN201910744018.5A CN201910744018A CN110438507A CN 110438507 A CN110438507 A CN 110438507A CN 201910744018 A CN201910744018 A CN 201910744018A CN 110438507 A CN110438507 A CN 110438507A
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- ammonia
- ammonium hydroxide
- recovery system
- water recovery
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/46—Regeneration of etching compositions
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Removal Of Specific Substances (AREA)
- Physical Water Treatments (AREA)
Abstract
The present invention provides a kind of alkali etching ammonia water recovery system, including S1 charging process, S2 abstraction process, S3 wastewater treatment process, S4 ammonium hydroxide generates technique: the high ammonia-nitrogen wastewater collected in step S2 is passed through inside stripping equipment, then the concentrated sulfuric acid is added as absorbing liquid, pH value adjustment agent is added to control the pH value of high ammonia-nitrogen wastewater 12, rotation speed of fan is 35-45HZ, temperature is heated to 19 degree, soak time was controlled at 5-10 hours, ammonium hydroxide is prepared, the ammonium hydroxide being prepared in step S3 is passed through in the ammonia generated in step S1, the ammonium hydroxide of new concentration is prepared, the ammonium hydroxide of new concentration is recycled into storage.Invention is handled waste water by supersaturated stripping tower, effective 100% recycling ammonia nitrogen resource, is reduced cost for wastewater treatment, and handle the waste water after extracting copper using milk of lime, is effectively reduced Waste water treatment medicament cost.
Description
Technical field
The present invention relates to alkaline etching liquid recovery technology field more particularly to a kind of alkali etching ammonia water recovery systems.
Background technique
Contain cupric ammine complex, ammonium chloride and ammonium hydroxide in alkaline etching waste liquid for producing, wherein copper content can reach 120-170g/L.If
Direct emission can bring serious harm to environment.In PCB Production, needs to carry out circular regeneration to etching waste liquor, reach
To make full use of resource, reduce cost, reduce pollutant row.
However, being left a large amount of ammonia nitrogen mixing after alkaline etching liquid has extracted metallic copper, big pollution is deposited very much to environment,
Directly processing has a large amount of dangerous waste and generates, and in the treatment process of waste water, expensive income is low.
Therefore, it is necessary to solve the above problems to invent a kind of alkali etching ammonia water recovery system
Summary of the invention
The purpose of the present invention is to provide a kind of alkali etching ammonia water recovery systems, to solve the above technical problems.
The present invention using following technical scheme in order to solve the above technical problems, realized:
A kind of alkali etching ammonia water recovery system, comprising the following steps:
S1 charging process: alkaline etching waste liquid for producing is added in reaction kettle, and being passed through temperature into reaction kettle is 60-80 degree
Then sodium hydroxide solution is added in vapor, when being stirred to react 3-4 after, obtain ammonia, copper oxide and sodium chloride, it is anti-
Answer equation as follows:
Cu(NH3)Cl2+ 2NaOH=Δ=12NH3+CuO+2NaCl；
S2 abstraction process: the ammonia generated in step S1 extraction is stored first, then by copper oxide and sodium chloride
It is filtered, washed and dries, be collected, remaining high ammonia-nitrogen wastewater is collected separately after finally reacting in step S1, stays
Make it is spare, and inside the copper oxide of collection be added salting liquid reacted, then washed using tap water, filter and
Drying, is prepared crystal form copper oxide；
S3 wastewater treatment process: the high ammonia-nitrogen wastewater collected in step S2 is passed through inside stripping equipment, is then added dense
PH value control of the pH value adjustment agent by high ammonia-nitrogen wastewater is added in 12, rotation speed of fan 35-45HZ, temperature as absorbing liquid in sulfuric acid
Degree is heated to 19 degree, and soak time was controlled at 5-10 hours, so that the Nitrogen ion in high ammonia-nitrogen wastewater be removed, ammonia is prepared
Water；
S4 ammonium hydroxide generates technique: the ammonium hydroxide being prepared in step S3 being passed through in the ammonia generated in step S1, will be filled
There is the storage equipment of ammonia to be rocked, be fully immersed into ammonia in ammonium hydroxide, the ammonium hydroxide of new concentration is prepared, by new concentration
Ammonium hydroxide recycling storage.
Preferably, the content of copper ion is the 80% of waste liquid in the step S1 neutral and alkali etching waste liquor.
Preferably, the mass concentration of sodium hydroxide solution is 30% in the step S1, and the moles total number of sodium hydroxide is
1-3 times of the mole of copper ion in alkaline etching waste liquid for producing.
Preferably, ammonia is stored after first passing around cold-zone to room temperature in the step S2, in the step S2
Drying temperature be 100-110 degree.
Preferably, stripping equipment is arranged using supersaturated stripping tower setting, and in supersaturated stripping tower in the step S3
There is polyhedron baton round filler.
Preferably, stripping equipment uses surface whole sealed set in the step S3, and its ammonium hydroxide rate of discharge is lower than
15mg/L。
Preferably, pH value adjustment agent is arranged using milk of lime in the step S3, and the milk of lime uses 80% lime
Amount and 20% water are stirred and are made.
The beneficial effects of the present invention are:
(1) present invention extracts the middle copper of alkaline etching liquid by using sodium hydroxide first, and will be alkaline
Ammonium ion generates ammonia in etching, reduces the ammonium ion in remaining waste water, improves the subsequent treatment effect to waste water.
(2) present invention is handled waste water by supersaturated stripping tower, adds the technique without steam, electric energy
Heat, and 100% recycling ammonia nitrogen resource, complete offset run processing cost, not only reduce cost for wastewater treatment, or even can also produce
Raw certain economic benefit, and the waste water after extracting copper is handled using milk of lime, it effectively reduces at waste water
Manage reagent cost.
Detailed description of the invention
Fig. 1 is the overall structure flow chart of invention.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained, and however, the following embodiments are merely preferred embodiments of the present invention, and not all.
Based on the implementation example in the implementation mode, those skilled in the art's obtained other realities without making creative work
Example is applied, protection scope of the present invention is belonged to.Experimental method in following embodiments is unless otherwise specified conventional method,
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment one:
The present invention provides a kind of alkali etching ammonia water recovery systems as shown in Figure 1, comprising the following steps:
S1 charging process: 80% alkaline etching waste liquid for producing that the content of middle copper ion is waste liquid is added in reaction kettle, and
The vapor that temperature is 60-80 degree is passed through into reaction kettle, it is 30% sodium hydroxide solution that mass concentration, which is then added, wherein hydrogen
The moles total number of sodium oxide molybdena is 1-3 times of the mole of copper ion in alkaline etching waste liquid for producing, when being stirred to react 3-4 after, obtain
To ammonia, copper oxide and sodium chloride, reaction equation is as follows:
Cu(NH3)Cl2+ 2NaOH=Δ=12NH3+CuO+2NaCl；
S2 abstraction process: the ammonia generated in step S1 extraction is stored first, then by copper oxide and sodium chloride
It is filtered, washed and dries, be collected, remaining high ammonia-nitrogen wastewater is collected separately after finally reacting in step S1, stays
Make it is spare, and inside the copper oxide of collection be added salting liquid reacted, then washed using tap water, filter and
Drying, is prepared crystal form copper oxide；
S3 wastewater treatment process: the high ammonia-nitrogen wastewater collected in step S2 is passed through inside supersaturated stripping tower, then plus
Enter the concentrated sulfuric acid as absorbing liquid, pH value adjustment agent milk of lime is added by the pH value control of high ammonia-nitrogen wastewater 12, rotation speed of fan is
35-45HZ, temperature are heated to 19 degree, and soak time was controlled at 5 hours, to the Nitrogen ion in high ammonia-nitrogen wastewater be removed, system
It is standby to obtain ammonium hydroxide；
S4 ammonium hydroxide generates technique: the ammonium hydroxide being prepared in step S3 being passed through in the ammonia generated in step S1, will be filled
There is the storage equipment of ammonia to be rocked, be fully immersed into ammonia in ammonium hydroxide, the ammonium hydroxide of new concentration is prepared, by new concentration
Ammonium hydroxide recycling storage.
Embodiment two:
A kind of alkali etching ammonia water recovery system, comprising the following steps:
S1 charging process: 80% alkaline etching waste liquid for producing that the content of middle copper ion is waste liquid is added in reaction kettle, and
The vapor that temperature is 60-80 degree is passed through into reaction kettle, it is 30% sodium hydroxide solution that mass concentration, which is then added, wherein hydrogen
The moles total number of sodium oxide molybdena is 1-3 times of the mole of copper ion in alkaline etching waste liquid for producing, when being stirred to react 3-4 after, obtain
To ammonia, copper oxide and sodium chloride, reaction equation is as follows:
Cu(NH3)Cl2+ 2NaOH=Δ=12NH3+CuO+2NaCl；
S2 abstraction process: the ammonia generated in step S1 extraction is stored first, then by copper oxide and sodium chloride
It is filtered, washed and dries, be collected, remaining high ammonia-nitrogen wastewater is collected separately after finally reacting in step S1, stays
Make it is spare, and inside the copper oxide of collection be added salting liquid reacted, then washed using tap water, filter and
Drying, is prepared crystal form copper oxide；
S3 wastewater treatment process: the high ammonia-nitrogen wastewater collected in step S2 is passed through inside supersaturated stripping tower, then plus
Enter the concentrated sulfuric acid as absorbing liquid, pH value adjustment agent milk of lime is added by the pH value control of high ammonia-nitrogen wastewater 12, rotation speed of fan is
35-45HZ, temperature are heated to 19 degree, and soak time was controlled at 8 hours, to the Nitrogen ion in high ammonia-nitrogen wastewater be removed, system
It is standby to obtain ammonium hydroxide；
S4 ammonium hydroxide generates technique: the ammonium hydroxide being prepared in step S3 being passed through in the ammonia generated in step S1, will be filled
There is the storage equipment of ammonia to be rocked, be fully immersed into ammonia in ammonium hydroxide, the ammonium hydroxide of new concentration is prepared, by new concentration
Ammonium hydroxide recycling storage.
Embodiment three:
A kind of alkali etching ammonia water recovery system, comprising the following steps:
S1 charging process: 80% alkaline etching waste liquid for producing that the content of middle copper ion is waste liquid is added in reaction kettle, and
The vapor that temperature is 60-80 degree is passed through into reaction kettle, it is 30% sodium hydroxide solution that mass concentration, which is then added, wherein hydrogen
The moles total number of sodium oxide molybdena is 1-3 times of the mole of copper ion in alkaline etching waste liquid for producing, when being stirred to react 3-4 after, obtain
To ammonia, copper oxide and sodium chloride, reaction equation is as follows:
Cu(NH3)Cl2+ 2NaOH=Δ=12NH3+CuO+2NaCl；
S2 abstraction process: the ammonia generated in step S1 extraction is stored first, then by copper oxide and sodium chloride
It is filtered, washed and dries, be collected, remaining high ammonia-nitrogen wastewater is collected separately after finally reacting in step S1, stays
Make it is spare, and inside the copper oxide of collection be added salting liquid reacted, then washed using tap water, filter and
Drying, is prepared crystal form copper oxide；
S3 wastewater treatment process: the high ammonia-nitrogen wastewater collected in step S2 is passed through inside supersaturated stripping tower, then plus
Enter the concentrated sulfuric acid as absorbing liquid, pH value adjustment agent milk of lime is added by the pH value control of high ammonia-nitrogen wastewater 12, rotation speed of fan is
35-45HZ, temperature are heated to 19 degree, and soak time was controlled at 10 hours, to the Nitrogen ion in high ammonia-nitrogen wastewater be removed, system
It is standby to obtain ammonium hydroxide；
S4 ammonium hydroxide generates technique: the ammonium hydroxide being prepared in step S3 being passed through in the ammonia generated in step S1, will be filled
There is the storage equipment of ammonia to be rocked, be fully immersed into ammonia in ammonium hydroxide, the ammonium hydroxide of new concentration is prepared, by new concentration
Ammonium hydroxide recycling storage.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
For personnel it should be appreciated that the present invention is not limited to the above embodiments, described in the above embodiment and specification is only the present invention
Preference, be not intended to limit the invention, without departing from the spirit and scope of the present invention, the present invention also has various
Changes and improvements, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by institute
Attached claims and its equivalent thereof.
Claims (7)
1. a kind of alkali etching ammonia water recovery system, which comprises the following steps:
S1 charging process: alkaline etching waste liquid for producing is added in reaction kettle, and is passed through the water that temperature is 60-80 degree into reaction kettle and is steamed
Then sodium hydroxide solution is added in gas, when being stirred to react 3-4 after, obtain ammonia, copper oxide and sodium chloride, reaction side
Formula is as follows:
Cu(NH3)Cl2+ 2NaOH=Δ=12NH3+CuO+2NaCl；
S2 abstraction process: first storing the ammonia generated in step S1 extraction, then filter copper oxide and sodium chloride,
Washing and drying, are collected, and remaining high ammonia-nitrogen wastewater is collected separately after finally reacting in step S1, give over to standby
With, and salting liquid is added inside the copper oxide of collection and is reacted, it then washed, filtered and is dried using tap water
It is dry, crystal form copper oxide is prepared；
S3 wastewater treatment process: the high ammonia-nitrogen wastewater collected in step S2 is passed through inside stripping equipment, the concentrated sulfuric acid is then added
As absorbing liquid, pH value adjustment agent is added and controls the pH value of high ammonia-nitrogen wastewater 12, rotation speed of fan 35-45HZ, temperature adds
To 19 degree, soak time was controlled at 5-10 hours heat, so that the Nitrogen ion in high ammonia-nitrogen wastewater be removed, ammonium hydroxide is prepared；
S4 ammonium hydroxide generates technique: the ammonium hydroxide being prepared in step S3 being passed through in the ammonia generated in step S1, ammonia will be housed
The storage equipment of gas is rocked, and is fully immersed into ammonia in ammonium hydroxide, and the ammonium hydroxide of new concentration is prepared, by the ammonium hydroxide of new concentration
Recycling storage.
2. a kind of alkali etching ammonia water recovery system according to claim 1, it is characterised in that: the step S1 neutral and alkali
The content of copper ion is the 80% of waste liquid in etching waste liquor.
3. a kind of alkali etching ammonia water recovery system according to claim 1, it is characterised in that: hydrogen-oxygen in the step S1
The mass concentration for changing sodium solution is 30%, and the moles total number of sodium hydroxide is the 1- of the mole of copper ion in alkaline etching waste liquid for producing
3 times.
4. a kind of alkali etching ammonia water recovery system according to claim 1, it is characterised in that: ammonia in the step S2
It is stored after first passing around cold-zone to room temperature, the drying temperature in the step S2 is 100-110 degree.
5. a kind of alkali etching ammonia water recovery system according to claim 1, it is characterised in that: stripping in the step S3
Equipment is provided with polyhedron baton round filler using supersaturated stripping tower setting, and in supersaturated stripping tower.
6. a kind of alkali etching ammonia water recovery system according to claim 1, it is characterised in that: stripping in the step S3
Equipment uses surface whole sealed set, and its ammonium hydroxide rate of discharge is lower than 15mg/L.
7. a kind of alkali etching ammonia water recovery system according to claim 1, it is characterised in that: pH value in the step S3
Regulator is arranged using milk of lime, and the milk of lime is stirred and is made using 80% amount of lime and 20% water.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910744018.5A CN110438507A (en) | 2019-08-13 | 2019-08-13 | A kind of alkali etching ammonia water recovery system |
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| CN201910744018.5A CN110438507A (en) | 2019-08-13 | 2019-08-13 | A kind of alkali etching ammonia water recovery system |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110723799A (en) * | 2019-11-18 | 2020-01-24 | 中核核电运行管理有限公司 | Nuclear power unit conventional island ammonia-containing wastewater collection and discharge device and method |
| CN110921695A (en) * | 2019-12-20 | 2020-03-27 | 广东臻鼎环境科技有限公司 | Method for recycling alkaline etching waste liquid |
| CN112274827A (en) * | 2020-11-11 | 2021-01-29 | 郭铁良 | Formula aqueous fire extinguisher is thrown to hand with passageway opens up function |
| CN118387894A (en) * | 2024-06-20 | 2024-07-26 | 昆山华拓环保科技有限公司 | Ammonia gas recovery processing device for alkaline etching solution copper extraction |
| CN118387894B (en) * | 2024-06-20 | 2024-10-29 | 昆山华拓环保科技有限公司 | Ammonia gas recovery processing device for alkaline etching solution copper extraction |
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| JPH02254188A (en) * | 1989-03-27 | 1990-10-12 | Kamioka Kogyo Kk | Method for electrolyzing copper chloride solution |
| CN102925704A (en) * | 2012-11-22 | 2013-02-13 | 上海绿澄环保科技有限公司 | Method and equipment for producing copper oxide and ammonia water by using alkaline copper etching liquid waste |
| CN103602988A (en) * | 2013-10-30 | 2014-02-26 | 中国科学院过程工程研究所 | Resourceful treatment and cyclic utilization method of PCB circuit board waste etching liquid |
| CN105859028A (en) * | 2016-04-29 | 2016-08-17 | 红板（江西）有限公司 | Process for treating circuit board alkaline etching ammonia-nitrogen wastewater |
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2019
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|---|---|---|---|---|
| JPH02254188A (en) * | 1989-03-27 | 1990-10-12 | Kamioka Kogyo Kk | Method for electrolyzing copper chloride solution |
| CN102925704A (en) * | 2012-11-22 | 2013-02-13 | 上海绿澄环保科技有限公司 | Method and equipment for producing copper oxide and ammonia water by using alkaline copper etching liquid waste |
| CN103602988A (en) * | 2013-10-30 | 2014-02-26 | 中国科学院过程工程研究所 | Resourceful treatment and cyclic utilization method of PCB circuit board waste etching liquid |
| CN105859028A (en) * | 2016-04-29 | 2016-08-17 | 红板（江西）有限公司 | Process for treating circuit board alkaline etching ammonia-nitrogen wastewater |
Non-Patent Citations (1)
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| 张乐红等: "过饱和吹脱塔处理铍冶炼高浓度氨氮废水的工长实践研究", 《湖南有色金属》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110723799A (en) * | 2019-11-18 | 2020-01-24 | 中核核电运行管理有限公司 | Nuclear power unit conventional island ammonia-containing wastewater collection and discharge device and method |
| CN110921695A (en) * | 2019-12-20 | 2020-03-27 | 广东臻鼎环境科技有限公司 | Method for recycling alkaline etching waste liquid |
| CN110921695B (en) * | 2019-12-20 | 2023-02-03 | 广东臻鼎环境科技有限公司 | Method for recycling alkaline etching waste liquid |
| CN112274827A (en) * | 2020-11-11 | 2021-01-29 | 郭铁良 | Formula aqueous fire extinguisher is thrown to hand with passageway opens up function |
| CN118387894A (en) * | 2024-06-20 | 2024-07-26 | 昆山华拓环保科技有限公司 | Ammonia gas recovery processing device for alkaline etching solution copper extraction |
| CN118387894B (en) * | 2024-06-20 | 2024-10-29 | 昆山华拓环保科技有限公司 | Ammonia gas recovery processing device for alkaline etching solution copper extraction |
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Application publication date: 20191112 |