CN110408937A - A kind of alkali etching recovery ammonia utilizes system - Google Patents
A kind of alkali etching recovery ammonia utilizes system Download PDFInfo
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- CN110408937A CN110408937A CN201910743936.6A CN201910743936A CN110408937A CN 110408937 A CN110408937 A CN 110408937A CN 201910743936 A CN201910743936 A CN 201910743936A CN 110408937 A CN110408937 A CN 110408937A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/10—Sulfates
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- 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
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Removal Of Specific Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention provides a kind of alkali etching recovery ammonia and utilizes system, the sulfuric acid solution of various concentration is added in three containers respectively as stripping agent, in the case where reaction temperature is 10-60 degree, reaction is carried out to the alkali phase solution that various concentration sulfuric acid solution is added respectively and generates copper-bath, it is cooling that the copper-bath of generation is subjected to room temperature, the solution containing crystal copper sulphate is prepared, ammonia and ammonium chloride are added inside to reaction kettle, reaction temperature heating is stirred, alkaline etching liquid is prepared.Alkaline etching liquid is divided into water phase by using the mode of extraction and mutually carries out separating processing with alkali by the present invention, using water phase as while the regenerated resources of new etching solution, aqueous slkali is passed through to the effect of Extraction and back extraction, copper resource therein is recycled, and by whole spent solution regenerations in removal process, non-wastewater discharge has reached the recycling and recycling of resource, achieve the purpose that saving, realizes and reduce energy consumption.
Description
Technical field
The present invention relates to alkaline etching liquid recycling fields more particularly to a kind of alkali etching recovery ammonia to utilize system.
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, serious harm can be brought to environment.In PCB Production, need to carry out circular regeneration to etching waste liquor,
Reach and makes 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, invent a kind of alkali etching recovery ammonia solved the above problems using system it is necessary
Summary of the invention
The purpose of the present invention is to provide a kind of alkali etching recovery ammonias to utilize system, 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 recovery ammonia utilizes system, comprising the following steps:
S1: choose copper content be 120-180g/L alkaline etching liquid, be added into extraction tank, and be added extractant into
Row stirring, and internal addition separatory funnel take out the water phase and alkali phase in separatory funnel after stratification respectively, spare,
It is as follows in its chemical reaction equation:
S2: the alkali phase solution being prepared in step S1 is respectively put into identical container according to identical percentage,
The sulfuric acid solution of addition various concentration is as stripping agent in three containers respectively, in the case where reaction temperature is 10-60 degree,
Reaction is carried out to the alkali phase solution that various concentration sulfuric acid solution is added respectively and generates copper-bath, by the copper-bath of generation
It is cooling to carry out room temperature, the solution containing crystal copper sulphate is prepared；
S3: by the solution containing crystal copper sulphate being prepared in step S2 using after filter press filters pressing, crystal is obtained
Copper sulphate and copper content are higher than the alkali phase solution of 0.2g/L and a large amount of ammonium chloride compounds, crystal copper sulphate are collected, so
The alkali phase solution that will be above 0.2g/L and a large amount of ammonium chloride compounds afterwards continues to extract repeatedly by the way of step S1 and step S2
It takes 2-3 times, crystal copper sulphate is prepared and copper content is lower than the alkali phase solution of 0.2g/L；
S4: the copper content being prepared in the water phase being prepared in step S1 and step S3 is lower than to the alkali of 0.2g/L
Phase solution is sequentially added to being mixed inside reaction kettle, and to ammonia and ammonium chloride is added inside reaction kettle, by reaction temperature
It is heated to 35-45 degree, is stirred, is reacted 2-3 hours, the alkaline etching liquid that pH value is 8.2-8.5, chemistry is prepared
It is as follows in reactional equation:
CuCl2+2NH4Cl+2NH3=[Cu (NH3)4]Cl2+3H2O
+nNH4Cl+nNH3
CuCl22H2O+4NH4OH=[Cu (NH3)4]Cl2+6H2O。
Preferably, extractant is hydrophobicity beta-diketon kind of extractants, concentration 100mol/L in the step S1.
Preferably, the concentration of sulfuric acid solution stripping agent is respectively 2mol/L, 3mol/L and 4mol/L in the step S2,
Its reaction temperature uses 10,25,40 and 60 to compare setting for reaction temperature.
Preferably, it is stripped, or is used in different temperatures using the stripping agent of identical solubility in the step S2
It is stripped at the same temperature using the stripping agent of different solubility.
The beneficial effects of the present invention are:
(1) alkaline etching liquid is divided into water phase by using the mode of extraction and mutually carries out separating processing with alkali by the present invention, will
While regenerated resources of the water phase as new etching solution, aqueous slkali is passed through to the effect of Extraction and back extraction, by copper resource therein
It is recycled, and by whole spent solution regenerations in removal process, non-wastewater discharge, the recycling for having reached resource and circulation are again
It makes profits use, achievees the purpose that saving, realize and reduce energy consumption.
Detailed description of the invention
Fig. 1 is that the stripping agent of different solubility at the identical temperature invented extracts schematic diagram to copper；
Fig. 2 is that the extractant of the identical solubility of invention extracts schematic diagram to copper in different temperatures.
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 recovery ammonias as shown in Figs. 1-2 to utilize system, comprising the following steps:
S1: the alkaline etching liquid that copper content is 120-180g/L is chosen, is added into extraction tank, and concentration is added and is
100mol/L hydrophobicity beta-diketon kind of extractants is stirred, and the internal separatory funnel that is added takes respectively after stratification
Water phase in separatory funnel and alkali phase out, it is spare, as follows in chemical reaction equation:
S2: the alkali phase solution being prepared in step S1 is respectively put into identical container according to identical percentage,
The sulfuric acid solution of 2mol/L, 3mol/L and 4mol/L is added in three containers respectively as stripping agent, is 10 in reaction temperature
In the case where degree, reaction is carried out to the alkali phase solution that various concentration sulfuric acid solution is added respectively and generates copper-bath, will be generated
Copper-bath to carry out room temperature cooling, the solution containing crystal copper sulphate is prepared；
S3: by the solution containing crystal copper sulphate being prepared in step S2 using after filter press filters pressing, crystal is obtained
Copper sulphate and copper content are higher than the alkali phase solution of 0.2g/L and a large amount of ammonium chloride compounds, crystal copper sulphate are collected, so
The alkali phase solution that will be above 0.2g/L and a large amount of ammonium chloride compounds afterwards continues to extract repeatedly by the way of step S1 and step S2
It takes 2-3 times, crystal copper sulphate is prepared and copper content is lower than the alkali phase solution of 0.2g/L；
S4: the copper content being prepared in the water phase being prepared in step S1 and step S3 is lower than to the alkali of 0.2g/L
Phase solution is sequentially added to being mixed inside reaction kettle, and to ammonia and ammonium chloride is added inside reaction kettle, by reaction temperature
It is heated to 35-45 degree, is stirred, is reacted 2-3 hours, the alkaline etching liquid that pH value is 8.2-8.5, chemistry is prepared
It is as follows in reactional equation:
CuCl2+2NH4Cl+2NH3=[Cu (NH3)4]Cl2+3H2O
+nNH4Cl+nNH3
CuCl22H2O+4NH4OH=[Cu (NH3)4]Cl2+6H2O。
Embodiment two:
The present invention provides a kind of alkali etching recovery ammonias to utilize system, comprising the following steps:
S1: the alkaline etching liquid that copper content is 120-180g/L is chosen, is added into extraction tank, and concentration is added and is
100mol/L hydrophobicity beta-diketon kind of extractants is stirred, and the internal separatory funnel that is added takes respectively after stratification
Water phase in separatory funnel and alkali phase out, it is spare, as follows in chemical reaction equation:
S2: the alkali phase solution being prepared in step S1 is respectively put into identical container according to identical percentage,
The sulfuric acid solution of 2mol/L, 3mol/L and 4mol/L is added in three containers respectively as stripping agent, is 25 in reaction temperature
In the case where degree, reaction is carried out to the alkali phase solution that various concentration sulfuric acid solution is added respectively and generates copper-bath, will be generated
Copper-bath to carry out room temperature cooling, the solution containing crystal copper sulphate is prepared；
S3: by the solution containing crystal copper sulphate being prepared in step S2 using after filter press filters pressing, crystal is obtained
Copper sulphate and copper content are higher than the alkali phase solution of 0.2g/L and a large amount of ammonium chloride compounds, crystal copper sulphate are collected, so
The alkali phase solution that will be above 0.2g/L and a large amount of ammonium chloride compounds afterwards continues to extract repeatedly by the way of step S1 and step S2
It takes 2-3 times, crystal copper sulphate is prepared and copper content is lower than the alkali phase solution of 0.2g/L；
S4: the copper content being prepared in the water phase being prepared in step S1 and step S3 is lower than to the alkali of 0.2g/L
Phase solution is sequentially added to being mixed inside reaction kettle, and to ammonia and ammonium chloride is added inside reaction kettle, by reaction temperature
It is heated to 35-45 degree, is stirred, is reacted 2-3 hours, the alkaline etching liquid that pH value is 8.2-8.5, chemistry is prepared
It is as follows in reactional equation:
CuCl2+2NH4Cl+2NH3=[Cu (NH3)4]Cl2+3H2O
+nNH4Cl+nNH3
CuCl22H2O+4NH4OH=[Cu (NH3)4]Cl2+6H2O。
Embodiment three:
The present invention provides a kind of alkali etching recovery ammonias to utilize system, comprising the following steps:
S1: the alkaline etching liquid that copper content is 120-180g/L is chosen, is added into extraction tank, and concentration is added and is
100mol/L hydrophobicity beta-diketon kind of extractants is stirred, and the internal separatory funnel that is added takes respectively after stratification
Water phase in separatory funnel and alkali phase out, it is spare, as follows in chemical reaction equation:
S2: the alkali phase solution being prepared in step S1 is respectively put into identical container according to identical percentage,
The sulfuric acid solution of 2mol/L, 3mol/L and 4mol/L is added in three containers respectively as stripping agent, is 40 in reaction temperature
In the case where degree, reaction is carried out to the alkali phase solution that various concentration sulfuric acid solution is added respectively and generates copper-bath, will be generated
Copper-bath to carry out room temperature cooling, the solution containing crystal copper sulphate is prepared；
S3: by the solution containing crystal copper sulphate being prepared in step S2 using after filter press filters pressing, crystal is obtained
Copper sulphate and copper content are higher than the alkali phase solution of 0.2g/L and a large amount of ammonium chloride compounds, crystal copper sulphate are collected, so
The alkali phase solution that will be above 0.2g/L and a large amount of ammonium chloride compounds afterwards continues to extract repeatedly by the way of step S1 and step S2
It takes 2-3 times, crystal copper sulphate is prepared and copper content is lower than the alkali phase solution of 0.2g/L；
S4: the copper content being prepared in the water phase being prepared in step S1 and step S3 is lower than to the alkali of 0.2g/L
Phase solution is sequentially added to being mixed inside reaction kettle, and to ammonia and ammonium chloride is added inside reaction kettle, by reaction temperature
It is heated to 35-45 degree, is stirred, is reacted 2-3 hours, the alkaline etching liquid that pH value is 8.2-8.5, chemistry is prepared
It is as follows in reactional equation:
CuCl2+2NH4Cl+2NH3=[Cu (NH3)4]Cl2+3H2O
+nNH4Cl+nNH3
CuCl22H2O+4NH4OH=[Cu (NH3)4]Cl2+6H2O。
Example IV:
The present invention provides a kind of alkali etching recovery ammonias to utilize system, comprising the following steps:
S1: the alkaline etching liquid that copper content is 120-180g/L is chosen, is added into extraction tank, and concentration is added and is
100mol/L hydrophobicity beta-diketon kind of extractants is stirred, and the internal separatory funnel that is added takes respectively after stratification
Water phase in separatory funnel and alkali phase out, it is spare, as follows in chemical reaction equation:
S2: the alkali phase solution being prepared in step S1 is respectively put into identical container according to identical percentage,
The sulfuric acid solution of 2mol/L, 3mol/L and 4mol/L is added in three containers respectively as stripping agent, is 60 in reaction temperature
In the case where degree, reaction is carried out to the alkali phase solution that various concentration sulfuric acid solution is added respectively and generates copper-bath, will be generated
Copper-bath to carry out room temperature cooling, the solution containing crystal copper sulphate is prepared；
S3: by the solution containing crystal copper sulphate being prepared in step S2 using after filter press filters pressing, crystal is obtained
Copper sulphate and copper content are higher than the alkali phase solution of 0.2g/L and a large amount of ammonium chloride compounds, crystal copper sulphate are collected, so
The alkali phase solution that will be above 0.2g/L and a large amount of ammonium chloride compounds afterwards continues to extract repeatedly by the way of step S1 and step S2
It takes 2-3 times, crystal copper sulphate is prepared and copper content is lower than the alkali phase solution of 0.2g/L；
S4: the copper content being prepared in the water phase being prepared in step S1 and step S3 is lower than to the alkali of 0.2g/L
Phase solution is sequentially added to being mixed inside reaction kettle, and to ammonia and ammonium chloride is added inside reaction kettle, by reaction temperature
It is heated to 35-45 degree, is stirred, is reacted 2-3 hours, the alkaline etching liquid that pH value is 8.2-8.5, chemistry is prepared
It is as follows in reactional equation:
CuCl2+2NH4Cl+2NH3=[Cu (NH3)4]Cl2+3H2O
+nNH4Cl+nNH3
CuCl22H2O+4NH4OH=[Cu (NH3)4]Cl2+6H2O。
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 (4)
1. a kind of alkali etching recovery ammonia utilizes system, it is characterised in that: the following steps are included:
S1: the alkaline etching liquid that copper content is 120-180g/L is chosen, is added into extraction tank, and extractant is added and is stirred
It mixes, and internal addition separatory funnel, after stratification, takes out the water phase and alkali phase in separatory funnel respectively, it is spare, change
It learns as follows in reactional equation:
S2: the alkali phase solution being prepared in step S1 is respectively put into identical container according to identical percentage, respectively
The sulfuric acid solution of various concentration is added in three containers as stripping agent, in the case where reaction temperature is 10-60 degree, respectively
Reaction is carried out to the alkali phase solution that various concentration sulfuric acid solution is added and generates copper-bath, the copper-bath of generation is carried out
Room temperature is cooling, and the solution containing crystal copper sulphate is prepared；
S3: by the solution containing crystal copper sulphate being prepared in step S2 using after filter press filters pressing, crystal sulfuric acid is obtained
Copper and copper content are higher than the alkali phase solution of 0.2g/L and a large amount of ammonium chloride compounds, and crystal copper sulphate is collected, and then will
Alkali phase solution higher than 0.2g/L and a large amount of ammonium chloride compounds continues to extract 2-3 repeatedly by the way of step S1 and step S2
Time, crystal copper sulphate is prepared and copper content is lower than the alkali phase solution of 0.2g/L；
S4: the copper content being prepared in the water phase being prepared in step S1 and step S3 is lower than to the alkali phase solution of 0.2g/L
It sequentially adds to being mixed inside reaction kettle, and to ammonia and ammonium chloride is added inside reaction kettle, reaction temperature is heated to
35-45 degree, is stirred, and reacts 2-3 hours, and the alkaline etching liquid that pH value is 8.2-8.5, chemical reaction equation is prepared
In it is as follows:
CuCl2+2NH4Cl+2NH3=[Cu (NH3)4]Cl2+3H2O+nNH4Cl+nNH3
CuCl22H2O+4NH4OH=[Cu (NH3)4]Cl2+6H2O。
2. a kind of alkali etching recovery ammonia according to claim 1 utilizes system, it is characterised in that: extract in the step S1
Taking agent is hydrophobicity beta-diketon kind of extractants, concentration 100mol/L.
3. a kind of alkali etching recovery ammonia according to claim 1 utilizes system, it is characterised in that: sulphur in the step S2
The concentration of acid solution stripping agent is respectively 2mol/L, 3mol/L and 4mol/L, and it is anti-that reaction temperature, which uses 10,25,40 and 60,
Temperature comparisons are answered to be arranged.
4. a kind of alkali etching recovery ammonia according to claim 1 utilizes system, it is characterised in that: adopted in the step S2
It is stripped with the stripping agent of identical solubility in different temperatures, or using the back extraction for using different solubility at the same temperature
Agent is stripped.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08311664A (en) * | 1995-05-12 | 1996-11-26 | Ain:Kk | Method for reutilizing waste liquid etchant |
| CN105002500A (en) * | 2015-07-17 | 2015-10-28 | 中南大学 | Alkaline CuC12 spent etching solution copper removal regeneration method |
| CN109319823A (en) * | 2017-07-31 | 2019-02-12 | 中国瑞林工程技术有限公司 | The method of Treatment of Copper etching waste liquor |
-
2019
- 2019-08-13 CN CN201910743936.6A patent/CN110408937A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08311664A (en) * | 1995-05-12 | 1996-11-26 | Ain:Kk | Method for reutilizing waste liquid etchant |
| CN105002500A (en) * | 2015-07-17 | 2015-10-28 | 中南大学 | Alkaline CuC12 spent etching solution copper removal regeneration method |
| CN109319823A (en) * | 2017-07-31 | 2019-02-12 | 中国瑞林工程技术有限公司 | The method of Treatment of Copper etching waste liquor |
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