CN108821492A - A kind of purification process technique of circuit board etching waste liquor - Google Patents
A kind of purification process technique of circuit board etching waste liquor Download PDFInfo
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- CN108821492A CN108821492A CN201810649840.9A CN201810649840A CN108821492A CN 108821492 A CN108821492 A CN 108821492A CN 201810649840 A CN201810649840 A CN 201810649840A CN 108821492 A CN108821492 A CN 108821492A
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- etching waste
- circuit board
- ammonia
- purification process
- liquid
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/026—Preparation of ammonia from inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/28—Chlorides by chlorination of alkaline-earth metal compounds
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- 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
Abstract
The invention discloses a kind of purification process techniques of circuit board etching waste liquor, the purification process technique uses solid-phase flow settling separation and ammonia nitrogen vapor absorption technology, this two technologies make the condensed water ammonia-nitrogen content of the generation after ammonia nitrogen waste liquid evaporation process lower than 10ppm, the ammonium chloride in waste liquid is changed into standard compliant ammonium hydroxide and calcium chloride product simultaneously, good economic benefit and environmental benefit are achieved, is had a vast market foreground.
Description
Technical field
The present invention relates to sewage treatment process field, in particular to a kind of purification process technique of circuit board etching waste liquor.
Background technique
As the continuous development of PCB industry is grown, the environmental issue of the sector is also become more and more important, wherein main
One of pollution is exactly a large amount of copper-containing etching waste solutions caused by etching work procedure.This waste liquid mainly comes from PCB etching work procedure,
Extra copper foil on etching solution energy open circuit potential plate, so that the copper ion concentration in etching solution constantly increases, when copper in etching solution
When the content of ion reaches a certain concentration, the efficiency of etching corrosion copper will be gradually reduced until failure, etches to become
Waste liquid and discharge.Etching waste liquor belongs to dangerous liquid waste, containing pollutant components such as a large amount of copper, ammonia nitrogen, chlorine, if without
Stringent processing is just directly discharged in environment, not only causes the waste and loss of resource, but also can be to the mankind and natural ring
Very big harm is caused in border, and the copper of trace can destroy bio-tissue, and excessive copper then can be carcinogenic
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of purification process techniques of circuit board etching waste liquor, to solve
The above-mentioned defects caused by the prior art.
To achieve the above object, the present invention provides technical solution below：A kind of purified treatment of circuit board etching waste liquor
Technique includes the following steps：
(1) neutralization reaction
Acidic etching waste liquid is added in alkaline etching waste liquid for producing first, adjusts the pH value of its mixed liquor, during the two occurs
And reaction, basic copper chloride precipitating is generated, the pH of the mixed liquor is 5-7；
(2) filters pressing separation and slurrying
Mixed liquor after neutralization reaction is separated by solid-liquid separation, liquid phase 1 is obtained, the basic copper chloride obtained after then reacting
In plus water slurrying, obtain basic copper chloride slurry, while also adding water to prepare lime white quick lime, it is spare；
(3) add alkali conversion process
Then lime white is added in basic copper chloride slurry, stirs to get mixture, the time of the stirring is 30-
50min；
(4) it is separated by solid-liquid separation and roasts
Mixture is separated by solid-liquid separation, liquid phase 2 is obtained, isolated solid phase is then sent into converter and is being roasted
It burns, obtains product of roasting, the temperature of the converter is 400-600 DEG C；
(5) dissolution and gravity separation
Water is added into above-mentioned product of roasting, and then wherein remaining chlorination calcium component is left away using separation by shaking table method
It removes, to obtain oxidation copper products；
(6) evaporating concentration process
Liquid phase 1 and liquid phase 2 are evaporated concentration together, the steam evaporated by acidic etching waste liquid absorb after again
It is absorbed with lime white, the vapor for removing ammonia nitrogen is condensed again；
(7) add quick lime ammonia still process
Add quick lime into concentrate, ammonia evaporates evolution in the form of a vapor, is then separated by solid-liquid separation, described
P H value after adding quick lime is 12-14；
(8) absorption process of ammonia
The ammonia of generation is fully incorporated in absorption tower, is absorbed with water spray, ammonium hydroxide product is obtained.
Preferably, the time roasted in the step (4) is 30-50min.
Preferably, the purity of oxidation copper products is 97-99% in the step (5).
Preferably, the time condensed in the step (6) is 50-70min.
Preferably, the temperature of ammonia still process is 140-160 DEG C in the step (7).
Preferably, spray is that three-level sprays in the step (8).
It is using the beneficial effect of above technical scheme：A kind of purified treatment work of circuit board etching waste liquor of the invention
Skill, the purification process technique use solid-phase flow settling separation and ammonia nitrogen vapor absorption technology, this two technologies make ammonia
The condensed water ammonia-nitrogen content of generation after nitrogen waste liquid evaporation process is lower than 10ppm, while the ammonium chloride in waste liquid is changed into symbol
The ammonium hydroxide and calcium chloride product of standardization, achieve good economic benefit and environmental benefit, have a vast market foreground.
Specific embodiment
Below with reference to embodiment detailed description of the preferred embodiments of the present invention.
Embodiment 1：
A kind of purification process technique of circuit board etching waste liquor, includes the following steps：
(1) neutralization reaction
Acidic etching waste liquid is added in alkaline etching waste liquid for producing first, adjusts the pH value of its mixed liquor, during the two occurs
And reaction, basic copper chloride precipitating is generated, the pH of the mixed liquor is 5；
(2) filters pressing separation and slurrying
Mixed liquor after neutralization reaction is separated by solid-liquid separation, liquid phase 1 is obtained, the basic copper chloride obtained after then reacting
In plus water slurrying, obtain basic copper chloride slurry, while also adding water to prepare lime white quick lime, it is spare；
(3) add alkali conversion process
Then lime white is added in basic copper chloride slurry, stirs to get mixture, the time of the stirring is
30min；
(4) it is separated by solid-liquid separation and roasts
Mixture is separated by solid-liquid separation, liquid phase 2 is obtained, isolated solid phase is then sent into converter and is being roasted
It burns, obtains product of roasting, the temperature of the converter is 400 DEG C, and the time of the roasting is 30min；
(5) dissolution and gravity separation
Water is added into above-mentioned product of roasting, and then wherein remaining chlorination calcium component is left away using separation by shaking table method
It removes, to obtain oxidation copper products, the purity of the oxidation copper products is 97%；
(6) evaporating concentration process
Liquid phase 1 and liquid phase 2 are evaporated concentration together, the steam evaporated by acidic etching waste liquid absorb after again
It is absorbed with lime white, the vapor for removing ammonia nitrogen is condensed again, and the time of the condensation is 50min；
(7) add quick lime ammonia still process
Add quick lime into concentrate, ammonia evaporates evolution in the form of a vapor, is then separated by solid-liquid separation, described
P H value after adding quick lime is 12, and the temperature of the ammonia still process is 140 DEG C；
(8) absorption process of ammonia
The ammonia of generation is fully incorporated in absorption tower, is absorbed with water spray, ammonium hydroxide product is obtained, the spray is three-level
Spray.
Embodiment 2：
A kind of purification process technique of circuit board etching waste liquor, includes the following steps：
(1) neutralization reaction
Acidic etching waste liquid is added in alkaline etching waste liquid for producing first, adjusts the pH value of its mixed liquor, during the two occurs
And reaction, basic copper chloride precipitating is generated, the pH of the mixed liquor is 6；
(2) filters pressing separation and slurrying
Mixed liquor after neutralization reaction is separated by solid-liquid separation, liquid phase 1 is obtained, the basic copper chloride obtained after then reacting
In plus water slurrying, obtain basic copper chloride slurry, while also adding water to prepare lime white quick lime, it is spare；
(3) add alkali conversion process
Then lime white is added in basic copper chloride slurry, stirs to get mixture, the time of the stirring is
40min；
(4) it is separated by solid-liquid separation and roasts
Mixture is separated by solid-liquid separation, liquid phase 2 is obtained, isolated solid phase is then sent into converter and is being roasted
It burns, obtains product of roasting, the temperature of the converter is 500 DEG C, and the time of the roasting is 40min；
(5) dissolution and gravity separation
Water is added into above-mentioned product of roasting, and then wherein remaining chlorination calcium component is left away using separation by shaking table method
It removes, to obtain oxidation copper products, the purity of the oxidation copper products is 98%；
(6) evaporating concentration process is evaporated concentration, the steam evaporated by acidic etching waste liquid absorb after again
Liquid phase 1 and liquid phase 2 are reinstated lime white to absorb, the vapor for removing ammonia nitrogen is condensed again, the condensation
Time is 60min；
(7) add quick lime ammonia still process
Add quick lime into concentrate, ammonia evaporates evolution in the form of a vapor, is then separated by solid-liquid separation, described
P H value after adding quick lime is 13, and the temperature of the ammonia still process is 150 DEG C；
(8) absorption process of ammonia
The ammonia of generation is fully incorporated in absorption tower, is absorbed with water spray, ammonium hydroxide product is obtained, the spray is three-level
Spray.
Embodiment 3：
A kind of purification process technique of circuit board etching waste liquor, includes the following steps：
(1) neutralization reaction
Acidic etching waste liquid is added in alkaline etching waste liquid for producing first, adjusts the pH value of its mixed liquor, during the two occurs
And reaction, basic copper chloride precipitating is generated, the pH of the mixed liquor is 7；
(2) filters pressing separation and slurrying
Mixed liquor after neutralization reaction is separated by solid-liquid separation, liquid phase 1 is obtained, the basic copper chloride obtained after then reacting
In plus water slurrying, obtain basic copper chloride slurry, while also adding water to prepare lime white quick lime, it is spare；
(3) add alkali conversion process
Then lime white is added in basic copper chloride slurry, stirs to get mixture, the time of the stirring is
50min；
(4) it is separated by solid-liquid separation and roasts
Mixture is separated by solid-liquid separation, liquid phase 2 is obtained, isolated solid phase is then sent into converter and is being roasted
It burns, obtains product of roasting, the temperature of the converter is 600 DEG C, and the time of the roasting is 50min；
(5) dissolution and gravity separation
Water is added into above-mentioned product of roasting, and then wherein remaining chlorination calcium component is left away using separation by shaking table method
It removes, to obtain oxidation copper products, the purity of the oxidation copper products is 99%；
(6) evaporating concentration process
Liquid phase 1 and liquid phase 2 are evaporated concentration together, the steam evaporated by acidic etching waste liquid absorb after again
It is absorbed with lime white, the vapor for removing ammonia nitrogen is condensed again, and the time of the condensation is 70min；
(7) add quick lime ammonia still process
Add quick lime into concentrate, ammonia evaporates evolution in the form of a vapor, is then separated by solid-liquid separation, described
P H value after adding quick lime is 14, and the temperature of the ammonia still process is 160 DEG C；
(8) absorption process of ammonia
The ammonia of generation is fully incorporated in absorption tower, is absorbed with water spray, ammonium hydroxide product is obtained, the spray is three-level
Spray.
After above method, sample is taken out respectively, and measurement result is as follows：
According to above table data, it can be concluded that, when the parameter of embodiment 2, the rate of recovery and processing cost reduced rate are high,
Economic benefit and environmental benefit are good, are more advantageous to the purified treatment of circuit board etching waste liquor at this time.
The present invention provides a kind of purification process technique of circuit board etching waste liquor, which is flowed using solid phase
Sedimentation-separation technology and ammonia nitrogen vapor absorption technology, this two technologies make the condensed water of the generation after ammonia nitrogen waste liquid evaporation process
Ammonia-nitrogen content is lower than 10ppm, while the ammonium chloride in waste liquid is changed into standard compliant ammonium hydroxide and calcium chloride product, achieves
Good economic benefit and environmental benefit, have a vast market foreground.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention
Protection scope.
Claims (6)
1. a kind of purification process technique of circuit board etching waste liquor, which is characterized in that include the following steps：
(1) neutralization reaction
Acidic etching waste liquid is added in alkaline etching waste liquid for producing first, adjusts the pH value of its mixed liquor, the two occurs to neutralize anti-
It answers, generates basic copper chloride precipitating, the pH of the mixed liquor is 5-7；
(2) filters pressing separation and slurrying
Mixed liquor after neutralization reaction is separated by solid-liquid separation, liquid phase 1 is obtained, is added in the basic copper chloride obtained after then reacting
Water slurrying obtains basic copper chloride slurry, while also adding water to prepare lime white quick lime, spare；
(3) add alkali conversion process
Then lime white is added in basic copper chloride slurry, stirs to get mixture, the time of the stirring is 30-50min；
(4) it is separated by solid-liquid separation and roasts
Mixture is separated by solid-liquid separation, liquid phase 2 is obtained, isolated solid phase is then sent into converter and is being roasted, is obtained
To product of roasting, the temperature of the converter is 400-600 DEG C；
(5) dissolution and gravity separation
Water is added into above-mentioned product of roasting, and then wherein remaining chlorination calcium component is left away using separation by shaking table method and is removed, from
And obtain oxidation copper products；
(6) evaporating concentration process
Liquid phase 1 and liquid phase 2 are evaporated concentration together, the steam evaporated uses stone after absorbing by acidic etching waste liquid again
Mortar absorbs, and the vapor for removing ammonia nitrogen is condensed again；
(7) add quick lime ammonia still process
Into concentrate plus quick lime, ammonia evaporate evolution in the form of a vapor, are then separated by solid-liquid separation, described plus life
P H value after lime is 12-14；
(8) absorption process of ammonia
The ammonia of generation is fully incorporated in absorption tower, is absorbed with water spray, ammonium hydroxide product is obtained.
2. a kind of purification process technique of circuit board etching waste liquor according to claim 1, which is characterized in that the step
(4) time roasted in is 30-50min.
3. a kind of purification process technique of circuit board etching waste liquor according to claim 1, which is characterized in that the step
(5) purity of oxidation copper products is 97-99% in.
4. a kind of purification process technique of circuit board etching waste liquor according to claim 1, which is characterized in that the step
(6) time condensed in is 50-70min.
5. a kind of purification process technique of circuit board etching waste liquor according to claim 1, which is characterized in that the step
(7) temperature of ammonia still process is 140-160 DEG C in.
6. a kind of purification process technique of circuit board etching waste liquor according to claim 1, which is characterized in that the step
(8) spray is that three-level sprays in.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810649840.9A CN108821492A (en) | 2018-06-22 | 2018-06-22 | A kind of purification process technique of circuit board etching waste liquor |
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| CN201810649840.9A CN108821492A (en) | 2018-06-22 | 2018-06-22 | A kind of purification process technique of circuit board etching waste liquor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112011781A (en) * | 2019-05-30 | 2020-12-01 | 上海名古屋精密工具股份有限公司 | Process for wet etching of binder phase and method for recovering waste liquid thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654275A (en) * | 2009-08-21 | 2010-02-24 | 广州市白云区南溪化工厂 | Comprehensive utilization method of acidic and alkaline waste etching solution |
| CN103466683A (en) * | 2013-09-12 | 2013-12-25 | 昆山德阳新材料科技有限公司 | Preparation method of high-purity electroplating-grade copper oxide |
-
2018
- 2018-06-22 CN CN201810649840.9A patent/CN108821492A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654275A (en) * | 2009-08-21 | 2010-02-24 | 广州市白云区南溪化工厂 | Comprehensive utilization method of acidic and alkaline waste etching solution |
| CN103466683A (en) * | 2013-09-12 | 2013-12-25 | 昆山德阳新材料科技有限公司 | Preparation method of high-purity electroplating-grade copper oxide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112011781A (en) * | 2019-05-30 | 2020-12-01 | 上海名古屋精密工具股份有限公司 | Process for wet etching of binder phase and method for recovering waste liquid thereof |
| WO2020238342A1 (en) * | 2019-05-30 | 2020-12-03 | 上海名古屋精密工具股份有限公司 | Process for wet etching binding phase and method for recovering waste liquid therefrom |
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