CN111499029B - Two-stage method for quickly removing copper ions in copper ammonia complexing wastewater - Google Patents
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Abstract
The invention relates to a two-stage method for quickly removing copper ions in copper ammonia complexing wastewater. The method comprises the following steps: the method comprises the steps of adding alkali into copper ammonia complexing wastewater, adjusting the pH value of the wastewater to a proper value, performing one-section complex breaking precipitation, and removing part of copper, wherein the chemical reaction formula is as follows:
secondly, adding hydroxamic acid type separating agent into the obtained copper-containing suspension, uniformly mixing, standing, and carrying out two-stage deep chelation copper removal and flocculation sedimentation separation; a chelation reaction formula: [ Cu (NH)3)4]2++RCONHO‑→RCONHOCu↓+NH3·H2OCu(OH)2+RCONHO‑→RCONHO‑Cu(OH)2↓; thirdly, the settled bottom flow is high-content copper sludge, and the high-purity copper hydroxide powder is formed after the bottom flow is taken out and dehydrated and dried; and overflowing the filtrate and the supernatant into a subsequent deamination system.
Description
Technical Field
The invention belongs to the field of sewage treatment, relates to a method for quickly removing copper ions in copper ammonia complex wastewater, and particularly relates to a method for quickly removing copper ions in copper ammonia cleaning wastewater produced in an alkaline etching process of a printed circuit board and recovering copper resources.
Background
Alkaline etching is a commonly adopted process in Printed Circuit Board (PCB) production, and a large amount of alkaline washing water containing copper-ammonia complex and free ammonia is generated in the subsequent cleaning process, and accounts for about 3-5% of the total amount of waste water generated by PCB. The wastewater is dark blue, the pH value is about 8.5-9.5, the copper ion content is 100-1000 mg/L, the ammonia nitrogen content is 500-5000 mg/L, and the wastewater has great harm to water environment and human body and needs to be effectively treated.
The free copper-containing wastewater is easier to remove by a common chemical precipitation method, but the copper ammonia wastewater mainly containing low-concentration complex copper and medium-concentration ammonia nitrogen is difficult to treat by a conventional method, and is generally removed by adding agents such as sodium sulfide, ferrous sulfate, PAC (polyaluminium chloride), PAM (polyacrylamide) and the like after being mixed and diluted with a large amount of other types of wastewater for precipitation. In order to reduce the copper ion residue in the wastewater and improve the flocculation sedimentation performance of the precipitated particle slurry, excessive sodium sulfide and ferrous sulfate are added, and a large amount of medicament is consumed in repeatedly adjusting the pH value of the wastewater, so that a large amount of dangerous waste sludge with more impurities and lower copper content (about 3-5%) is generated, and the dangerous waste sludge still needs to be handed over to an enterprise with related qualification for special treatment, thereby increasing the wastewater treatment cost, and causing the waste of copper resources and potential risks of subsequent treatment. Meanwhile, the whole ammonia nitrogen content of the wastewater after dilution and mixing treatment is still high, and the wastewater is difficult to be effectively treated by the existing biochemical facilities, so that great burden and pressure are caused to final water drainage of a plant area.
Therefore, the property characteristics of the copper ammonia complex wastewater are fully utilized, based on the copper ammonia complex reaction-chemical equilibrium theory, the copper ion pollution is removed in a proper mode, the copper ion pollution is recovered in a copper-containing byproduct form, favorable conditions are created for subsequent ammonia nitrogen treatment, and the method is very necessary and valuable. Meanwhile, because the hydroxamic acid functional group (R-CONHOH) has stronger chelating adsorption capacity on transition metals (such as copper and iron elements) and rare earth elements, the hydroxamic acid type reagent is commonly used as a collector for rare earth mineral flotation and a flocculating agent for red mud sedimentation in alumina production, but the hydroxamic acid type separating reagent is not reported to be used for copper ammonia wastewater treatment.
Disclosure of Invention
The invention aims to solve the problems that the removal of complex copper in the cleaning wastewater after the existing PCB alkaline etching is difficult, the treatment cost is high, the copper resource cannot be effectively recycled and the like, and provides a two-stage method for quickly removing the copper ions in the copper ammonia complex wastewater, which can realize the decomplexation of the copper ammonia complex ions in the wastewater and the quick precipitation removal of the copper ions by controlling the pH value of the wastewater and adding a hydroxamic acid type separating agent and can recover the copper resource in the wastewater in the form of high-purity copper hydroxide.
The technical scheme of the invention is that the two-stage method for rapidly removing the copper ions in the copper ammonia complexing wastewater is characterized by comprising a first-stage alkaline decomplexation precipitation and a second-stage deep chelation-flocculation; the method comprises the following steps:
the method comprises the steps of carrying out alkali regulation on copper-ammonia complex ions by utilizing the difference of chemical reaction equilibrium constants according to the concentrations of copper and ammonia nitrogen in wastewater, and controlling the degree of reaction crystallization to form copper hydroxide fine particles;
and secondly, adding a hydroxamic acid type separating agent, and quickly separating and removing the hydroxamic acid type separating agent by a two-stage deep chelation-flocculation method.
Preferably, the method comprises the following steps: the alkali used for adjusting the alkali is one or more of sodium hydroxide, potassium hydroxide and calcium hydroxide, and preferably sodium hydroxide; the pH value of the copper ammonia wastewater is adjusted to be more than 10, and preferably is 11-13.
Preferably, the method comprises the following steps: the step includes: adding 200g/L of alkali into the cuprammonia complexing wastewater, adjusting the pH value of the wastewater to 11.80-12.10, performing first-stage complex breaking precipitation to remove part of copper, wherein the chemical reaction formula is as follows:
preferably, the method comprises the following steps: the step includes: and (3) removing copper from the industrial copper ammonia wastewater by adopting a continuous precipitation tank: gradually adding 35% sodium hydroxide solution into the reaction tank under mechanical stirring, controlling the pH value of the wastewater to be 11.80-11.95, and keeping the time for 60 min.
Preferably, the method comprises the following steps: the hydroxamic acid type separating agent is characterized in that the hydroxamic acid type separating agent is an organic high-molecular polymer containing hydroxamic acid functional groups, the content of the hydroxamic acid functional groups is 5-30%, and the molecular weight is larger than 100 ten thousand; the dosage is 0.1-0.001%, preferably 0.02-0.002% of the total amount of the wastewater.
Preferably, the method comprises the following steps: the step further includes: gradually adding 30mg/L hydroxamic acid type separating agent solution into the coagulation tank, and keeping the time for 20 min; then the wastewater enters a settling separation tank and stays for 60min to 100 min; the residual solid content in the overflow of the settling separation tank is 2.4 mg/L-5.8 mg/L, the copper content in the filtered water sample is 3.6 mg/L-6.9 mg/L, and the copper removal rate is 99.1-99.3%.
Preferably, the method comprises the following steps: the step further includes: adding hydroxamic acid type separating agent into the obtained copper-containing suspension, uniformly mixing, standing, and performing two-stage deep chelation copper removal and flocculation settling separation;
the chelation reaction formula is as follows:
[Cu(NH3)4]2++RCONHO-→RCONHOCu↓+NH3·H2O
Cu(OH)2+RCONHO-→RCONHO-Cu(OH)2↓。
preferably, the method comprises the following steps: further comprising the steps of: the settled underflow is copper-containing slurry, the solid content of the underflow is higher than 5% before dehydration, the underflow is taken out and dehydrated and dried to form copper hydroxide powder with the purity of more than 95% and the copper content of more than 63%, and the copper hydroxide powder is used as a raw material of a related copper-containing reagent and preferably used as an agricultural copper hydroxide bactericide; and overflowing the filtrate and the supernatant into a subsequent deamination system.
Preferably, the method comprises the following steps: the treated copper ammonia wastewater is cleaning wastewater after printed circuit alkaline etching, and comprises copper ammonia complex and free ammonia; the treated overflow and filtrate are ammonia nitrogen wastewater after copper removal, and directly enter ammonia nitrogen treatment systems such as stripping and membrane separation, or enter a biochemical treatment system after dilution, preferably directly enter the ammonia nitrogen membrane separation system.
Preferably, the method comprises the following steps: the solid content of copper-containing slurry obtained after copper deposition treatment of copper ammonia wastewater is 80-210 g/L, after filtration, washing and drying, the average particle size is 1.85-2.32 μm through laser particle size analysis, the copper-containing slurry is crystalline copper hydroxide through X-ray diffraction analysis, and the content of the copper hydroxide is 98.3-99.1% through fluorescence spectrum analysis.
The other technical scheme of the invention is that the two-stage method for quickly removing the copper ions in the copper ammonia complexing wastewater is characterized by comprising the following steps:
(1) adding 10-40% alkali into the cuprammonia complexing wastewater to adjust the wastewater to a proper pH value, carrying out first-stage complex breaking precipitation to remove part of copper, wherein the chemical reaction formula is as follows:
(2) adding hydroxamic acid type separating agent accounting for 0.1-0.001% of the total amount of the wastewater into the obtained copper-containing suspension, uniformly mixing, standing, and performing two-stage deep chelation copper removal and flocculation sedimentation separation;
the chelation reaction formula is as follows:
[Cu(NH3)4]2++RCONHO-→RCONHOCu↓+NH3·H2O
Cu(OH)2+RCONHO-→RCONHO-Cu(OH)2↓
the flocculation mechanism is as follows:
(3) taking out the settled bottom flow which is the copper-containing slurry, and dehydrating and drying the bottom flow to form copper hydroxide powder; and overflowing the filtrate and the supernatant into a subsequent deamination system.
Compared with the prior art, the invention has the beneficial effects that:
the method is simple, high in copper removal rate and low in comprehensive cost, and can promote subsequent ammonia nitrogen treatment.
The invention only adds alkali and hydroxamic acid type separating agents on the basis that the wastewater is alkaline, and can avoid the problems of easy residue of agents, poor water quality, poor precipitation effect, excessive sludge and the like caused by adding ferrous sulfate, sodium sulfide, conventional flocculating agents, repeatedly adjusting pH and the like in the conventional treatment method.
The byproduct of the method is the copper hydroxide particles, so that the purity is high, the dispersibility is good, and the additional value is high.
The method is beneficial to subsequent treatment of ammonia nitrogen pollutants, and can be used as a key basic link for cooperative treatment of the copper ammonia wastewater.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention;
FIG. 2 is a schematic illustration of the flocculation mechanism of the present invention;
FIG. 3 is a schematic representation of the results of XRD of a by-product of the present invention;
FIG. 4 is a photograph of a sample of the by-product copper hydroxide recovered by the present invention.
Detailed Description
The invention will be further described in detail with reference to the following examples:
the two-stage method for quickly removing the copper ions in the copper ammonia complexing wastewater is characterized by comprising the following steps of:
the method comprises the steps of adding alkali into copper ammonia complexing wastewater, adjusting the pH value of the wastewater to a proper value, performing one-section complex breaking precipitation, and removing part of copper, wherein the chemical reaction formula is as follows:
adding hydroxamic acid type separating agent into the obtained copper-containing suspension, uniformly mixing, standing, and performing two-stage deep chelation copper removal and flocculation sedimentation separation.
The chelation reaction formula is as follows:
[Cu(NH3)4]2++RCONHO-→RCONHOCu↓+NH3·H2O
Cu(OH)2+RCONHO-→RCONHO-Cu(OH)2↓
the flocculation mechanism is shown in figure 2;
(3) and taking out the settled underflow, namely the copper-containing slurry, and dehydrating and drying the underflow to form copper hydroxide powder. And overflowing the filtrate and the supernatant into a subsequent deamination system.
The cuprammonium wastewater used in examples 1-3 was a self-made cuprammonium solution, and the components are shown in table 1; the cuprammonium waste water used in examples 4-6 is cuprammonium cleaning waste water generated in the alkaline etching process in the actual production of Shenzhen electronic factory, and the composition is shown in Table 2.
TABLE 1 self-made cuprammonium solution composition
| Composition (I) | Cu2+ | NH4-N | Cl- | pH |
| Content mg/L | 201.4 | 1422.0 | 240.0 | 8.90 |
TABLE 2 composition of waste water containing copper and ammonia from alkaline etching line of PCB manufacturer
| Composition (I) | Cu2+ | NH4-N | Cl- | pH |
| Content mg/L | 507.5 | 1980.0 | 3100.0 | 9.15 |
Example 1
Referring to fig. 1, sodium hydroxide solution (200g/L) is added dropwise into the self-made copper ammonia wastewater, the pH value of the wastewater is adjusted to 11.80, 50mg/L hydroxamic acid type separating agent solution is added after stirring reaction for 30min, and standing and settling are carried out for 15 min. The residual solid content of the supernatant is 3.5mg/L, the copper content in the filtered water sample is 1.6mg/L, and the copper removal rate is 99.2%.
Example 2
Referring to fig. 1, sodium hydroxide solution (200g/L) is added dropwise into the self-made copper ammonia wastewater, the pH value of the wastewater is adjusted to 12.10, 80mg/L hydroxamic acid type separating agent solution is added after stirring reaction for 30min, and standing and settling are carried out for 15 min. The residual solid content of the supernatant is 2.7mg/L, the copper content in the filtered water sample is 1.1mg/L, and the copper removal rate is 99.4%.
Example 3
Referring to fig. 1, the copper-containing slurry obtained by copper deposition of the self-made cuprammonium wastewater contains about 80g/L of solid, and after filtering, washing and drying, the average particle size is 2.32 μm as shown by laser particle size analysis, and the copper-containing slurry is crystalline copper hydroxide as shown in fig. 4 as shown by X-ray diffraction analysis, and the content of the copper hydroxide is 99.1% as shown by fluorescence spectrum analysis.
Example 4
Referring to fig. 1, a continuous precipitation tank is used for removing copper from industrial cuprammonia wastewater. Gradually adding 35% sodium hydroxide solution into the reaction tank under mechanical stirring, controlling the pH value of the wastewater to be 11.80, and keeping the time for about 60 min; gradually adding hydroxamic acid type separating agent solution into the coagulation tank, wherein the dosage is about 30mg/L, and the retention time is 20 min; then the wastewater enters a settling separation tank and stays for about 60 min. The residual solid content in the overflow of the settling separation tank is 5.8mg/L, the copper content in the filtered water sample is 6.9mg/L, and the copper removal rate is 99.1%.
Example 5
Referring to fig. 1, a continuous precipitation tank is used for removing copper from industrial cuprammonia wastewater. Gradually adding 35% sodium hydroxide solution into the reaction tank under mechanical stirring, controlling the pH value of the wastewater to be 11.95, and keeping the time for about 60 min; gradually adding hydroxamic acid type separating agent solution into the coagulation tank, wherein the dosage is about 30mg/L, and the retention time is 20 min; then the wastewater enters a settling separation tank and stays for about 100 min. The residual solid content in the overflow of the settling separation tank is 2.4mg/L, the copper content in the filtered water sample is 3.6mg/L, and the copper removal rate is 99.3 percent.
Example 6
Referring to fig. 1, the solid content of the copper-containing slurry obtained by the copper deposition treatment of the industrial cuprammonium wastewater is about 210g/L, and the sample obtained by filtering, washing and drying is shown in fig. 4, wherein the average particle size is 1.85 μm by laser particle size analysis, the sample is crystalline copper hydroxide by X-ray diffraction analysis, and the content of the copper hydroxide is 98.3% by fluorescence spectrum analysis.
The above-mentioned embodiments are only preferred embodiments of the present invention, and all equivalent changes and modifications made within the scope of the claims of the present invention should be covered by the claims of the present invention.
Claims (10)
1. A two-stage method for quickly removing copper ions in copper ammonia complexing wastewater is characterized by comprising a first-stage alkaline decomplexation precipitation and a second-stage deep chelation-flocculation; the method comprises the following steps:
adding 10-40% of alkali in copper ammonia complexing wastewater, adjusting the pH of the copper ammonia wastewater to be more than 10, performing one-section breaking precipitation to remove part of copper, decomplexing copper ammonia complexing ions, and controlling the degree of reaction crystallization to form copper hydroxide fine particles; the chemical reaction formula is as follows:
secondly, adding hydroxamic acid type separating agent accounting for 0.1 to 0.001 percent of the total amount of the wastewater into the obtained copper-containing suspension, uniformly mixing, standing, and quickly separating and removing the hydroxamic acid type separating agent by a two-stage deep chelation-flocculation method; the hydroxamic acid type separating agent is characterized in that the hydroxamic acid type separating agent is an organic high-molecular polymer containing hydroxamic acid functional groups, the content of the hydroxamic acid functional groups is 5-30%, and the molecular weight is larger than 100 ten thousand;
the chelation reaction formula of the step (2) is as follows:
[Cu(NH3)4]2++RCONHO-→RCONHOCu↓+NH3·H2O
Cu(OH)2+RCONHO-→RCONHO-Cu(OH)2↓
the flocculation mechanism is as follows:
thirdly, taking out the bottom flow after sedimentation, namely the copper-containing slurry, and dehydrating and drying the bottom flow to form copper hydroxide powder; and overflowing the filtrate and the supernatant into a subsequent deamination system.
2. The two-stage method for quickly removing copper ions in copper ammonia complexing wastewater according to claim 1, characterized in that alkali used in the alkali adjustment is one or more of sodium hydroxide, potassium hydroxide and calcium hydroxide.
3. The two-stage method for rapidly removing the copper ions in the copper ammonia complexing wastewater according to claim 2, wherein the pH of the copper ammonia complexing wastewater is adjusted to 11-13.
4. The method for rapidly removing the copper ions in the copper ammonia complex wastewater by the two-stage method according to claim 1, which is characterized in that the hydroxamic acid type separating agent is used in an amount of 0.02 to 0.002 percent of the total amount of the wastewater in the step II.
5. The two-stage method for rapidly removing copper ions in cuprammonia complexing wastewater according to claim 2, characterized in that the step comprises: adding 200g/L of alkali into the cuprammonia complexing wastewater, adjusting the pH value of the wastewater to 11.80-12.10, and performing first stepAnd (3) breaking the complex and precipitating to remove part of copper, wherein the chemical reaction formula is as follows:
6. the two-stage method for rapidly removing copper ions in cuprammonia complexing wastewater according to claim 1, characterized in that the step comprises: and (3) removing copper from the industrial copper ammonia wastewater by adopting a continuous precipitation tank: gradually adding 35% sodium hydroxide solution into the reaction tank under mechanical stirring, controlling the pH value of the wastewater to be 11.80-11.95, and keeping the time for 60 min.
7. The two-stage method for rapidly removing the copper ions in the cuprammonia complexing wastewater according to claim 1, which is characterized by further comprising the following steps: gradually adding 30mg/L hydroxamic acid type separating agent solution into the coagulation tank, and keeping the time for 20 min; then the wastewater enters a settling separation tank and stays for 60min to 100 min; the residual solid content in the overflow of the settling separation tank is 2.4 mg/L-5.8 mg/L, the copper content in the filtered water sample is 3.6 mg/L-6.9 mg/L, and the copper removal rate is 99.1-99.3%.
8. The two-stage method for rapidly removing the copper ions in the cuprammonia complexing wastewater according to claim 1, which is characterized by further comprising the following steps: the settled underflow is copper-containing slurry, the solid content of the underflow is higher than 5 percent before dehydration, the underflow is taken out and dehydrated and dried to form copper hydroxide powder, the purity is higher than 95 percent, the copper content is higher than 63 percent, and the copper hydroxide powder is used as a raw material of a related copper-containing reagent and is used as an agricultural copper hydroxide bactericide; and overflowing the filtrate and the supernatant into a subsequent deamination system.
9. The two-stage method for rapidly removing the copper ions in the copper ammonia complex wastewater according to claim 8, wherein the treated copper ammonia wastewater is the cleaning wastewater after the alkaline etching of the printed circuit and comprises the components of a copper ammonia complex and free ammonia; the treated overflow and filtrate are ammonia nitrogen wastewater after copper removal, and directly enter ammonia nitrogen treatment systems such as stripping and membrane separation, or enter a biochemical treatment system after dilution.
10. The two-stage method for rapidly removing the copper ions from the cuprammonium complex wastewater according to claim 8, wherein the solid content of the copper-containing slurry obtained by the cuprammonium complex wastewater after the cuprammonium complex wastewater is subjected to copper deposition treatment is 80 g/L-210 g/L, after the copper-containing slurry is filtered, washed and dried, the average particle size of the copper-containing slurry is 1.85 μm-2.32 μm as shown by laser particle size analysis, the copper-containing slurry is crystalline copper hydroxide as shown by X-ray diffraction analysis, and the content of the copper-containing slurry is 98.3% -99.1% as shown by fluorescence spectrum analysis.
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| CN102466637A (en) * | 2010-11-01 | 2012-05-23 | 袁俊海 | Method for measuring static ion removal rate of hydroxamic acid type polymeric chelant |
| CN102765829A (en) * | 2011-05-04 | 2012-11-07 | 上海焦化有限公司 | Treatment method for urea-containing high concentration copper ammonium wastewater |
| CN103466770A (en) * | 2013-09-27 | 2013-12-25 | 中南大学 | Copper ammonia complexation wastewater treatment method |
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| CN102466637A (en) * | 2010-11-01 | 2012-05-23 | 袁俊海 | Method for measuring static ion removal rate of hydroxamic acid type polymeric chelant |
| CN102765829A (en) * | 2011-05-04 | 2012-11-07 | 上海焦化有限公司 | Treatment method for urea-containing high concentration copper ammonium wastewater |
| CN103466770A (en) * | 2013-09-27 | 2013-12-25 | 中南大学 | Copper ammonia complexation wastewater treatment method |
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