CN110683676A - Copper-containing printed circuit board wastewater treatment method - Google Patents
Copper-containing printed circuit board wastewater treatment method Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F1/722—Oxidation by peroxides
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- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
- C02F11/122—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering using filter presses
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Abstract
The invention discloses a method for treating copper-containing printed circuit board wastewater, which specifically comprises the following steps: step 1, pumping copper-containing printed circuit board wastewater into a reaction kettle by a pump, wherein the wastewater contains a copper complex, and adjusting the pH value of the wastewater; step 2, adding a complex breaking agent into the reaction kettle, carrying out complex breaking reaction on the complex breaking agent and the wastewater copper complex, and stirring for 30-40 minutes; step 3, adding an oxidant into the reaction kettle, carrying out an enhanced reaction on the oxidant and the wastewater copper complex, and stirring for 30-40 minutes; step 4, adjusting the pH value of the wastewater, adding a precipitator, carrying out precipitation reaction on the precipitator and the wastewater copper complex, and stirring for 20-30 minutes; and 5, adjusting the pH value of the wastewater, adding a flocculating agent, stirring for 5-10 minutes, and standing for 2-3 hours after precipitation. The invention solves the problems of high cost and poor precipitation effect of the existing wastewater treatment method.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and relates to a method for treating copper-containing printed circuit board wastewater.
Background
In the rapid development of the semiconductor electronic information industry, the wastewater generated by chemical copper plating of circuit boards contains a large amount of copper, thus destroying the ecological environment and threatening the human health. Heavy metal copper ions in the wastewater form a stable complex, the copper ions in a complex structure are difficult to precipitate by a precipitation and coagulation treatment method which is conventionally adopted, COD (chemical oxygen demand) and copper are difficult to reach the standard, particularly, the copper ions are difficult to stably reach the standard, a complex breaking reaction is required to be firstly carried out to enable the copper ions to be dissociated from the complex structure, and then precipitation and coagulation are carried out. The ferrous sulfate or sodium sulfide method is generally adopted to break the network, the ferrous sulfate method has the advantages of low cost and little influence by the concentration of suspended matters in the wastewater, and the disadvantages of yellowing of the treated water, high mud content and poor settling effect are that the sludge treated by a settling tank is easy to rebound the concentration of copper ions after being contacted with the supernatant for a long time, thereby influencing the quality of the effluent. The sodium sulfide method for treating the complex water has the advantages that copper ions do not rebound after treatment, the sludge production is small, and the defects of high price, high cost, easy formation of colloidal solution, difficult filtration, pipeline blockage, large influence of suspended substances in water and odor are caused. If the control is not good, the effluent quality is black, the sulfur ions can exceed the standard, and secondary pollution is easy to form.
Disclosure of Invention
The invention aims to provide a copper-containing printed circuit board wastewater treatment method, which solves the problems of high cost and poor precipitation effect of the existing wastewater treatment method.
The technical scheme adopted by the invention is that the method for treating the copper-containing printed circuit board wastewater specifically comprises the following steps:
step 2, adding a complex breaking agent into the reaction kettle, carrying out complex breaking reaction on the complex breaking agent and the wastewater copper complex, and stirring for 30-40 minutes;
step 3, adding an oxidant into the reaction kettle, carrying out an enhanced reaction on the oxidant and the wastewater copper complex, and stirring for 30-40 minutes;
step 4, adjusting the pH value of the wastewater, adding a precipitator, carrying out precipitation reaction on the precipitator and the wastewater copper complex, and stirring for 20-30 minutes;
and 5, adjusting the pH value of the wastewater, adding a flocculating agent, stirring for 5-10 minutes, standing for 2-3 hours after precipitation, discharging supernatant, and performing filter pressing on lower-layer sludge to a filter press to form cakes.
The present invention is also characterized in that,
the Cu-containing complex in the step 1 is a copper ammonia complex [ Cu (NH) ] generated by the printed circuit board3)4]2+Copper-chlorine complex [ Cu (Cl)-)4]2-Copper ethylenediaminetetraacetic acid complex [ Cu (EDTA)]2+At least one of (1).
The pH value in the step 1 is 2.5-3.0, and the pH regulator is sulfuric acid with the mass percentage concentration of 98%.
The stirring temperature in the step 1 is 40-50 ℃.
In the step 2, the complex breaking agent is ferrous sulfate particles.
In the step 3, the oxidant is hydrogen peroxide with the mass percentage concentration of 30%.
In the step 4, the pH value is 7.0-8.0, and the pH regulator is sodium hydroxide particles.
The precipitant in step 4 is sodium sulfide.
The pH value in the step 5 is 7.0-8.0, and the flocculating agent is a polyacrylamide solution with the mass percentage concentration of 1 per mill.
The invention has the following beneficial effects: the invention provides a method for treating copper-containing printed circuit board wastewater, which overcomes the defects of yellowing of water quality and poor precipitation effect after ferrous sulfate treatment, and the addition of hydrogen peroxide strengthens the complex breaking reaction: sodium sulfide is added, copper ions do not rebound after treatment, the sludge production is small, meanwhile, excessive iron ions and sulfur ions generate iron sulfide precipitation, the influence of sulfur ions is eliminated, and effluent quality is effectively prevented from blackening and the sulfur ions exceed the standard. The copper and COD concentration of the effluent treated by the method reaches the discharge standard, the cost is low, and the effluent can stably run in a production workshop.
Drawings
FIG. 1 is a flow chart of a method for treating wastewater containing copper printed circuit boards according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a method for treating copper-containing printed circuit board wastewater, which comprises the following steps: pumping copper-containing printed circuit board wastewater into a reaction kettle by a pump, adjusting the pH value of the wastewater, starting stirring, and controlling the temperature; adding a complex breaking agent into the reaction kettle, carrying out complex breaking reaction on the complex breaking agent and the copper complex, and stirring for 30-40 minutes; adding an oxidant into the reaction kettle, carrying out an enhanced reaction on the oxidant and the copper complex, and stirring for 30-40 minutes; adjusting the pH value of the wastewater, adding a precipitator, carrying out precipitation reaction on the precipitator and the copper complex, and stirring for 20-30 minutes; and adjusting the pH value of the wastewater, adding a flocculating agent, stirring for 5-10 minutes, standing for 2-3 hours after precipitation, discharging supernatant, and carrying out filter pressing on lower-layer sludge in a filter press to form cakes.
Specifically, in combination with the above method, the flow chart of the wastewater treatment method according to the present invention is shown in FIG. 1, and is specifically described in conjunction with FIG. 1.
Firstly, step S1 is executed, copper-containing printed circuit board wastewater is pumped into a reaction kettle by a pump, the wastewater contains a copper complex, the pH value of the wastewater is adjusted, stirring is started, and the temperature is controlled.
The copper-containing complex is copper-containing ammonia complex [ Cu (NH) ] generated by printed circuit board3)4]2+Copper-chlorine complex [ Cu (Cl)-)4]2+And EDTA complex of copper [ Cu (EDTA)]2+One or more mixed waste water, wherein the concentration of copper ions is dozens of to hundreds of mg/L, the original waste water is acidic or alkaline, a pH regulator used for regulating the pH value is sulfuric acid with the mass percentage concentration of 98 percent, the added regulator is determined according to the requirement, and the stirring temperature is 40-50 ℃.
Next, step S2 is executed, and a complex breaking agent is added into the reaction kettle for carrying out a complex breaking reaction with the wastewater copper complex. In the invention, the ferrous sulfate particles adopted by the complex breaking agent are determined according to the requirement. Ferrous iron ion Fe of ferrous sulfate2+Has the advantages of reducing property,when the pH value is 2.5-3.0, Cu in water can be removed2+Reduction to Cu+And Cu+And NH3EDTA and Cl-The formed complex is degraded in stability and is further dehydrated to form cuprous oxide precipitate in the next step S3. The reaction equation is as follows:
[Cu(NH3)4]2++Fe2+≒Cu++Fe3++4NH3
[Cu(Cl-)4]2-+Fe2+≒Cu++Fe3++4Cl-
[Cu(EDTA)]2++Fe2+≒Cu++Fe3++EDTA
the complex reaction is generally carried out stepwise, and side reactions also occur, forming a portion of the monovalent copper ion complex:
[Cu(NH3)4]2++Fe2+≒[Cu(NH3)2]++Fe3++2NH3
[Cu(Cl-)4]2-+Fe2+≒[Cu(Cl-)2]-+Fe3++2Cl-
[Cu(EDTA)]2++Fe2+≒[Cu(EDTA)]++Fe3+
in the present invention, the decomplexing agent is not limited to ferrous sulfate, but may be other iron salts, such as ferric sulfate, ferric chloride, etc., as long as the decomplexing reaction of the present invention can be achieved, and is also within the protection scope of the present invention.
And step S3 is executed, an oxidant is added into the reaction kettle, the oxidant reacts with the copper complex, and the mixture is stirred for 30-40 minutes. The oxidant is hydrogen peroxide (H) with the mass percentage concentration of 30 percent2O2). The hydrogen peroxide can strengthen the complex breaking reaction in the step S2 and mainly plays the following roles:
① A monovalent copper complex is stable under oxygen-free, reducing conditions, but under aerobic conditions, [ Cu (NH)3)2]+Is easy to be H2O2By oxidation to [ Cu(NH3)4]2+Or divalent copper ion Cu2+For example, the monovalent copper ammonia complex is oxidized, and the reaction formula is as follows:
4[Cu(NH3)2]++8NH3·H2O+O2＝4[Cu(NH3)4]2++4OH-+6H2O
4[Cu(NH3)2]++8NH3·H2O+O2＝4Cu2++6H2O+4OH-+NH4 +
②H2O2can also reduce COD and NH in the wastewater3-N。H2O2The addition amount is determined according to actual conditions.
And step S4, adjusting the pH value of the wastewater, adding a precipitator, carrying out precipitation reaction on the precipitator and the wastewater copper complex, and stirring for 20-30 minutes. The pH value is 7.0-8.0, the pH regulator is sodium hydroxide particles, the precipitator is sodium sulfide, and the addition amount is determined according to the actual situation. Sulfide ion (S) in sodium sulfide2-) Can form a very stable compound with copper ions, and the stability constant of the compound is higher than that of the copper ions and ammonia (NH)3) EDTA, chloride ion (Cl)-) Stability constant of the complex, formation of a black precipitate, the reaction formula is as follows:
Cu2++S2-＝CuS↓
meanwhile, the excessive iron ions and the sulfur ions generate iron sulfide precipitates, the influence of the sulfur ions is eliminated, the effluent quality is effectively prevented from blackening, the standard exceeding of the sulfur ions is avoided, and the reaction formula is as follows:
Fe2++S2-＝FeS↓
and finally, executing the step S5, adjusting the pH value of the wastewater, adding a flocculating agent, stirring for 5-10 minutes, standing for 2-3 hours after precipitation, discharging supernatant, and performing pressure filtration on lower-layer sludge in a pressure filter to form cakes. The pH value is 7.0-8.0, and the flocculating agent is a Polyacrylamide (PAM) solution with the mass percentage concentration of 1 per mill. In the course of precipitation, Fe3+Hydrolysis to produce ferric hydroxide, which has the following reaction formula:
Fe3++3H2O＝Fe(OH)3↓+3H+
meanwhile, cupric hydroxide is formed under the alkaline condition of divalent copper ions, and the reaction formula is as follows:
Cu2++2OH-＝Cu(OH)2↓
the univalent copper ions are unstable and are easy to react with hydroxyl to generate cuprous hydroxide, and the cuprous hydroxide is dehydrated to generate cuprous oxide precipitate, and the reaction formula is as follows:
2Cu++2OH-＝Cu2O↓+H2O
the flocculant PAM makes the flocculant form large floccules to be precipitated together.
Example 1
A method for treating wastewater of a copper-containing printed circuit board comprises the following steps: pumping the copper-containing printed circuit board wastewater into a reaction kettle by a pump, wherein the wastewater contains [ Cu (NH)3)4]2+A complex, adjusting the pH value of the wastewater to 2.5 by using sulfuric acid, starting stirring, and controlling the stirring temperature to be 40 ℃; adding a complex breaking agent ferrous sulfate particle, the ferrous sulfate particle and a catalyst containing [ Cu (NH) into a reaction kettle3)4]2+Complex is subjected to complex breaking reaction and stirred for 30 minutes; adding hydrogen peroxide (H) with the mass percent concentration of 30 percent into a reaction kettle2O2) As the oxidizing agent, an oxidizing agent with [ Cu (NH)3)4]2+Carrying out an intensified reaction on the complex, and stirring for 30 minutes; adjusting pH of the wastewater to 7.0, adding sodium sulfide as precipitant, and precipitating with [ Cu (NH)3)4]2+Carrying out precipitation reaction on the complex, and stirring for 20 minutes; adjusting the pH value of the wastewater to 7.0, adding a polyacrylamide solution with the mass percent concentration of 1 thousandth as a flocculating agent, stirring for 5 minutes, standing for 2 hours after precipitation, discharging supernatant, and performing filter pressing on lower-layer sludge in a filter press to form cakes.
Example 2
A method for treating wastewater of a copper-containing printed circuit board comprises the following steps: pumping the copper-containing printed circuit board wastewater into a reaction kettle by a pump, wherein the wastewater contains a copper-chlorine complex [ Cu (Cl)-)4]2Adjusting the pH value of the waste water to 2.8,starting stirring, and controlling the stirring temperature to be 45 ℃; adding a complex breaking agent ferrous sulfate particle, the ferrous sulfate particle and a complex containing copper and chlorine [ Cu (Cl)-)4]2Carrying out a complex breaking reaction, and stirring for 35 minutes; adding hydrogen peroxide (H) with the mass percent concentration of 30 percent into a reaction kettle2O2) As the oxidizing agent, an oxidizing agent and a copper chloride complex [ Cu (Cl)-)4]2-Carrying out an enhanced reaction, and stirring for 35 minutes; adjusting pH of the wastewater to 7.5, adding sodium sulfide as precipitant, and mixing the precipitant with copper-chlorine complex [ Cu (Cl)-)4]2-Carrying out precipitation reaction, and stirring for 25 minutes; adjusting the pH value of the wastewater to 7.5, adding a polyacrylamide solution with the mass percent concentration of 1 thousandth as a flocculating agent, stirring for 8 minutes, standing for 2.5 hours after precipitation, discharging supernatant, and performing pressure filtration on lower-layer sludge in a filter press to form cakes.
Example 3
A method for treating wastewater of a copper-containing printed circuit board comprises the following steps: pumping the waste water containing copper printed circuit board into a reaction kettle by a pump, wherein the waste water contains EDTA complex [ Cu (EDTA)]2+Adjusting the pH value of the wastewater to 3.0, starting stirring, and controlling the stirring temperature to be 50 ℃; adding a complex breaking agent ferrous sulfate particle, a ferrous sulfate particle and [ Cu (EDTA) ]into a reaction kettle]2+Carrying out a complex breaking reaction, and stirring for 40 minutes; adding hydrogen peroxide (H) with the mass percent concentration of 30 percent into a reaction kettle2O2) EDTA complex of oxidizing agent and copper [ Cu (EDTA) ]as oxidizing agent]2+Carrying out an enhanced reaction, and stirring for 40 minutes; adjusting the pH of the wastewater to 8.0, adding sodium sulfide as a precipitant, the precipitant and [ Cu (EDTA)]2+Carrying out precipitation reaction, and stirring for 30 minutes; adjusting the pH value of the wastewater to 8.0, adding a polyacrylamide solution with the mass percent concentration of 1 thousandth as a flocculating agent, stirring for 10 minutes, standing for 3 hours after precipitation, discharging supernatant, and performing filter pressing on lower-layer sludge in a filter press to form cakes.
After the wastewater treatment method of the embodiments 1 to 3 is used for treatment, the removal rate of copper can reach more than 98%, after precipitation, supernatant and lower-layer sludge are separated, and the concentrations of copper ions and COD in the treated mixed wastewater reach the national discharge standard and can be discharged. The sludge from which the copper precipitated compounds are separated can be sent to a filter press by a pressure pump to be filter-pressed into cakes for dehydration treatment, and can be recovered in a entrusted treatment mode after dehydration treatment.
Claims (9)
1. A method for treating wastewater of a copper-containing printed circuit board is characterized by comprising the following steps: the method specifically comprises the following steps:
step 1, pumping copper-containing printed circuit board wastewater into a reaction kettle by a pump, adjusting the pH value of the wastewater, starting stirring, and controlling the stirring temperature;
step 2, adding a complex breaking agent into the reaction kettle, carrying out complex breaking reaction on the complex breaking agent and the wastewater copper complex, and stirring for 30-40 minutes;
step 3, adding an oxidant into the reaction kettle, carrying out an enhanced reaction on the oxidant and the wastewater copper complex, and stirring for 30-40 minutes;
step 4, adjusting the pH value of the wastewater, adding a precipitator, carrying out precipitation reaction on the precipitator and the wastewater copper complex, and stirring for 20-30 minutes;
and 5, adjusting the pH value of the wastewater, adding a flocculating agent, stirring for 5-10 minutes, standing for 2-3 hours after precipitation, discharging supernatant, and performing filter pressing on lower-layer sludge to a filter press to form cakes.
2. The method for treating wastewater containing copper printed circuit boards according to claim 1, wherein the method comprises the following steps: the copper-containing complex in the step 1 is a copper ammonia complex [ Cu (NH) generated by a printed circuit board3)4]2+Copper-chlorine complex [ Cu (Cl)-)4]2-EDTA complex of copper [ Cu (EDTA)]2+At least one of (1).
3. The method for treating wastewater containing copper printed circuit boards according to claim 2, wherein the method comprises the following steps: the pH value in the step 1 is 2.5-3.0, and the pH regulator is sulfuric acid with the mass percentage concentration of 98%.
4. The method for treating wastewater containing copper printed circuit boards according to claim 1, wherein the method comprises the following steps: the stirring temperature in the step 1 is 40-50 ℃.
5. The method for treating wastewater containing copper printed circuit boards according to claim 1, wherein the method comprises the following steps: the complex breaking agent in the step 2 is ferrous sulfate particles.
6. The method for treating wastewater containing copper printed circuit boards according to claim 1, wherein the method comprises the following steps: the oxidant in the step 3 is hydrogen peroxide with the mass percentage concentration of 30%.
7. The method for treating wastewater containing copper printed circuit boards according to claim 1, wherein the method comprises the following steps: in the step 4, the pH value is 7.0-8.0, and the pH regulator is sodium hydroxide particles.
8. The method for treating wastewater containing copper printed circuit boards according to claim 7, wherein the method comprises the following steps: the precipitant in the step 4 is sodium sulfide.
9. The method for treating wastewater containing copper printed circuit boards according to claim 1, wherein the method comprises the following steps: the pH value in the step 5 is 7.0-8.0, and the flocculating agent is a polyacrylamide solution with the mass percentage concentration of 1 per mill.
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Cited By (7)
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| CN111320302A (en) * | 2020-03-12 | 2020-06-23 | 江苏中电创新环境科技有限公司 | Process for standard emission and efficient sedimentation of low-concentration copper-containing wastewater in semiconductor industry |
| CN111333219A (en) * | 2020-03-11 | 2020-06-26 | 深圳清华大学研究院 | Online purification and recycling method of PCB washing wastewater |
| CN111394736A (en) * | 2020-04-09 | 2020-07-10 | 北方华锦化学工业股份有限公司 | Preparation method and cleaning method of copper ion ferrous sulfide cleaning agent |
| CN112499739A (en) * | 2020-11-11 | 2021-03-16 | 中南大学 | Method for treating copper-containing wastewater through ore grinding mechanochemical regulation and control |
| CN112624402A (en) * | 2020-12-08 | 2021-04-09 | 泰州市惠明固废处置有限公司 | Copper-containing waste liquid pretreatment process |
| CN113025811A (en) * | 2021-03-05 | 2021-06-25 | 衢州华友钴新材料有限公司 | Deep elution method for chlorine in copper sulfide precipitation slag |
| CN113200625A (en) * | 2021-05-17 | 2021-08-03 | 中南大学 | Method for realizing deep purification of EDTA-Ni/Cu complex wastewater based on complex transformation |
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| CN111333219A (en) * | 2020-03-11 | 2020-06-26 | 深圳清华大学研究院 | Online purification and recycling method of PCB washing wastewater |
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| CN111394736A (en) * | 2020-04-09 | 2020-07-10 | 北方华锦化学工业股份有限公司 | Preparation method and cleaning method of copper ion ferrous sulfide cleaning agent |
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| CN112624402A (en) * | 2020-12-08 | 2021-04-09 | 泰州市惠明固废处置有限公司 | Copper-containing waste liquid pretreatment process |
| CN113025811A (en) * | 2021-03-05 | 2021-06-25 | 衢州华友钴新材料有限公司 | Deep elution method for chlorine in copper sulfide precipitation slag |
| CN113025811B (en) * | 2021-03-05 | 2023-08-08 | 衢州华友钴新材料有限公司 | Deep elution method for chlorine in copper sulfide precipitation slag |
| CN113200625A (en) * | 2021-05-17 | 2021-08-03 | 中南大学 | Method for realizing deep purification of EDTA-Ni/Cu complex wastewater based on complex transformation |
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