CN112573734A - Environment-friendly discharge method of ammonia nitrogen wastewater in regeneration and recycling process of etching solution - Google Patents
Environment-friendly discharge method of ammonia nitrogen wastewater in regeneration and recycling process of etching solution Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F9/00—Multistage treatment of water, waste water or sewage
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- 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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- 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
- C02F2001/007—Processes including a sedimentation step
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Abstract
The invention discloses an environment-friendly discharge method of ammonia nitrogen wastewater in the process of regeneration and recycling of etching solution, which is characterized by comprising the following steps: s1, collecting and removing impurities from ammonia nitrogen wastewater; step S2, wastewater treatment; step S3, settling and filtering; and step S4, nanofiltration membrane treatment. The environment-friendly discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of the etching solution disclosed by the invention can safely, efficiently and quickly treat the ammonia nitrogen wastewater in the regeneration and recycling process of the etching solution, has small influence on the environment, short treatment period, less equipment investment and lower operation cost, does not cause air pollution, and is suitable for large-scale industrial application.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to an environment-friendly discharge method of ammonia nitrogen wastewater in an etching solution regeneration and recycling process.
Background
Printed Circuit Boards (PCBs) are important components of electronic products, which are the basis of the electronic information industry, and advanced technology products are not separated from PCBs. With the development of the electronic industry, the production of printed circuit boards is developed very rapidly, and a large amount of circuit board etching solution is generated. In the etching process, when the concentration of copper ions in the etching solution reaches saturation, the etching solution loses etching capability to form etching waste liquid, and the etching waste liquid contains a large amount of components harmful to the environment, such as copper ions and the like. Therefore, the treatment of the waste etching solution is always a problem for enterprises.
The regeneration and recycling of the etching solution is the most effective method for treating the etching waste solution, so that the problem of environmental pollution is reduced, resources can be saved, and waste is changed into valuable. In the process of regeneration and recycling of the etching solution, some ammonia nitrogen wastewater is inevitably generated, and the ammonia nitrogen in the ammonia nitrogen wastewater is mainly ammonium ions (NH)4 +) The biological fertilizer is an important substance causing water eutrophication and environmental pollution, easily causes mass propagation of algae and other microorganisms in water, and can reduce dissolved oxygen in water and kill fishes in a large amount in severe cases, even cause drying of lakes; the ammonia nitrogen can also increase the chlorine consumption in the processes of water supply disinfection and industrial circulating water sterilization treatment; in addition, ammonia nitrogen is corrosive to certain metals (copper), and when sewage is recycled, the ammonia nitrogen in the regenerated water can promote the reproduction of microorganisms in water pipelines and water using equipment, so that biological scale is formed, the pipelines and the water using equipment are blocked, and the heat exchange efficiency is influenced. Therefore, the environmental protection discharge of ammonia nitrogen wastewater in the regeneration and recycling process of the etching solution draws extensive attention in the industry.
At present, more environmental-friendly discharge methods are used for ammonia nitrogen wastewater in the process of recycling etching solution at home and abroad, but the methods have the disadvantages of higher operation cost, more serious equipment corrosion, easy secondary air pollution and adverse safety and environment; complex process operation, short treatment period, high treatment cost, easy secondary pollution, unsuitability for large-scale industrial application, large energy consumption and the like.
For example, CN 105600923B discloses a biological denitrification process for high ammonia nitrogen wastewater, which is to add aerobic or anaerobic sludge as inoculated sludge into a reactor under anaerobic or anoxic conditions; adding ferric ions into the high ammonia nitrogen wastewater according to the molar ratio of the ferric ions to the ammonia nitrogen concentration of 1.0-6.0:1, mixing, then adding the high ammonia nitrogen wastewater into a reactor, adjusting the pH value of the high ammonia nitrogen wastewater to 6.5-8.5, staying the high ammonia nitrogen wastewater in the reactor for 0.5-5 days at 15-35 ℃, and then discharging the wastewater up to the standard or entering the next treatment process. The invention overcomes the technical defects of high operating cost, incapability of realizing complete denitrification and long time consumption of the existing anaerobic ammonia oxidation denitrification process, and provides the biological denitrification process for the high-ammonia nitrogen wastewater, which has the advantages of whole-course unpowered autotrophic operation, high denitrification efficiency and short start time. However, the ammonia nitrogen concentration of the inlet water of the method is generally too high, otherwise the normal operation is influenced, and the high-concentration ammonia nitrogen per se has an inhibiting effect on the activity and the propagation of microorganisms. In addition, biochemical reactions are slow, often requiring long hydraulic residence times, and therefore require large structures and large floor space.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the environment-friendly discharge method of the ammonia nitrogen wastewater in the regeneration and recycling process of the etching solution.
In order to achieve the purpose, the invention adopts the technical scheme that: an environment-friendly discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of etching solution is characterized by comprising the following steps:
s1, collecting and removing impurities of ammonia nitrogen wastewater: collecting ammonia nitrogen wastewater generated in the regeneration and recycling process of the etching solution in a liquid storage tank, and filtering to remove impurities in the ammonia nitrogen wastewater;
step S2, wastewater treatment: putting the ammonia nitrogen wastewater treated in the step S1 into a purification device, adding a wastewater treatment agent into the purification device, uniformly stirring, and exposing and aerating the purification device;
step S3, settling and filtering: sequentially settling and filtering the wastewater treated in the step S2 to obtain filtrate; adding water into the filtrate for dilution, and adjusting the pH value to be between 6 and 8;
step S4, nanofiltration membrane treatment: after the wastewater treated in the step S3 is treated by the nanofiltration membrane, the wastewater penetrating through the nanofiltration membrane is directly discharged; and (4) performing rotary evaporation and concentration on the nanofiltration membrane trapped fluid to obtain a chemical product.
Preferably, the mass ratio of the ammonia nitrogen wastewater to the wastewater treatment agent in the step S2 is 100 (2-5).
Preferably, the wastewater treatment agent in step S2 is prepared from the following components in parts by weight: 3-6 parts of titanium dioxide quantum dots, 1-3 parts of rare earth oxide, 3-5 parts of alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyl tri (acetylene-2, 1-diyl)) triphenylamine, 2-5 parts of sodium phosphate and 1-3 parts of sepiolite powder.
Preferably, the rare earth oxide is an oxide of yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium or terbium.
Preferably, the preparation method of the alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine comprises the following steps: adding silane coupling agents KH560 and 4,4 '- (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine into an organic solvent, stirring and reacting for 6-8 hours at 70-80 ℃, and then removing the solvent by rotary evaporation to obtain the alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine.
Preferably, the silane coupling agent KH560, 4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine and the organic solvent are in a molar ratio of 3:1 (15-25).
Preferably, the organic solvent is any one of dimethyl sulfoxide, acetone, tetrahydrofuran and N, N-dimethylformamide.
Preferably, the aeration time in step S2 is 40-60min, and the exposure time is 1-3 hours.
Preferably, the settling time in step S3 is 1 to 3 hours.
Preferably, the nanofiltration membrane in the step S4 is any one of SS-NF1-8338-F, SS-NF3-8038-F, SS-NF 7-4040-F.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the invention provides an environment-friendly discharge method of ammonia nitrogen wastewater in the process of etching solution regeneration and recycling, which can safely, efficiently and quickly treat the ammonia nitrogen wastewater in the process of etching solution regeneration and recycling, has small influence on the environment, short treatment period, less equipment investment and lower operation cost, does not cause air pollution, and is suitable for large-scale industrial application.
Detailed Description
The following detailed description of preferred embodiments of the invention will be made.
An environment-friendly discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of etching solution is characterized by comprising the following steps:
s1, collecting and removing impurities of ammonia nitrogen wastewater: collecting ammonia nitrogen wastewater generated in the regeneration and recycling process of the etching solution in a liquid storage tank, and filtering to remove impurities in the ammonia nitrogen wastewater;
step S2, wastewater treatment: putting the ammonia nitrogen wastewater treated in the step S1 into a purification device, adding a wastewater treatment agent into the purification device, uniformly stirring, and exposing and aerating the purification device;
step S3, settling and filtering: sequentially settling and filtering the wastewater treated in the step S2 to obtain filtrate; adding water into the filtrate for dilution, and adjusting the pH value to be between 6 and 8;
step S4, nanofiltration membrane treatment: after the wastewater treated in the step S3 is treated by the nanofiltration membrane, the wastewater penetrating through the nanofiltration membrane is directly discharged; and (4) performing rotary evaporation and concentration on the nanofiltration membrane trapped fluid to obtain a chemical product.
Preferably, the mass ratio of the ammonia nitrogen wastewater to the wastewater treatment agent in the step S2 is 100 (2-5).
Preferably, the wastewater treatment agent in step S2 is prepared from the following components in parts by weight: 3-6 parts of titanium dioxide quantum dots, 1-3 parts of rare earth oxide, 3-5 parts of alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyl tri (acetylene-2, 1-diyl)) triphenylamine, 2-5 parts of sodium phosphate and 1-3 parts of sepiolite powder.
Preferably, the rare earth oxide is an oxide of yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium or terbium.
Preferably, the preparation method of the alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine comprises the following steps: adding silane coupling agents KH560 and 4,4 '- (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine into an organic solvent, stirring and reacting for 6-8 hours at 70-80 ℃, and then removing the solvent by rotary evaporation to obtain the alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine.
Preferably, the silane coupling agent KH560, 4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine and the organic solvent are in a molar ratio of 3:1 (15-25).
Preferably, the organic solvent is any one of dimethyl sulfoxide, acetone, tetrahydrofuran and N, N-dimethylformamide.
Preferably, the aeration time in step S2 is 40-60min, and the exposure time is 1-3 hours.
Preferably, the settling time in step S3 is 1 to 3 hours.
Preferably, the nanofiltration membrane in the step S4 is any one of SS-NF1-8338-F, SS-NF3-8038-F, SS-NF 7-4040-F.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the invention provides an environment-friendly discharge method of ammonia nitrogen wastewater in the process of etching solution regeneration and recycling, which can safely, efficiently and quickly treat the ammonia nitrogen wastewater in the process of etching solution regeneration and recycling, has small influence on the environment, short treatment period, less equipment investment and lower operation cost, does not cause air pollution, and is suitable for large-scale industrial application.
The invention will be further described with reference to specific examples, but the scope of protection of the invention is not limited thereto:
example 1
The embodiment 1 provides an environment-friendly discharge method of ammonia nitrogen wastewater in an etching solution regeneration and recycling process, which is characterized by comprising the following steps:
s1, collecting and removing impurities of ammonia nitrogen wastewater: collecting ammonia nitrogen wastewater generated in the regeneration and recycling process of the etching solution in a liquid storage tank, and filtering to remove impurities in the ammonia nitrogen wastewater;
step S2, wastewater treatment: putting the ammonia nitrogen wastewater treated in the step S1 into a purification device, adding a wastewater treatment agent into the purification device, uniformly stirring, and exposing and aerating the purification device;
step S3, settling and filtering: sequentially settling and filtering the wastewater treated in the step S2 to obtain filtrate; adding water into the filtrate for dilution, and adjusting the pH value to be 6;
step S4, nanofiltration membrane treatment: after the wastewater treated in the step S3 is treated by the nanofiltration membrane, the wastewater penetrating through the nanofiltration membrane is directly discharged; and (4) performing rotary evaporation and concentration on the nanofiltration membrane trapped fluid to obtain a chemical product.
And in the step S2, the mass ratio of the ammonia nitrogen wastewater to the wastewater treatment agent is 100: 2.
The wastewater treatment agent in the step S2 is prepared from the following components in parts by weight: 3 parts of titanium dioxide quantum dots, 1 part of rare earth oxide, 3 parts of alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyl tri (acetylene-2, 1-diyl)) triphenylamine, 2 parts of sodium phosphate and 1 part of sepiolite powder.
The rare earth oxide is an oxide of yttrium.
The preparation method of the alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyl tri (acetylene-2, 1-diyl)) triphenylamine comprises the following steps: adding silane coupling agents KH560 and 4,4 '- (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine into an organic solvent, stirring and reacting for 6 hours at 70 ℃, and then removing the solvent by rotary evaporation to obtain alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine; the silane coupling agent KH560, 4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine and the organic solvent are in a molar ratio of 3:1: 15; the organic solvent is dimethyl sulfoxide.
The aeration time in the step S2 is 40min, and the exposure time is 1 hour; the settling time in step S3 is 1 hour; and in the step S4, the mark of the nanofiltration membrane is SS-NF 1-8338-F.
Example 2
Embodiment 2 provides an environment-friendly discharge method of ammonia nitrogen wastewater in an etching solution regeneration recycling process, which is basically the same as that in embodiment 1, except that the wastewater treatment agent in step S2 is prepared from the following components in parts by weight: 4 parts of titanium dioxide quantum dots, 1.5 parts of rare earth oxide, 3.5 parts of alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyl tri (acetylene-2, 1-diyl)) triphenylamine, 3 parts of sodium phosphate and 1.5 parts of sepiolite powder.
Example 3
Embodiment 3 provides an environment-friendly discharge method of ammonia nitrogen wastewater in an etching solution regeneration recycling process, which is basically the same as that in embodiment 1, except that the wastewater treatment agent in step S2 is prepared from the following components in parts by weight: 4.5 parts of titanium dioxide quantum dots, 2 parts of rare earth oxide, 4 parts of alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyl tri (acetylene-2, 1-diyl)) triphenylamine, 3.5 parts of sodium phosphate and 2 parts of sepiolite powder.
Example 4
Embodiment 4 provides an environment-friendly discharge method of ammonia nitrogen wastewater in an etching solution recycling process, which is basically the same as that in embodiment 1, except that the wastewater treatment agent in step S2 is prepared from the following components in parts by weight: 5.5 parts of titanium dioxide quantum dots, 2.5 parts of rare earth oxide, 4.5 parts of alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyl tri (acetylene-2, 1-diyl)) triphenylamine, 4.5 parts of sodium phosphate and 2.5 parts of sepiolite powder.
Example 5
Embodiment 5 provides an environment-friendly discharge method of ammonia nitrogen wastewater in an etching solution recycling process, which is basically the same as that in embodiment 1, except that the wastewater treatment agent in step S2 is prepared from the following components in parts by weight: 6 parts of titanium dioxide quantum dots, 3 parts of rare earth oxide, 5 parts of alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyl tri (acetylene-2, 1-diyl)) triphenylamine, 5 parts of sodium phosphate and 3 parts of sepiolite powder.
Comparative example 1
Comparative example 1 provides an environmentally friendly discharge method of ammonia nitrogen wastewater in the process of recycling etching solution, which is basically the same as example 1 except that the wastewater treatment agent in step S2 does not include titanium dioxide quantum dots.
Comparative example 2
Comparative example 2 provides an environmentally friendly discharge method of ammonia nitrogen wastewater in the process of recycling etching solution, which is substantially the same as example 1 except that the wastewater treatment agent does not include rare earth oxide in step S2.
Comparative example 3
Comparative example 3 provides an environmentally friendly discharge method of ammonia nitrogen wastewater in the process of recycling etching solution, which is substantially the same as example 1 except that the wastewater treatment agent described in step S2 does not include silicon alkoxide-modified 4,4',4 ″ - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine.
In order to further illustrate the beneficial technical effects of the embodiments, ammonia nitrogen wastewater in the same etching solution regeneration and recycling process is treated according to the discharge method of each embodiment, and the COD and ammonia nitrogen content after treatment are tested. In the regeneration and recycling process of untreated etching solution, COD of ammonia nitrogen wastewater is 2100mg/L, and the content of ammonia nitrogen is 1750 mg/L. The test results are shown in Table 1.
TABLE 1
| Detecting items | COD | Content of ammonia and nitrogen |
| Unit of | mg/L | mg/L |
| Example 1 | 7.3 | 4.2 |
| Example 2 | 6.6 | 3.9 |
| Example 3 | 6.1 | 3.6 |
| Example 4 | 5.7 | 3.3 |
| Example 5 | 4.8 | 3.0 |
| Comparative example 1 | 35.5 | 25.7 |
| Comparative example 2 | 42.8 | 28.5 |
| Comparative example 3 | 40.3 | 26.6 |
As can be seen from the table above, the environment-friendly discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of the etching solution according to the embodiment of the invention has better wastewater treatment effect, which is the result of synergistic effect of the raw materials in each step.
The above-mentioned embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (10)
1. An environment-friendly discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of etching solution is characterized by comprising the following steps:
s1, collecting and removing impurities of ammonia nitrogen wastewater: collecting ammonia nitrogen wastewater generated in the regeneration and recycling process of the etching solution in a liquid storage tank, and filtering to remove impurities in the ammonia nitrogen wastewater;
step S2, wastewater treatment: putting the ammonia nitrogen wastewater treated in the step S1 into a purification device, adding a wastewater treatment agent into the purification device, uniformly stirring, and exposing and aerating the purification device;
step S3, settling and filtering: sequentially settling and filtering the wastewater treated in the step S2 to obtain filtrate; adding water into the filtrate for dilution, and adjusting the pH value to be between 6 and 8;
step S4, nanofiltration membrane treatment: after the wastewater treated in the step S3 is treated by the nanofiltration membrane, the wastewater penetrating through the nanofiltration membrane is directly discharged; and (4) performing rotary evaporation and concentration on the nanofiltration membrane trapped fluid to obtain a chemical product.
2. The environment-friendly discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of etching solution as claimed in claim 1, wherein the mass ratio of the ammonia nitrogen wastewater to the wastewater treatment agent in step S2 is 100 (2-5).
3. The environment-friendly discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of etching solution as claimed in claim 1, wherein the wastewater treatment agent in step S2 is prepared from the following components in parts by weight: 3-6 parts of titanium dioxide quantum dots, 1-3 parts of rare earth oxide, 3-5 parts of alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyl tri (acetylene-2, 1-diyl)) triphenylamine, 2-5 parts of sodium phosphate and 1-3 parts of sepiolite powder.
4. The method of claim 3, wherein the rare earth oxide is yttrium oxide, lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, gadolinium oxide or terbium oxide.
5. The environment-friendly discharge method of ammonia nitrogen wastewater in the process of regeneration and recycling of etching solution as claimed in claim 3, wherein the preparation method of alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine comprises the following steps: adding silane coupling agents KH560 and 4,4 '- (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine into an organic solvent, stirring and reacting for 6-8 hours at 70-80 ℃, and then removing the solvent by rotary evaporation to obtain the alkoxy silicon modified 4,4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine.
6. The environment-friendly discharge method of ammonia nitrogen wastewater in the process of regeneration and recycling of etching solution as claimed in claim 5, wherein the molar ratio of the silane coupling agent KH560, 4' - (benzene-1, 3, 5-triyltris (acetylene-2, 1-diyl)) triphenylamine and the organic solvent is 3:1 (15-25).
7. The environment-friendly discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of etching solution as claimed in claim 5, wherein the organic solvent is any one of dimethyl sulfoxide, acetone, tetrahydrofuran and N, N-dimethylformamide.
8. The environmental protection discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of etching solution as claimed in claim 1, wherein the aeration time in step S2 is 40-60min, and the exposure time is 1-3 hours.
9. The environment-friendly discharge method of ammonia nitrogen wastewater in the regeneration and recycling process of etching solution as claimed in claim 1, wherein the settling time in step S3 is 1-3 hours.
10. The environment-friendly discharge method of ammonia nitrogen wastewater in the process of regeneration and recycling of etching solution as claimed in any one of claims 1 to 9, wherein the nanofiltration membrane in step S4 is of any one of SS-NF1-8338-F, SS-NF3-8038-F, SS-NF 7-4040-F.
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