CN112010488B - Method for preparing nano particles from heavy metal wastewater - Google Patents
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- CN112010488B CN112010488B CN202010943136.1A CN202010943136A CN112010488B CN 112010488 B CN112010488 B CN 112010488B CN 202010943136 A CN202010943136 A CN 202010943136A CN 112010488 B CN112010488 B CN 112010488B
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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
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
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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
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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Abstract
The invention belongs to the technical field of environmental protection and resource recovery, and discloses a method for preparing nano particles from heavy metal wastewater. Adding a complexing agent and a phase transfer agent into the heavy metal wastewater, stirring and mixing uniformly, then adding alkali to adjust the pH value to be alkaline, heating the obtained mixed solution to 100-230 ℃ for solvothermal reaction, and cooling to room temperature after the reaction is finished to obtain an obviously layered phase transfer solution with a lower layer of purified water and an upper layer of nano particles and the complexing agent; the lower layer is separated to obtain purified water, and the upper layer contains phase transfer solution of nano particles and complexing agent, and is centrifugally separated to obtain phase transfer solvent containing complexing agent and nano particles. The method can recover the heavy metal nanoparticles while efficiently purifying the heavy metal wastewater in a recycling manner, thereby not only reducing the wastewater treatment cost, but also increasing the economic benefit of additional products of enterprises. Has obvious application value.
Description
Technical Field
The invention belongs to the technical field of environmental protection and resource recovery, and particularly relates to a method for preparing nanoparticles from heavy metal wastewater.
Background
The pollution of the environment by heavy metals and their compounds is generally referred to as heavy metal pollution. In recent years, with the rapid development of industries such as coal mining and smelting, discharged industrial heavy metal waste is accumulated in an explosive manner. Industrial heavy metal waste materials, if not properly disposed of, can have a serious impact on the natural environment and human life. Particularly, if the heavy metal wastewater is not treated in an effective and reasonable manner and is directly discharged, the heavy metals in the wastewater can be circulated and adsorbed in the soil through underground water, and serious pollution is caused to drinking water of human beings and crops. On the other hand, heavy metals belong to non-renewable resources, and the large discharge of the heavy metals causes waste and loss of the non-renewable resources. In conclusion, the purification of heavy metal wastewater discharged by heavy industry enterprises and the recycling of heavy metal ions become one of the environmental, economic and energy problems which are paid keen attention and need to be solved urgently in the society of the current time.
In recent years, people are exploring and excavating more environment-friendly and economic methods for treating wastewater containing heavy metals. At present, the main treatment methods of heavy metal wastewater comprise chemical precipitation, ion exchange, adsorption, flocculation and the like. Although the chemical precipitation method has a simple treatment mode, a large amount of electroplating sludge is generated in the treatment process, and serious secondary pollution is caused to the natural environment and human health. The treatment process of the electroplating sludge is added, and the economic cost of treating the wastewater is improved. The methods of ion exchange, adsorption and flocculation have the defects of easy oxidation of an ion exchanger and high cost of an adsorbent and a flocculating agent, and increase the economic cost and difficulty of heavy metal wastewater treatment. Patent CN103693789A discloses a resource recovery method of heavy metals in heavy metal wastewater, which comprises adding complexing agent and reducing agent into heavy metal wastewater, adjusting the pH of the wastewater with alkaline solution, heating for full reaction, cooling to room temperature, and separating to obtain the product. The method can effectively remove heavy metals in the wastewater, and can prepare metal oxide or metal simple substance nanoparticles at the same time. However, the method needs to use a consumable reducing agent and a complexing agent which is adapted to a treatment system, although the method can effectively remove heavy metals in wastewater and recover to obtain metal oxides or metal simple substance nanoparticles, the product of the reaction of the reducing agent and the complexing agent are still left in the treated water, the separation and recovery difficulty is high, the increase of COD content in the water cannot reach the standard of water purification, and the treatment cost is obviously increased. Patent CN105347547A discloses a method for treating heavy metal wastewater, and provides a solution to the problems of the previous patent, namely, heavy metal is enriched by using a heavy metal adsorbent, the liquid obtained after heavy metal precipitation is separated by a complex reduction reaction is further subjected to activated CD-180 macroporous adsorption resin, and the effluent liquid is subjected to D113 cation exchange resin. So that the liquid after the heavy metal recovery can reach the sewage discharge standard. But this method significantly increases the process steps and the process cost.
The nano material has the advantages of small size, exposure of a large number of active sites and the like, and is widely applied to the fields of medical treatment, energy and environment at present. The method directly prepares high-value nano metal particles from the heavy metals in the heavy metal wastewater in the recovery treatment process, thereby not only reducing the harm of the heavy metal wastewater to the environment and human beings, but also generating high economic benefit. Therefore, a simple and efficient method for preparing high-value nano metal particles from heavy metal wastewater and purifying the wastewater is needed.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a method for preparing nano particles from heavy metal wastewater. The method can recycle heavy metals in the heavy metal wastewater and purify the heavy metal wastewater simultaneously.
The purpose of the invention is realized by the following technical scheme:
a method for preparing nano particles from heavy metal wastewater comprises the following steps:
adding a complexing agent and a phase transfer agent into the heavy metal wastewater, stirring and mixing uniformly, then adding alkali to adjust the pH value to be alkaline, heating the obtained mixed solution to 100-230 ℃ for solvothermal reaction, and cooling to room temperature after the reaction is finished to obtain an obviously layered phase transfer solution with a lower layer of purified water and an upper layer of nano particles and the complexing agent; the lower layer is separated to obtain purified water, and the upper layer contains phase transfer solution of nano particles and complexing agent, and is centrifugally separated to obtain phase transfer solvent containing complexing agent and nano particles.
Further, the content of heavy metals in the heavy metal wastewater is 60-5000 mg/L.
Further, the heavy metal wastewater is electroplating wastewater containing at least one heavy metal ion of nickel, zinc, chromium, cadmium and copper.
Further, the complexing agent is selected from at least one of sodium oleate, oleic acid, oleylamine and octadecene.
Further, the phase transfer agent is selected from one or a mixture of more than two of n-hexane, petroleum ether, chloroform and acetone.
Furthermore, the mass ratio of the heavy metal wastewater, the complexing agent and the phase transfer agent is 60 (1-80) to 10-200.
Further, the alkali is selected from at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium dihydrogen phosphate, calcium hydroxide, magnesium hydroxide, and ammonia water.
Further, the mass ratio of the addition amount of the alkali to the heavy metal wastewater is (1-21) to (1-120).
Further, the solvothermal reaction time is 3-48 hours.
Further, the phase transfer solvent containing the complexing agent obtained by separation is recycled.
The principle of the invention is as follows: and carrying out phase transfer and complexing reaction with heavy metals in the heavy metal wastewater by using a phase transfer agent and a complexing agent. After the phase transfer agent and the complexing agent are added into the heavy metal wastewater, the acidity and alkalinity of the heavy metal wastewater need to be adjusted so as to achieve a condition that the heavy metal in the heavy metal wastewater can be highly complexed. After the solutions are fully mixed, a high-temperature high-pressure reaction is carried out on the solutions, so that the heavy metals in the heavy metal wastewater can be completely separated out to obtain the metal nanoparticles. The purified water and the phase transfer solution containing the complexing agent can be separated simply by a two-phase separation principle between organic and inorganic substances, such as simple liquid separation. In the process of forming the nano particles, firstly, heavy metal ions are complexed with a complexing agent, then, with the addition of an alkali solution, the metal ions react with the alkali to generate the nano particles, and the heavy metal ions are transferred from a water phase to an organic phase through a solvothermal reaction.
Compared with the prior art, the method has the following advantages and beneficial effects:
(1) the invention provides a method for recovering and preparing nano particles from heavy metal wastewater, which has a simple process and can obviously improve the recovery and reutilization rate of heavy metals in the heavy metal wastewater.
(2) The nano particles prepared by the method have better dispersion and size uniformity.
(3) The method can recover the heavy metal nanoparticles while efficiently purifying the heavy metal wastewater in a recycling manner, thereby not only reducing the wastewater treatment cost, but also increasing the economic benefit of additional products of enterprises.
(4) The complexing agent and the phase transfer agent used in the method can be recycled, and the loss of raw materials is low.
(5) The method can obtain the purified water reaching safe discharge and realize the safe detoxification treatment of the heavy metal sewage.
Drawings
FIG. 1 is a transmission electron micrograph of nanoparticles prepared in example 1.
FIG. 2 is an X-ray diffraction (XRD) pattern of a sample powder of nanoparticles prepared in example 2.
FIG. 3 is a scanning electron micrograph of nanoparticles prepared in example 3.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
Taking Ni2+60mL of nickel-containing electroplating wastewater with the content of 100mg/L is added with 8g of sodium oleate and 20mL of n-hexane, stirred for 1 hour, added with 2g of sodium hydroxide and continuously stirred for 1 hour. The resulting solution was heated to 180 ℃ to effect a reaction. Reacting for 28 hours, cooling to room temperature to obtain an obviously layered solution, separating the lower layer to obtain purified water, and centrifuging the upper layer mixed solution to respectively obtain the normal hexane solvent containing the sodium oleate and the nano particles.
FIG. 1 is a transmission electron microscope image of the prepared nanoparticles, which shows that the nanoparticles are uniformly dispersed and all have a nanoscale size. The obtained n-hexane solvent containing complexing agent sodium oleate can be recycled. And (4) detecting and analyzing the purified water separated after the reaction, wherein the content of nickel ions is lower than 1 mg/L. Hydrochloric acid is used for neutralization, so that the pH value of the purified water can be safely discharged after about 7.
Example 2
Taking Ni2+60mL of nickel-containing electroplating wastewater with the content of 100mg/L is added with 5mL of oleylamine and 20mL of n-hexane, stirred for 1 hour, added with 2g of sodium hydroxide and stirred for 1 hour. The resulting solution was heated to 180 ℃ to effect a reaction. Reacting for 24 hours, cooling to room temperature to obtain an obviously layered solution, separating the lower layer to obtain purified water, and centrifugally separating the upper layer mixed solution to respectively obtain the normal hexane solvent containing complexing agent oleylamine and the nano particles.
FIG. 2 is an X-ray diffraction chart of the obtained nanoparticles, and it can be seen from the chart that the obtained nanoparticles have good crystallinity. The obtained n-hexane solvent containing complexing agent oleylamine can be recycled. And (4) detecting and analyzing the purified water separated after the reaction, wherein the content of nickel ions is lower than 1 mg/L. Hydrochloric acid is used for neutralization, so that the pH value of the purified water can be safely discharged after about 7.
Example 3
Taking Zn2+60mL of zinc-containing electroplating wastewater with the content of 105mg/L is added with 5mL of oleic acid and 20mL of n-hexane, stirred for 1 hour, added with 1g of sodium hydroxide and stirred for 1 hour. The resulting solution was heated to 170 ℃ to effect reaction. Reacting for 22 hours, cooling to room temperature to obtain an obviously layered solution, separating the lower layer to obtain purified water, and centrifugally separating the upper layer mixed solution to respectively obtain the normal hexane solvent containing complexing agent oleic acid and the nano particles.
FIG. 3 is a scanning electron micrograph of the nanoparticles obtained, from which it can be seen that the particles obtained have good dispersibility and a uniform size scale. The obtained normal hexane solvent containing complexing agent oleic acid can be recycled. And (4) detecting and analyzing the purified water separated after the reaction, wherein the content of zinc ions is lower than 1 mg/L. Hydrochloric acid is used for neutralization, so that the pH value of the purified water can be safely discharged after about 7.
Example 4
Taking Cr3+60mL of chromium-containing electroplating wastewater having a content of 105mg/L was added with 5mL of oleic acid and 20mL of acetone, stirred for 1 hour, added with 1.5g of sodium hydroxide, and stirred for 1 hour. The resulting solution was heated to 160 ℃ to effect a reaction. Reacting for 24 hours, cooling to room temperature to obtain obviously layered solution, separating the lower layer to obtain purified water, and centrifugally separating the upper layer mixed solution to respectively obtain the acetone solvent containing complexing agent oleic acid and the nano particles.
The obtained acetone solvent containing complexing agent oleic acid can be recycled. And (4) detecting and analyzing the purified water obtained after the reaction, wherein the content of chromium ions is lower than 1 mg/L. Hydrochloric acid is used for neutralization, so that the pH value of the purified water can be safely discharged after about 7.
Example 5
Taking Cd2+Cadmium-containing electroplating wastewater 6 with content of 105mg/L0mL, 5mL of sodium oleate and 20mL of petroleum ether were added thereto, and stirring was continued for 1 hour, and 2.1g of sodium hydroxide was added thereto and stirring was continued for 1 hour. The resulting solution was heated to 200 ℃ to effect a reaction. Reacting for 18 hours, cooling to room temperature to obtain obviously layered solution, separating the lower layer to obtain purified water, and centrifugally separating the upper layer mixed solution to respectively obtain petroleum ether solvent containing complexing agent sodium oleate and nano particles.
The petroleum ether solvent containing complexing agent sodium oleate can be recycled. And (4) detecting and analyzing the purified water after reaction, wherein the content of cadmium ions is lower than 1 mg/L. Hydrochloric acid is used for neutralization, so that the pH value of the purified water can be safely discharged after about 7.
Example 6
Taking Zn2+60mL of zinc-containing electroplating wastewater with the content of 105mg/L is added with 5mL of octadecene and 20mL of n-hexane, stirred for 1 hour, added with 2g of sodium hydroxide and stirred for 1 hour. The resulting solution was heated to 180 ℃ to effect a reaction. Reacting for 24 hours, cooling to room temperature to obtain an obviously layered solution, separating the lower layer to obtain purified water, and centrifugally separating the upper layer mixed solution to respectively obtain the n-hexane solvent containing the complexing agent octadecene and the nano particles.
The obtained n-hexane solvent containing complexing agent octadecene can be recycled. And (4) detecting and analyzing the purified water after reaction, wherein the content of zinc ions is lower than 1 mg/L. Hydrochloric acid is used for neutralization, so that the pH value of the purified water can be safely discharged after about 7.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A method for preparing nano particles from heavy metal wastewater is characterized by comprising the following steps:
adding a complexing agent and a phase transfer agent into the heavy metal wastewater, stirring and mixing uniformly, then adding alkali to adjust the pH value to be alkaline, heating the obtained mixed solution to 100-230 ℃ for solvothermal reaction, and cooling to room temperature after the reaction is finished to obtain an obviously layered phase transfer solution with a lower layer of purified water and an upper layer of nano particles and the complexing agent; separating the lower layer to obtain purified water, and centrifugally separating the phase transfer solution containing the nanoparticles and the complexing agent in the upper layer to obtain a phase transfer solvent containing the complexing agent and nanoparticles;
the complexing agent is selected from at least one of sodium oleate, oleic acid, oleylamine and octadecene;
the phase transfer agent is selected from one or a mixture of more than two of n-hexane, petroleum ether, trichloromethane and acetone;
the alkali is at least one selected from sodium hydroxide, potassium hydroxide, sodium carbonate, sodium dihydrogen phosphate, calcium hydroxide, magnesium hydroxide and ammonia water.
2. The method for preparing nano particles from heavy metal wastewater as claimed in claim 1, wherein the method comprises the following steps: the content of heavy metals in the heavy metal wastewater is 60-5000 mg/L.
3. The method for preparing nano particles from heavy metal wastewater according to claim 1 or 2, wherein the method comprises the following steps: the heavy metal wastewater is electroplating wastewater containing at least one heavy metal ion of nickel, zinc, chromium, cadmium and copper.
4. The method for preparing nano particles from heavy metal wastewater as claimed in claim 1, wherein the method comprises the following steps: the mass ratio of the heavy metal wastewater to the complexing agent to the phase transfer agent is 60 (1-80) to 10-200.
5. The method for preparing nano particles from heavy metal wastewater as claimed in claim 1, wherein the method comprises the following steps: the mass ratio of the addition amount of the alkali to the heavy metal wastewater is (1-21) to (1-120).
6. The method for preparing nano particles from heavy metal wastewater as claimed in claim 1, wherein the method comprises the following steps: the solvothermal reaction time is 3-48 hours.
7. The method for preparing nano particles from heavy metal wastewater as claimed in claim 1, wherein the method comprises the following steps: and the phase transfer solvent containing the complexing agent obtained by separation is recycled.
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| CN113106254B (en) * | 2021-03-24 | 2022-07-05 | 华南理工大学 | Method for extracting nano noble metal and fine iron powder from municipal sludge |
| CN113120977B (en) * | 2021-04-30 | 2023-06-23 | 佛山经纬纳科环境科技有限公司 | Method for preparing nickel ferrite nano material from nickel-containing ferroelectric plating wastewater and application thereof |
| CN113735363A (en) * | 2021-10-15 | 2021-12-03 | 嘉兴学院 | Treatment method of chrome tanning waste liquid |
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| CN103693789B (en) * | 2013-12-09 | 2016-01-13 | 华南师范大学 | The resource recycle method of heavy metal in a kind of heavy metal wastewater thereby |
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Denomination of invention: A method for preparing nanoparticles from heavy metal wastewater Effective date of registration: 20211125 Granted publication date: 20210525 Pledgee: Guangdong Nanhai Rural Commercial Bank branch branch of Limited by Share Ltd. Pledgor: Foshan Jingwei NACO Environmental Technology Co.,Ltd. Registration number: Y2021440000352 |