CN110339592B - Heavy metal ion extracting agent based on fatty acid, preparation method and extraction method - Google Patents
Heavy metal ion extracting agent based on fatty acid, preparation method and extraction method Download PDFInfo
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- CN110339592B CN110339592B CN201910661846.2A CN201910661846A CN110339592B CN 110339592 B CN110339592 B CN 110339592B CN 201910661846 A CN201910661846 A CN 201910661846A CN 110339592 B CN110339592 B CN 110339592B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Abstract
The present disclosure provides a fatty acid-based heavy metal ion extractant, a preparation method and an extraction method, wherein the preparation method comprises the steps of uniformly mixing fatty acid and an alkali solution, and reacting to obtain the fatty acid-based heavy metal ion extractant; the fatty acid is one or more of caproic acid, heptanoic acid, caprylic acid and nonanoic acid. In the heavy metal ion extracting agent provided by the disclosure, fatty acid salt and high-valence heavy metal ions to be extracted act, the high-valence heavy metal ions are combined with fatty acid radicals, products are dissolved in fatty acid to form an upper phase, the upper phase is extracted from a lower phase water phase, separation can be realized through simple liquid separation, the operation is simple, and the removal speed is high.
Description
Technical Field
The disclosure belongs to the field of wastewater treatment and metal recovery, and relates to a fatty acid-based heavy metal ion extracting agent, a preparation method and an extraction method.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
With the development of industrialization, people pay more and more attention to resources and environmental problems. In the production process of chemical industry and metal smelting industry, a large amount of waste water is generated, and the waste water still contains a large amount of metal ions, particularly heavy metal ions, so that not only can serious environmental pollution be caused, but also the resource is greatly wasted. Therefore, it is very important to remove and recover metal ions from wastewater.
At present, the purification method of the wastewater containing heavy metal ions comprises a chemical method and a physical method. Chemical methods are the main methods at present, including chemical precipitation methods and electrolytic methods, and are suitable for wastewater containing heavy metal ions with higher concentration. The physical methods mainly include solvent extraction separation, ion exchange method, membrane separation technology and adsorption method. The inventor of the present disclosure has studied to understand that: the ion exchange method adopts ion exchange resin, chelating agent and the like to exchange with metal ions, and the ion exchanger has unstable chemical property, easy failure and higher regeneration operation cost; the membrane separation technology utilizes a special semipermeable membrane to separate or concentrate a solvent and a solute under the action of external pressure, and the problems of electrode polarization, scaling, corrosion and the like exist in the process of operation, so that the application of the solvent and the solute is limited; the adsorption method utilizes the adsorption effect of porous solid substances to remove heavy metal ions in water, has high removal rate, but has low regeneration efficiency and high price, so the application is limited. Compared with the prior art, the solvent extraction method is more convenient to operate. The method generally adopts a proper complexing agent to combine with heavy metal ions, then a single solvent which is not soluble in water or a mixed solvent consisting of a plurality of solvents is used for dissolving a complexing system combined with the heavy metals, and the water phase can be purified by separating liquid. The method generally needs two or more substances, solvent loss exists in the extraction process, and the energy consumption in the regeneration process is large. In recent years, much attention has been paid to ionic liquid extraction methods which employ an appropriate ionic liquid, extract metal ions into an ionic liquid phase by binding them to some of the ions in the ionic liquid, and then separate the liquid. The ionic liquid selected by the method generally has higher viscosity, certain difficulty exists in large-scale operation, the efficiency is influenced, and the cost is higher when the ionic liquid is used as an extracting agent.
Disclosure of Invention
In order to overcome the defects in the prior art, the purpose of the present disclosure is to provide a fatty acid-based heavy metal ion extraction agent, a preparation method and an extraction method, which can rapidly and efficiently remove heavy metal ions in wastewater, and have the advantages of environmental protection, low cost, simple operation, etc.
In order to achieve the purpose, the technical scheme of the disclosure is as follows:
in a first aspect, a fatty acid-based heavy metal ion extractant comprises a fatty acid and a fatty acid salt, wherein the fatty acid is one or more of caproic acid, heptanoic acid, caprylic acid and pelargonic acid, the fatty acid salt is one or more of caproate, heptanoate, caprylate and pelargonic acid, and the cation of the fatty acid salt is sodium ion, potassium ion or ammonium ion.
In the heavy metal ion extracting agent provided by the disclosure, fatty acid salt and high-valence heavy metal ions to be extracted act, the high-valence heavy metal ions are combined with fatty acid radicals, products are dissolved in fatty acid to form an upper phase, the upper phase is extracted from a lower phase water phase, separation can be realized through simple liquid separation, the operation is simple, and the removal speed is high. The caproic acid, the heptanoic acid, the octanoic acid and the nonanoic acid provided by the method are liquid fatty acids and cannot be mutually dissolved with water, so that the aim of extracting heavy metal ions in water is fulfilled.
In a second aspect, a preparation method of a fatty acid-based heavy metal ion extractant is obtained by uniformly mixing fatty acid and alkali solution and reacting; the fatty acid is one or more of caproic acid, heptanoic acid, caprylic acid and nonanoic acid.
In the present disclosure, the alkali solution causes the fatty acid and the alkali to perform a neutralization reaction, thereby preparing the fatty acid-based heavy metal ion extractant.
In a third aspect, a fatty acid-based heavy metal ion extraction method is provided, wherein the fatty acid-based heavy metal ion extraction agent or the extraction agent obtained by the fatty acid-based heavy metal ion extraction agent preparation method is added into wastewater containing heavy metal ions, the mixture is uniformly mixed and then is kept stand to separate into two phases, the heavy metal ions in the wastewater are extracted into an upper fatty acid phase, and the two phases are separated to remove the heavy metal ions in the wastewater.
According to the method, in the process of treating the wastewater containing the heavy metal ions, other organic solvents are not needed, the fatty acid is environment-friendly, and secondary pollution to the wastewater is avoided.
The essence of the extraction process disclosed by the invention is that fatty acid radicals and heavy metal ions are combined to form a water-insoluble substance, so that the distribution coefficient of two liquid phases does not exist, a complex extraction process is not needed in the process, the mixing and stirring are simple, the whole process is very quick and can be completed within half an hour, and compared with the traditional liquid-liquid extraction method, the contact and balance for a longer time are greatly saved by the method disclosed by the invention.
And fourthly, adding acid into the upper phase obtained by the fatty acid-based heavy metal ion extraction method for acidification, standing for layering, and separating to obtain an upper liquid phase, namely the recovered fatty acid.
The beneficial effect of this disclosure does:
1) the extraction agent disclosed by the invention is utilized to remove heavy metal ions in wastewater quickly. After the extractant is added and stirred, the phase separation is carried out within half an hour, and the heavy metal ions are extracted more thoroughly.
2) The extraction process using the extractant of the present disclosure only needs one organic substance of fatty acid, which is used as both the extractant and the solvent, and no additional organic solvent is needed.
3) The extraction agent has high removal rate. Under appropriate conditions, Pb2+、Cd2+、Hg2+、Cr3+、Cu2+、Ni2+、Zn2+The ion removal rate can be higher than 99 percent, and the Cd content is2+Can reach 99.96 percent, the residual quantity in the waste water is lower than 0.5ppm, and the national discharge requirement standard is met.
4) The cost of using the extractant of the present disclosure is low. The fatty acid is a common chemical raw material and has low price. And can be repeatedly used, and the regeneration process is simple and convenient.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure and are not to limit the disclosure.
FIG. 1 is a photograph of a sample obtained by mixing an extracting agent prepared in example 3 of the present disclosure and an aqueous solution containing different kinds of heavy metal ions in reaction amounts, wherein A is Ni2+B is Ag+C is Cd2+；
FIG. 2 shows Cd in the extraction water by the extractant prepared in example 3 of the present disclosure2+Then, the photo of the process of recovering the heptanoic acid is carried out, A is Cd in the extracted water2+The subsequent photograph, B is a photograph after recovering heptanoic acid, and in A, it can be seen that the sample is inclined at a certain angle because the viscosity of the oil phase in which cadmium heptanoate is dissolved is very highLarge, the liquid level does not change along with the inclination, and the angle between the liquid level and the pipe wall is still 90 degrees; b, when hydrochloric acid is added, cadmium heptanoate reacts with cadmium heptanoate to generate heptanoic acid and Cd2+，Cd2+Returning to the lower water phase, the upper heptanoic acid phase has low viscosity, and the upper and lower liquid phases are horizontal.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular is intended to include the plural unless the context clearly dictates otherwise. Furthermore, it will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
In view of the defects of easy solvent loss, complex regeneration process and the like of the solvent extraction method, and the defects of high cost, low efficiency and the like of the ionic liquid extraction method, the disclosure provides a fatty acid-based heavy metal ion extractant, a preparation method and an extraction method.
In an exemplary embodiment of the present disclosure, a fatty acid-based heavy metal ion extractant is provided, which includes a fatty acid and a fatty acid salt, wherein the fatty acid is one or more of caproic acid, enanthic acid, caprylic acid and pelargonic acid, the fatty acid salt is one or more of caproate, enanthic acid salt, caprylic acid salt and pelargonic acid salt, and a cation of the fatty acid salt is sodium ion, potassium ion or ammonium ion.
In the heavy metal ion extracting agent provided by the disclosure, fatty acid salt and high-valence heavy metal ions to be extracted act, the high-valence heavy metal ions are combined with fatty acid radicals, products are dissolved in fatty acid to form an upper phase, the upper phase is extracted from a lower phase water phase, separation can be realized through simple liquid separation, the operation is simple, and the removal speed is high.
In one or more embodiments of this embodiment, the fatty acid salt is 2 to 60% of the total molar amount of fatty acid and fatty acid salt.
In another embodiment of the disclosure, a preparation method of a fatty acid-based heavy metal ion extractant is provided, wherein fatty acid and alkali solution are uniformly mixed and obtained after reaction; the fatty acid is one or more of caproic acid, heptanoic acid, caprylic acid and nonanoic acid.
In the present disclosure, the alkali solution causes the fatty acid and the alkali to perform a neutralization reaction, thereby preparing the fatty acid-based heavy metal ion extractant.
The base in the present disclosure is a compound that dissolves in water to give a pH of greater than 7, e.g., NaOH, KOH, ammonia, Na2CO3And the like.
In one or more embodiments of this embodiment, the alkali solution is a sodium hydroxide solution, a potassium hydroxide solution, or ammonia. These alkaline solutions are more basic and are susceptible to complete reaction with fatty acids to form the corresponding salts.
In one or more embodiments of this embodiment, the molar ratio of fatty acid to base is 1:0.05 to 0.6.
In a third embodiment of the present disclosure, a fatty acid-based heavy metal ion extraction method is provided, in which the fatty acid-based heavy metal ion extractant or the extractant obtained by the fatty acid-based heavy metal ion extractant preparation method is added into wastewater containing heavy metal ions, the mixture is uniformly mixed and then left to stand to separate into two phases, the heavy metal ions in the wastewater are extracted into an upper fatty acid phase, and the liquid separation is performed to remove the heavy metal ions in the wastewater.
According to the method, in the process of treating the wastewater containing the heavy metal ions, other organic solvents are not needed, the fatty acid is environment-friendly, and secondary pollution to the wastewater is avoided.
The essence of the extraction process disclosed by the invention is that fatty acid radicals are combined with heavy metal ions to form a water-insoluble substance, so that the distribution coefficient of two liquid phases does not exist, a complex extraction process is not needed in the process, simple mixing and stirring are carried out, the whole process is very quick and can be completed within half an hour, and compared with the traditional liquid-liquid extraction method, the method disclosed by the invention has the advantage that the treatment time is greatly saved.
The heavy metal ion is Pb2+、Cd2+、Hg2+、Cr3+、Cu2+、Ni2+、Co2+、Mn2+、Zn2+、Fe3+、Ba2 +、Sr2+、Zn2+、Ca2+、Ag+、Pd2+And lanthanide metal ions.
In one or more embodiments of the present disclosure, the pH of the wastewater containing heavy metal ions is adjusted to 3 to 7, and then the extractant is added.
In one or more embodiments of the present disclosure, the volume ratio of the extractant to the wastewater is 1:1 to 20.
In a fourth embodiment of the present disclosure, an acid is added to the upper phase obtained by the fatty acid-based heavy metal ion extraction method for acidification, standing for layering, and the upper liquid phase obtained by liquid separation is the recovered fatty acid.
In one or more embodiments of this embodiment, the acid is hydrochloric acid, sulfuric acid, nitric acid, or acetic acid.
In one or more embodiments of this embodiment, the acid is added in the same molar amount as the fatty acid salt or the base.
In order to make the technical solutions of the present disclosure more clearly understood by those skilled in the art, the technical solutions of the present disclosure will be described in detail below with reference to specific embodiments.
Example 1:
adding 1.4mL of 2mol/L NaOH solution containing 0.0028mol NaOH to 5mL (about 0.028mol) of heptanoic acid, i.e., the molar ratio of nonanoic acid to NaOH is about 10:1, and shaking to form a mixed solution; the mixture was added to 10mL of a solution containing 0.12mol/L of copper ions (Cu)2+) The pH of the water phase is adjusted to 6.0, and the mixture is stirred vigorously; standing and separating liquid, and Ni in wastewater2+I.e., removed, with a removal rate of 99.60%.
Example 2:
adding 2.4mL of 2mol/L NaOH solution into 5mL (about 0.032mol) of caprylic acid, wherein the NaOH content is 0.0048mol, namely the molar ratio of the caprylic acid to the NaOH is about 10:1.5, and oscillating to form a mixed solution; the mixture was added to 20mL of a solution containing 0.10mol/L of mercury ions (Hg)2+) The pH of the water phase is adjusted to 6.0, and the mixture is stirred vigorously; standing for liquid separation, wherein Hg in wastewater2+I.e., removed, with a removal rate of 95.34%.
Example 3:
adding 5.0mL of 2mol/L NaOH solution into 5mL (about 0.034mol) of heptanoic acid, wherein the NaOH solution contains 0.010mol, namely the molar ratio of the heptanoic acid to the NaOH is about 10:3, and oscillating to form a mixed solution; the mixed solution was added to 10mL of each of nickel ion (Ni) containing solutions2+) Lead ion (Pb)2+) Silver ion (Ag)+) Cadmium ion (Cd)2+) The metal ion concentrations in the aqueous solution of (1) were 0.4mol/L, 0.8mol/L, and 0.4mol/L, the pH of the aqueous phase after mixing was adjusted to 7.0, 5.5, and 6.0, respectively, the solution was vigorously stirred, and then left to separate, whereby the metal ions were recovered and removed, and the removal rates were 98.28%, 94.58%, 95.54%, and 98.57%, respectively. In this example with Ni2+、Ag+、Cd2+As shown in FIG. 1, the resulting phase-separated sample showed that heptanoate was bound to metal ions (Ni) in the lower phase water2+、Ag+、Cd2+) Then the sodium heptanoate is extracted to the upper oil phase by the heptanoic acid to form a viscous mixture, which shows that the sodium heptanoate is combined with the heavy metal ions to form a water-insoluble salt which is dissolved in the heptanoic acid on the upper phase, so that the metal ions are extracted from the water phase and removed, thereby realizing the removal of the heavy metal ions in the water.
Example 4:
adding 5.9mL of 2mol/L NaOH solution into 5mL (about 0.039mol) of pelargonic acid, wherein the NaOH content is 0.0118mol, namely the molar ratio of pelargonic acid to NaOH is about 10:3, and oscillating to form a mixed solution; the mixture was added to 50mL of a solution containing 0.10mol/L of cobalt ion (Co)2+) The pH of the aqueous phase of (1) is adjusted to 5.0, and the mixture is stirred vigorously; standing and separating liquid, and Co in wastewater2+Namely, the removal rate was 98.86%.
Example 5:
cd was extracted into the upper layer separated in example 32+Adding 10.2mL of 1.0mol/L hydrochloric acid into the heptanoic acid phase, stirring or oscillating, and standing to separate into an oil/water phase; separating the upper phase to recover the corresponding heptanoic acid.
The extractant recovery process is shown in figure 2: the upper layer in the sample is extracted Cd2+Heptanoic acid phase (II) with lower layer of Cd2+After hydrochloric acid is added into the extracted water phase and oscillation is carried out, cadmium on the upper layer is quickly transferred to the water phase on the lower layer, and the recovery of the extractant heptanoic acid is realized.
In fig. 2A, the sample is tilted at an angle, and the viscosity of the oil phase with cadmium heptanoate dissolved therein is high, so that the liquid level of the oil phase does not change along with the tilt and is still at an angle of 90 degrees with the tube wall. FIG. 2B shows the reaction of cadmium heptanoate with hydrochloric acid to produce heptanoic acid and Cd2+，Cd2+Returning to the lower water phase, the upper heptanoic acid phase has low viscosity, and the upper and lower liquid phases are horizontal.
The above description is only a preferred embodiment of the present disclosure and is not intended to limit the present disclosure, and various modifications and changes may be made to the present disclosure by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present disclosure should be included in the protection scope of the present disclosure.
Claims (8)
1. A fatty acid-based heavy metal ion extractant is characterized by comprising a fatty acid and a fatty acid salt, wherein the fatty acid is one or more of caproic acid, heptanoic acid, caprylic acid and pelargonic acid, the fatty acid salt is one or more of caproate, heptanoate, caprylate and pelargonic acid, and the cation of the fatty acid salt is sodium ion, potassium ion or ammonium ion.
2. The fatty acid-based heavy metal ion extractant according to claim 1, wherein the fatty acid salt is 2 to 60% of the total molar amount of the fatty acid and the fatty acid salt.
3. A preparation method of a fatty acid-based heavy metal ion extractant is characterized in that fatty acid and alkali solution are uniformly mixed and reacted to obtain the heavy metal ion extractant; the fatty acid is one or more of caproic acid, heptanoic acid, caprylic acid and nonanoic acid.
4. The method of claim 3, wherein the alkali solution is selected from the group consisting of sodium hydroxide solution, potassium hydroxide solution, and ammonia water.
5. The method according to claim 3, wherein the molar ratio of the fatty acid to the alkali is 1:0.05 to 0.6.
6. A fatty acid-based heavy metal ion extraction method is characterized in that the fatty acid-based heavy metal ion extraction agent disclosed in claim 1 or 2 or the extraction agent obtained by the preparation method of the fatty acid-based heavy metal ion extraction agent disclosed in any one of claims 3 to 5 is added into wastewater containing heavy metal ions, the mixture is uniformly mixed and then stands to separate into two phases, the heavy metal ions in the wastewater are extracted into an upper fatty acid phase, and the two phases are separated to remove the heavy metal ions in the wastewater.
7. The fatty acid-based extraction method of heavy metal ions according to claim 6, wherein the pH of the wastewater containing heavy metal ions is adjusted to 3 to 7, and then the extractant is added.
8. The fatty acid-based heavy metal ion extraction method of claim 7, wherein the volume ratio of the extraction agent to the wastewater is 1:1 to 20.
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| SK4912001A3 (en) * | 2001-04-10 | 2002-11-06 | Jozef Siska | Extraction agent and method for the extraction of metals, ammonium and amines from waters |
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