CN114262795A - Water-in-oil emulsion and preparation method and application thereof - Google Patents
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Abstract
The invention belongs to the technical field of metal recovery, and particularly relates to a water-in-oil emulsion as well as a preparation method and application thereof. The invention provides a water-in-oil emulsion, which comprises kerosene, a surfactant, a carrier and an internal water phase solution; the water-in-oil emulsion takes kerosene as an oil phase and takes an internal water phase solution as a water phase; the surfactant comprises a hydrophilic group and a lipophilic group; the hydrophilic group is connected with the internal water phase solution, and the lipophilic group is connected with kerosene; the carrier moves in a shuttling way in an oil phase and an aqueous phase; the carrier comprises isoamyl acetate, alkyl phosphonic acid, dioctyl phosphate or methyl isobutyl ketone; the internal aqueous phase solution comprises a selenide solution and/or a sulfide solution. The water-in-oil emulsion provided by the invention can realize the directional recovery of metal.
Description
Technical Field
The invention belongs to the technical field of metal recovery, and particularly relates to a water-in-oil emulsion as well as a preparation method and application thereof.
Background
With the rapid development of the electronic information industry, the performance of electronic products is continuously improved, and the updating speed of the electronic products is faster and faster. Along with the shorter and shorter service life of electronic products, electronic wastes, especially waste circuit boards, are increasing year by year, and become one of the sources of the electronic wastes. The rapid development of electronic information technology generates a great deal of electronic garbage, and if the electronic garbage is not treated properly, the electronic garbage will cause great harm to the environment.
The publication No. CN102172597A discloses a method for recovering the total value of a waste circuit board, which obtains metal powder and non-metal powder by crushing, magnetic separation and flotation. Although the metal can be recovered from the circuit board, the various metals in the metal powder obtained are mixed together, and the directional recovery of the metal cannot be realized.
Disclosure of Invention
The invention aims to provide a water-in-oil emulsion, which can realize the directional recovery of metal when being applied to the recovery of metal from a circuit board.
In order to achieve the above object, the present invention provides a water-in-oil emulsion comprising kerosene, a surfactant, a carrier and an internal aqueous phase solution;
the water-in-oil emulsion takes kerosene as an oil phase and takes an internal water phase solution as a water phase;
the surfactant comprises a hydrophilic group and a lipophilic group; the hydrophilic group is connected with the internal water phase solution, and the lipophilic group is connected with kerosene;
the carrier moves in a shuttling way in an oil phase and an aqueous phase;
the carrier comprises isoamyl acetate, alkyl phosphonic acid, dioctyl phosphate or methyl isobutyl ketone;
the internal aqueous phase solution comprises a selenide solution and/or a sulfide solution.
Preferably, the surfactant comprises one or more of span 85, amino acid ester, sulfonated polybutadiene, polyethylene glycol octyl phenyl ether and tween 80.
Preferably, the concentration of the internal water phase solution is 0.1-0.5 mol/L.
Preferably, the volume ratio of the kerosene, the surfactant and the carrier is (6-7): (1-3): 1;
the volume ratio of the total volume of the kerosene, the surfactant and the carrier to the volume of the internal water phase solution is 1-2: 1 to 2.
The invention also provides a preparation method of the water-in-oil emulsion in the technical scheme, which comprises the following steps:
mixing kerosene, a surfactant, a carrier and an internal water phase solution to obtain the water-in-oil emulsion.
Preferably, the mixing is carried out under stirring;
the stirring speed is 2500-3500 rpm, and the time is 8-12 min.
The invention also provides the application of the water-in-oil emulsion in the technical scheme or the water-in-oil emulsion prepared by the preparation method in the technical scheme in metal recovery.
Preferably, the application comprises the following steps:
providing a solution containing metal ions; the metal ions in the solution containing metal ions include copper ions, nickel ions, zinc ions, and gold ions.
And mixing the water-in-oil emulsion and the solution containing the metal ions, and then sequentially performing demulsification and separation to obtain the recovered metal.
Preferably, the concentration of the solution containing the metal ions is 0.5-2.0 g/L;
the volume ratio of the solution containing metal ions to the water-in-oil emulsion is 1-3: 1.
preferably, the mixing is carried out under stirring;
the stirring speed is 300-700 rpm, and the time is 10-20 min.
The invention provides a water-in-oil emulsion, which comprises kerosene, a surfactant, a carrier and an internal water phase solution; the water-in-oil emulsion takes kerosene as an oil phase and takes an internal water phase solution as a water phase; the surfactant comprises a hydrophilic group and a lipophilic group; the hydrophilic group is connected with the internal water phase solution, and the lipophilic group is connected with kerosene; the carrier moves in a shuttling way in an oil phase and an aqueous phase; the carrier comprises isoamyl acetate, alkyl phosphonic acid, dioctyl phosphate or methyl isobutyl ketone; the internal aqueous phase solution comprises a selenide solution and/or a sulfide solution. The invention takes kerosene as an oil phase and an internal water phase solution as a water phase to obtain a water-in-oil emulsion, wherein a carrier moves in a shuttling way in the oil phase and the water phase, and after the carrier is contacted with metal ions, specific directional combination is generated, and after the carrier combined with the metal ions is contacted with the internal water phase solution, the metal ions on the carrier react with the internal water phase solution, so that the directional transfer of the metal ions is realized. When the water-in-oil emulsion provided by the invention is applied to metal recovery, the metal can be directionally recovered.
Drawings
FIG. 1 is a schematic diagram of metal recovery using a water-in-oil emulsion provided by the present invention;
FIG. 2 is an SEM photograph of copper sulfide obtained in example 1;
FIG. 3 is an XRD pattern of copper sulfide obtained in example 1;
FIG. 4 is a graph showing the results of the antibacterial test of copper sulfide obtained in example 1;
FIG. 5 is a graph showing the results of bacterial survival in the antibacterial test of copper sulfide obtained in example 1.
Detailed Description
The invention provides a water-in-oil emulsion, which comprises kerosene, a surfactant, a carrier and an internal water phase solution;
the water-in-oil emulsion takes kerosene as an oil phase and takes an internal water phase solution as a water phase;
the surfactant comprises a hydrophilic group and a lipophilic group; the hydrophilic group is connected with the internal water phase solution, and the lipophilic group is connected with kerosene;
the carrier moves in a shuttling way in an oil phase and an aqueous phase;
the carrier comprises isoamyl acetate, alkyl phosphonic acid, dioctyl phosphate or methyl isobutyl ketone;
the internal aqueous phase solution comprises a selenide solution and/or a sulfide solution.
In the present invention, all the components are commercially available products well known to those skilled in the art unless otherwise specified.
In the present invention, the carrier includes isoamyl acetate, alkyl phosphonic acid, dioctyl phosphate, or methyl isobutyl ketone. In the present invention, when the carrier is isoamyl acetate, the carrier can be specifically combined with copper ions; when the carrier is alkyl phosphonic acid, the carrier can be specifically combined with nickel ions; when the carrier is dioctyl phosphate, the carrier can be specifically combined with zinc ions; when the carrier is methyl isobutyl ketone, the carrier can be specifically combined with gold ions. In the invention, the carrier moves in a shuttling mode in an oil phase and a water phase, and the specific carrier is selected to be specifically combined with metal ions, so that the metal can be transferred directionally.
In the invention, the surfactant preferably comprises one or more of span 85, amino acid ester, sulfonated polybutadiene, polyethylene glycol octyl phenyl ether and tween 80; when the surfactant is two or more of the above specific choices, the specific material may be mixed at any ratio without any particular limitation in the present invention.
In the present invention, the internal aqueous phase solution preferably includes a selenide solution and/or a sulfide solution; when the inner water phase solution is a selenide solution and a sulfide solution, the proportion of the selenide solution and the sulfide solution is not particularly limited, and the selenide solution and the sulfide solution can be mixed according to any proportion.
In the invention, the concentration of the internal aqueous phase solution is preferably 0.1-0.5 mol/L, more preferably 0.2-0.4 mol/L, and even more preferably 0.25-0.3 mol/L.
In the present invention, the water-in-oil emulsion further comprises a film stabilizer; the film stabilizer includes liquid paraffin or glycerin. In the present invention, the volume ratio of the film stabilizer to kerosene is preferably 1: 5-20, and more preferably 1: 7-15, more preferably 1: 10 to 12. In the present invention, the film stabilizer is dispersed in kerosene, and the stability of the water-in-oil emulsion can be further improved.
In the invention, the volume ratio of the kerosene, the surfactant and the carrier is preferably (6-7): (1-3): 1, more preferably (6.2 to 6.8): (1.2-2.8): 1, more preferably (6.4 to 6.6): (1.5-2.5): 1. in the invention, the volume ratio of the total volume of the kerosene, the surfactant and the carrier to the inner water phase solution is preferably 1-2: 1 to 2, and more preferably 1.2 to 1.8: 1.2 to 1.8, more preferably 1.4 to 1.6: 1.4 to 1.6.
The invention also provides a preparation method of the water-in-oil emulsion in the technical scheme, which comprises the following steps:
mixing kerosene, a surfactant, a carrier and an internal water phase solution to obtain the water-in-oil emulsion. In the present invention, the mixing is preferably performed under stirring; the rotation speed of the stirring is preferably 2500-3500 rpm, more preferably 2600-3300 rpm, and even more preferably 2800-3000 rpm; the time is preferably 8 to 12min, more preferably 9 to 11min, and still more preferably 10 min.
In the present invention, the mixing preferably comprises the steps of: and premixing the kerosene, the surfactant and the carrier, and remixing the obtained premix and the internal water phase solution.
In the present invention, the premixing is preferably performed under stirring; the rotation speed of the stirring is preferably 300-600 rpm, more preferably 350-550 rpm, and even more preferably 400-500 rpm; the time is preferably 10 to 60min, more preferably 15 to 55min, and still more preferably 20 to 50 min. In the present invention, the remixing is preferably performed under stirring; the rotation speed of the stirring is preferably 2500-3500 rpm, more preferably 2600-3300 rpm, and even more preferably 2800-3000 rpm; the time is preferably 8 to 10min, and more preferably 9 min.
The invention also provides the application of the water-in-oil emulsion in the technical scheme or the water-in-oil emulsion prepared by the preparation method in the technical scheme in metal recovery.
In the present invention, the application comprises the following steps:
providing a solution containing metal ions; the metal ions in the solution containing the metal ions comprise copper ions, nickel ions, zinc ions and gold ions;
and mixing the water-in-oil emulsion and the solution containing the metal ions, and then sequentially performing demulsification and separation to obtain the recovered metal.
In the present invention, when a wiring board is used as a raw material for providing a solution containing metal ions, the process for providing a solution containing metal ions preferably includes the steps of: and digesting the circuit board to obtain a solution containing metal ions.
Before the digestion, the invention also preferably comprises the step of crushing the circuit board. The process of the crushing treatment is not particularly limited in the present invention, and those well known to those skilled in the art may be used.
In the present invention, the digestion process preferably comprises the following steps: and mixing the circuit board obtained by crushing with a digestion reagent, and digesting.
In the invention, the digestion reagent preferably comprises concentrated nitric acid and hydrogen peroxide. In the invention, the mass concentration of the concentrated nitric acid is preferably 68%; the mass concentration of the hydrogen peroxide is preferably 30%. In the present invention, the volume ratio of the concentrated nitric acid to the hydrogen peroxide is preferably 1: 1.
in the invention, the dosage ratio of the circuit board to the digestion reagent is preferably 1 g: 10-40 mL, more preferably 1 g: 15-35 mL, more preferably 1 g: 20-30 mL.
The mixing process is not particularly limited in the present invention, and may be performed as is well known to those skilled in the art.
In the present invention, the digestion is preferably carried out under stirring; the rotation speed of the stirring is preferably 300-600 rpm, more preferably 350-550 rpm, and even more preferably 400-500 rpm. In the present invention, the digestion temperature is preferably 50 ℃ and the time is preferably 2 hours.
After the digestion is finished, the invention also preferably comprises the steps of cooling, separating and adjusting the pH value of the product in sequence.
The cooling and separation processes are not particularly limited in the present invention and may be those well known to those skilled in the art.
In the present invention, the pH value after the pH adjustment is preferably 5.
In the present invention, the metal ions in the metal ion-containing solution preferably include copper ions, nickel ions, zinc ions, and gold ions.
After the solution containing the metal ions is obtained, the water-in-oil emulsion and the solution containing the metal ions are mixed, and then emulsion breaking and separation are sequentially carried out to obtain the recovered metal.
In the present invention, the concentration of the metal ion-containing solution is preferably 0.5 to 2.0g/L, more preferably 0.8 to 1.8g/L, and still more preferably 1.0 to 1.5 g/L. In the invention, the volume ratio of the metal ion-containing solution to the water-in-oil emulsion is preferably 1-3: 1, more preferably 1.2 to 2.8: 1, more preferably 1.5 to 2.5: 1.
in the present invention, the mixing is preferably performed under stirring; the rotation speed of the stirring is preferably 300-700 rpm, more preferably 350-550 rpm, and even more preferably 400-500 rpm; the time is 10 to 20min, more preferably 12 to 18min, and still more preferably 14 to 16 min.
In the mixing process, metal ions and a specific carrier are subjected to specific directional combination, when the carrier combined with the metal ions performs shuttle motion in kerosene and contacts with an internal aqueous phase solution, the metal ions in the carrier react with the internal aqueous phase solution, and further the directional transfer of the metal can be realized, and a schematic diagram is shown in fig. 1.
The present invention also preferably includes allowing the mixed solution to stand and separate prior to the demulsification. In the present invention, an organic phase and an aqueous phase are obtained by standing and separating. In the invention, the standing time is preferably 2-4 h. The process of the present invention for the standing and separation is not particularly limited, and those well known to those skilled in the art can be used.
In the present invention, the demulsification process preferably comprises the following steps: mixing the obtained organic phase with a polar solvent, and performing centrifugal demulsification.
In the present invention, the polar solvent preferably includes water and/or ethanol. The amount of the polar solvent to be added and the mixing process in the present invention are not particularly limited, and those known to those skilled in the art can be used. In the invention, the rotation speed of the centrifugation is preferably 5000-8000 rpm, more preferably 5500-7500 rpm, and more preferably 6000-7000 rpm; the time is preferably 1-3 min, more preferably 1.2-2.8 min, and even more preferably 1.5-2.5 min; the number of centrifugation is preferably 2-3. .
The present invention does not require any particular separation process, and can be used as is well known to those skilled in the art.
After the separation is completed, the invention also preferably comprises cooling the solid obtained by the separation to obtain the recovered metal. In the present invention, the cooling mode is preferably natural airing.
In the present invention, the recovered metal is preferably present in the form of a sulfide or selenide.
In order to further illustrate the present invention, the following detailed description of a water-in-oil emulsion and its preparation method and application are provided in connection with the accompanying drawings and examples, which should not be construed as limiting the scope of the present invention.
Example 1
Taking 9mL of span 85, 7mL of isoamyl acetate, 44mL of kerosene and 60mL of sodium sulfide solution with the concentration of 0.2mol/L, and stirring for 10min at the rotating speed of 3000rpm to obtain a water-in-oil type emulsion;
mixing 2g of the crushed circuit board, 20mL of concentrated nitric acid and 20mL of hydrogen peroxide, stirring for 2h at a stirring speed of 300rpm in a water bath at 50 ℃ after heat release is finished, carrying out digestion reaction, standing and cooling after the reaction is finished, separating to obtain a supernatant, and adjusting the pH value of the supernatant to 5 to obtain a solution containing metal ions;
stirring 30mL of water-in-oil emulsion and 50mL of solution containing metal ions with the mass concentration of 2g/L at the rotating speed of 600rpm for 15 min; standing for 2h for layering, mixing the separated organic phase with 50mL of water, performing centrifugal separation at the rotating speed of 6000rpm for 2min, repeating the centrifugation for 2 times, and naturally drying the centrifuged solid to obtain the copper sulfide.
Example 2
Taking 6mL of span 85, 6mL of alkyl phosphonic acid, 6mL of liquid paraffin, 42mL of kerosene and 60mL of sodium sulfide solution with the concentration of 0.2mol/L, and stirring at the rotating speed of 3500rpm for 10min to obtain water-in-oil type emulsion;
mixing 2g of the crushed circuit board, 20mL of concentrated nitric acid and 20mL of hydrogen peroxide, stirring for 2h at a stirring speed of 300rpm in a water bath at 50 ℃ after heat release is finished, carrying out digestion reaction, standing and cooling after the reaction is finished, separating to obtain a supernatant, and adjusting the pH value of the supernatant to 5 to obtain a solution containing metal ions;
taking 30mL of water-in-oil emulsion and 60mL of solution containing metal ions with the mass concentration of 1.5g/L, and stirring for 15min at the rotating speed of 600 rpm; standing for 2h for layering, mixing the separated organic phase with 50mL of ethanol, performing centrifugal separation at the rotating speed of 6000rpm for 2min, repeating the centrifugation for 2 times, and naturally drying the centrifuged solid to obtain the nickel sulfide.
Example 3
Taking 8mL of amino acid ester, 8mL of dioctyl phosphate, 44mL of kerosene and 60mL of sodium sulfide solution with the concentration of 0.3mol/L, and stirring for 10min at the rotating speed of 3200rpm to obtain a water-in-oil type emulsion;
mixing 2g of the crushed circuit board, 20mL of concentrated nitric acid and 20mL of hydrogen peroxide, stirring for 2h at a stirring speed of 300rpm in a water bath at 50 ℃ after heat release is finished, carrying out digestion reaction, standing and cooling after the reaction is finished, separating to obtain a supernatant, and adjusting the pH value of the supernatant to 5 to obtain a solution containing metal ions;
taking 20mL of water-in-oil emulsion and 50mL of solution containing metal ions with the mass concentration of 1.8g/L, and stirring at the rotating speed of 600rpm for 12 min; standing for 2h for layering, mixing the separated organic phase with 50mL of ethanol, performing centrifugal separation at the rotating speed of 6000rpm for 2min, repeatedly centrifuging for 3 times, and naturally drying the centrifuged solid to obtain the zinc sulfide.
Performance testing
Test example 1
Scanning electron microscope tests are carried out on the copper sulfide obtained in the embodiment 1, and the test result is shown in fig. 2, it can be seen from fig. 2 that the synthesized copper sulfide has a disordered stacking two-dimensional flaky nano morphology, the length of the nano sheet is about 100-200 nm, and the thickness of the nano sheet is about 5-10 nm.
Test example 2
XRD testing of the copper sulfide obtained in example 1 is carried out, the test result is shown in figure 3, and from figure 3, the extracted copper sulfide is basically not different from the standard card, which also shows that the successful synthesis of the copper sulfide has extremely individual impurity peak probably because the copper sulfide contains trace amount of other metal impurities.
Test example 3
The copper sulfide obtained in example 1 was tested for antibacterial properties;
the test method comprises the following steps:
in a 50mL glass conical flask, 100. mu.L of E.coli (E.coli) bacteria cultured to log phase were resuspended in 10mL of physiological saline, and a copper sulfide sample was added to the conical flask at the experimental concentration (50. mu.g/mL). For the control group, physiological saline was used instead of copper sulfide.
After co-incubation of the bacteria with the sample at 37 ℃ for 30 minutes, a 808nm laser (1.5 w/cm) was used under near infrared light (NIR)2) Irradiating for 10 minutes, diluting the illuminated and non-illuminated bacterial liquid by 10000 times with physiological saline respectively, uniformly coating 100 mu L of diluted bacterial liquid on an LB agar plate, incubating for 24 hours in an incubator at 37 ℃, recording the number of CFU, and calculating the survival rate of bacteria. The result of the antibacterial test is shown in fig. 4, and it can be seen from fig. 4 that the copper sulfide recovered by the present invention has excellent antibacterial effect under illumination; the results of the survival rate of bacteria are shown in FIG. 5, and it can be seen from FIG. 5 that the antibacterial effect of the copper sulfide recovered by the present invention on Escherichia coli under light conditions is 85%.
Although the above embodiments have been described in detail, they are only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and all of the embodiments belong to the protection scope of the present invention.
Claims (10)
1. A water-in-oil emulsion is characterized by comprising kerosene, a surfactant, a carrier and an internal water phase solution;
the water-in-oil emulsion takes kerosene as an oil phase and takes an internal water phase solution as a water phase;
the surfactant comprises a hydrophilic group and a lipophilic group; the hydrophilic group is connected with the internal water phase solution, and the lipophilic group is connected with kerosene;
the carrier moves in a shuttling way in an oil phase and an aqueous phase;
the carrier comprises isoamyl acetate, alkyl phosphonic acid, dioctyl phosphate or methyl isobutyl ketone;
the internal aqueous phase solution comprises a selenide solution and/or a sulfide solution.
2. A water-in-oil emulsion according to claim 1, wherein said surfactant comprises one or more of span 85, amino acid ester, sulfonated polybutadiene, polyethylene glycol octylphenyl ether and tween 80.
3. The water-in-oil emulsion according to claim 1, wherein the concentration of said internal aqueous phase solution is 0.1 to 0.5 mol/L.
4. A water-in-oil emulsion according to claim 3, wherein the volume ratio of kerosene, surfactant and carrier is (6-7): (1-3): 1;
the volume ratio of the total volume of the kerosene, the surfactant and the carrier to the volume of the internal water phase solution is 1-2: 1 to 2.
5. A process for the preparation of a water-in-oil emulsion as claimed in any one of claims 1 to 4, comprising the steps of:
mixing kerosene, a surfactant, a carrier and an internal water phase solution to obtain the water-in-oil emulsion.
6. The production method according to claim 5, wherein the mixing is performed under stirring;
the stirring speed is 2500-3500 rpm, and the time is 8-12 min.
7. Use of a water-in-oil emulsion according to any one of claims 1 to 4 or a water-in-oil emulsion obtained by the preparation process according to claim 5 or 6 for metal recovery.
8. The application according to claim 7, characterized in that it comprises the following steps:
providing a solution containing metal ions; the metal ions in the solution containing the metal ions comprise copper ions, nickel ions, zinc ions and gold ions;
and mixing the water-in-oil emulsion and the solution containing the metal ions, and then sequentially performing demulsification and separation to obtain the recovered metal.
9. The use according to claim 8, wherein the concentration of the solution containing metal ions is 0.5 to 2.0 g/L;
the volume ratio of the solution containing metal ions to the water-in-oil emulsion is 1-3: 1.
10. use according to claim 8, wherein the mixing is carried out under stirring;
the stirring speed is 300-700 rpm, and the time is 10-20 min.
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