CN111961355A - Polymer-coated vanadium-titanium waste residue nano particle and preparation method thereof - Google Patents
Polymer-coated vanadium-titanium waste residue nano particle and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
Abstract
The invention provides a polymer-coated vanadium-titanium waste residue nano particle and a preparation method thereof, wherein the preparation method comprises the following steps: mixing vanadium-titanium waste residues with a hydrophilic polymer solution, then adjusting the pH value of the solution to 9-13, then transferring the mixed solution into a ball mill for ball milling reaction, washing a ball milling product to be neutral by using an acid solution, drying, and finally ultrasonically dispersing the dried product in water to obtain the vanadium-titanium composite material. The method adopts vanadium-titanium waste residues as raw materials to prepare the nano particles, changes the vanadium-titanium waste residues into valuables, adopts a normal-temperature ball milling method in the preparation process, has mild reaction conditions, simple technical route and easy large-scale production, meets the requirements of large using amount and low cost of the nano particles, and can greatly expand the application field of the nano particles.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a polymer-coated vanadium-titanium waste residue nano particle and a preparation method thereof.
Background
The vanadium-titanium mineral resources in Panxi areas are rich, however, after the vanadium-titanium resources are mined and refined, a large amount of waste residues can be generated after titanium, vanadium, iron and other elements and oxides thereof are continuously recovered from the generated tailings. The generated vanadium-titanium waste residues are accumulated like a mountain, so that not only is land resource occupied, but also serious pollution is caused to the ecological environment, the ecological environment and water resources in the Jinshajiang upstream area are threatened, and a large amount of accumulated waste residues also have the risk of collapsing and leaking the slag dam and contain great potential safety hazards.
In recent years, the vanadium-titanium waste slag is mainly used as an inorganic filler and added into cement mixtures or concrete for preparing building bricks. However, the utilization rate of the vanadium-titanium waste residue is still less than 50%, and the accumulation amount thereof is still continuously increased year by year, so that the high-efficiency utilization and high-value-added utilization of the vanadium-titanium waste residue are urgently required to be explored.
The prepared nano-grade filler and nano-particles have wide application value in the fields of functional nano-materials and nano-reinforcing materials, for example, the nano-grade titanium dioxide filler is widely applied to the fields of photocatalysis, functional fibers, plastics, coatings, paints and the like. However, the vanadium-titanium industrial waste residue is difficult to obtain nano-scale particles through simple dry grinding, and the problem that how to prepare the nano-filler capable of being stably dispersed in a polymer mechanism is difficult to solve at present is also caused by the high specific surface area of the nano-particles.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a polymer-coated vanadium-titanium waste residue nanoparticle and a preparation method thereof, which can effectively solve the problem that vanadium-titanium industrial waste residue is difficult to stably disperse in a nano filler in a polymer in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of polymer-coated vanadium-titanium waste residue nanoparticles comprises the following steps:
mixing vanadium-titanium waste residues with a hydrophilic polymer solution according to a mass ratio of 1-3:200, adjusting the pH value of the solution to 9-13, transferring the mixed solution into a ball mill for ball milling reaction, washing a ball milling product with an acid solution to be neutral, drying, and finally ultrasonically dispersing the dried product in water to obtain the vanadium-titanium composite material.
Further, the concentration of the hydrophilic polymer solution is 1 to 5 wt%.
Further, the hydrophilic polymer is polyvinyl alcohol, polyethylene glycol, polyacrylate, polyacrylamide, polystyrene sulfonate, polyvinyl benzyl trimethylamine salt, polyvinylpyrrolidone, poly 2-acrylamide-2-methylpropanesulfonic acid or poly dimethylamino ethyl methacrylate quaternary ammonium salt. The hydrophilic polymer solution is prepared by dissolving hydrophilic polymer in solvent, wherein the solvent for dissolving polymer is one or mixture of two of water, N-dimethylformamide, N-methylpyrrolidone, ethyl acetate, tetrahydrofuran, ethanol and isopropanol.
Further, adjusting the pH value of the solution to 9-13 with an alkali solution, wherein the alkali solution is a sodium hydroxide solution, a potassium hydroxide solution, a sodium bicarbonate solution, a sodium carbonate solution, a potassium bicarbonate solution or a potassium carbonate solution.
Furthermore, the revolution speed is 80-200r/min, and the rotation speed is 400-800 r/min.
Further, in the ball milling reaction process, the mass ratio of the ball materials is 50-200: 1.
Further, the ball milling reaction time is 12-48 h.
Further, during ultrasonic dispersion, the ultrasonic power is 180-220W, and the power density of the ultrasonic is 4-6W/cm2The frequency is 15-25kHz, and the ultrasonic dispersion time is 1-3 h.
The polymer-coated vanadium-titanium waste residue nano particle and the preparation method thereof provided by the invention have the following beneficial effects:
the method adopts the vanadium-titanium waste residue as the raw material to prepare the nano particles, changes the vanadium-titanium waste residue into valuable, and effectively reduces the cost of the raw material for preparing the nano particles and the preparation cost.
When vanadium-titanium waste residues are used as raw materials for preparing nano particles and then mixed with a polymer solution, in order to improve the surface hydrophilicity of the vanadium-titanium waste residues and improve the dispersion stability of the vanadium-titanium waste residues in the polymer, the pH value of the solution is adjusted by using an alkali solution to be 9-13, so that the purpose is to modify OH < - > on the surface of the vanadium-titanium waste residues, improve the hydrophilicity of the vanadium-titanium waste residues and further improve the dispersion stability of the vanadium-titanium waste residues.
The pH value of the solution is adjusted to 9-13, then ball milling reaction is carried out, so that when the vanadium-titanium waste residue forms nanoparticles, the polymer is coated on the surfaces of the nanoparticles in an in-situ mode, and a polymer modified nanoparticle compound is prepared. The ball milling time, the ball milling speed and the ball-to-material ratio are matched with each other, so that the ball milling product has a proper particle size, when the particle size is smaller, the product loss in the washing process is increased, the yield is reduced, and when the particle size is larger, the ball milling product cannot play a role of the nano particles.
And washing a product obtained after the ball milling reaction, drying in vacuum, then ultrasonically dispersing the product in water, performing ball milling and then dispersing to obtain the nano particles with reduced particle size, and re-dispersing the nano particles aggregated together in the drying process by using ultrasound to finally obtain the stably dispersed nano particles.
The method takes the vanadium-titanium waste residue as the raw material, has rich and large amount of raw materials, can meet the large demand of nano particles, provides a new method for the high added value utilization of the vanadium-titanium waste residue, reduces the damage of the vanadium-titanium waste residue to the ecological environment, consumes a large amount of vanadium-titanium waste residue, and reduces the risk and harm of the slag dam collapse.
The preparation method adopts a normal-temperature ball milling method in the preparation process, has mild reaction conditions, simple technical route and easy large-scale production, meets the requirements of large using amount and low cost of the nano particles, and can greatly expand the application field of the nano particles.
Detailed Description
Example 1
A preparation method of polymer-coated vanadium-titanium waste residue nanoparticles comprises the following steps:
mixing the vanadium-titanium waste residue with 5 wt% of polyacrylate solution (the hydrophilic polymer is polyacrylate)Sodium polyacrylate and water as a solvent) are uniformly mixed according to the mass ratio of 1:200, then a sodium hydroxide solution is added to adjust the pH value of the solution to be 14, then zirconia balls are added to be grinding balls (the ball material ratio is 50:1), the revolution speed of ball milling is set to be 120r/min, the rotation speed is set to be 800r/min, the ball milling is carried out in a horizontal planetary ball mill for 48 hours, the pH value of the product after ball milling is adjusted to be neutral by HCl solution, the product is put into a vacuum drying oven for drying, and then the dried product is dispersed in water for ultrasonic treatment for 3 hours, thus obtaining the vanadium-titanium nano particles coated by polyacrylate (specifically sodium polyacrylate); wherein the ultrasonic power is 200W, and the ultrasonic power density is 5W/cm2The frequency is 20 +/-5 kHz; wherein the ultrasonic power is 200W, and the ultrasonic power density is 5W/cm2The frequency is 20 +/-5 kHz.
Example 2
A preparation method of polymer-coated vanadium-titanium waste residue nanoparticles comprises the following steps:
uniformly mixing vanadium-titanium waste residues with 3 wt% of polyvinyl benzyl trimethylamine salt solution (the hydrophilic polymer is polyvinyl benzyl trimethylamine salt, water is used as a solvent) according to the mass ratio of 1:100, then adding sodium carbonate solution to adjust the pH value of the solution to be 12, then adding zirconia balls as grinding balls (the ball material ratio is 100:1), setting the ball milling revolution speed to be 120r/min and the rotation speed to be 600r/min, putting the ball milling balls into a horizontal planetary ball mill for ball milling for 48 hours, adjusting the pH value of the ball-milled product to be neutral by using HCl solution, putting the ball-milled product into a vacuum drying box for drying, and then dispersing the dried product into water for ultrasonic treatment for 2 hours to obtain the vanadium-titanium waste residue nano particles coated by the polyvinyl benzyl trimethylamine salt; wherein the ultrasonic power is 200W, and the ultrasonic power density is 5W/cm2The frequency is 20 +/-5 kHz.
Example 3
A preparation method of polymer-coated vanadium-titanium waste residue nanoparticles comprises the following steps:
uniformly mixing vanadium-titanium waste residues with 1 wt% of polyvinyl alcohol solution (the hydrophilic polymer is polyvinyl alcohol, and N, N-dimethylformamide and water are mixed as a solvent according to the mass ratio of 5: 1) according to the mass ratio of 3:200, and then adding potassium hydroxide solution to adjust the pH value of the solution14, adding zirconia balls as grinding balls (the ball-material ratio is 100:1), setting the revolution speed of ball milling to be 100r/min and the rotation speed to be 600r/min, putting the ball milling into a horizontal planetary ball mill for ball milling for 36 hours, adjusting the pH value of a product after ball milling to be neutral by using an HCl solution, putting the product into a vacuum drying oven for drying, and dispersing the dried product into water for ultrasonic treatment for 2 hours to obtain the polyvinyl alcohol-coated vanadium-titanium waste residue nanoparticles; wherein the ultrasonic power is 200W, and the ultrasonic power density is 5W/cm2The frequency is 20 +/-5 kHz.
Example 4
A preparation method of polymer-coated vanadium-titanium waste residue nanoparticles comprises the following steps:
uniformly mixing vanadium-titanium waste residues with 2 wt% of polyacrylamide solution (a hydrophilic polymer is polyacrylamide, and N-methyl pyrrolidone and water are mixed as a solvent in a mass ratio of 6: 1) according to a mass ratio of 1:100, then adding potassium carbonate solution to adjust the pH value of the solution to be 13, then adding zirconia balls as grinding balls (the ball-to-material ratio is 200:1), setting the ball-milling revolution speed to be 100r/min and the rotation speed to be 600r/min, putting the grinding balls into a horizontal planetary ball mill for ball milling for 36 hours, adjusting the pH value of the ball-milled product to be neutral by using HCl solution, putting the ball-milled product into a vacuum drying box for drying, and then dispersing the dried product into water for ultrasonic treatment for 1 hour to obtain the polyacrylamide-coated vanadium-titanium waste residues nano particles; wherein the ultrasonic power is 200W, and the ultrasonic power density is 5W/cm2The frequency is 20 +/-5 kHz.
Example 5
A preparation method of polymer-coated vanadium-titanium waste residue nanoparticles comprises the following steps:
uniformly mixing vanadium-titanium waste residues with 2 wt% of polyvinylpyrrolidone solution (the hydrophilic polymer is polyvinylpyrrolidone, water and ethanol are mixed as a solvent in a mass ratio of 5: 1) according to a mass ratio of 1:100, then adding sodium hydroxide solution to adjust the pH value of the solution to 10, then adding zirconia balls as grinding balls (the ball material ratio is 200:1), setting the revolution speed of ball milling to be 120r/min and the rotation speed to be 400r/min, putting the mixture into a horizontal planetary ball mill to perform ball milling for 48 hours, adjusting the pH value of a ball-milled product to be neutral by using HCl solution, and putting the ball-milled product into a vacuum drying chamber to dry the productDrying in a drying box, and dispersing the dried product in water for ultrasonic treatment for 2 hours to obtain the vanadium-titanium waste residue nano particles coated by the polyvinylpyrrolidone; wherein the ultrasonic power is 200W, and the ultrasonic power density is 5W/cm2The frequency is 20 +/-5 kHz.
Example 6
A preparation method of polymer-coated vanadium-titanium waste residue nanoparticles comprises the following steps:
mixing the vanadium-titanium waste residue with 2 wt% of 2-acrylamide-2-methylpropanesulfonic acid solution (the hydrophilic polymer is 2-acrylamide-2-methylpropanesulfonic acid, water and ethyl acetate are mixed as a solvent according to the mass ratio of 5: 1) according to the mass ratio of 3:200, then adding sodium hydroxide solution to adjust the pH value of the solution to 10, adding zirconia balls as grinding balls (the ball-material ratio is 200:1), setting the revolution speed of ball milling to 80r/min and the rotation speed to 400r/min, putting the ball milling balls into a horizontal planetary ball mill to perform ball milling for 48 hours, adjusting the pH value of the ball-milled product to be neutral by using HCl solution, putting the ball-milled product into a vacuum drying oven to dry, dispersing the dried product into water to perform ultrasonic treatment for 2 hours, obtaining 2-acrylamide-2-methylpropanesulfonic acid coated vanadium-titanium waste residue nanoparticles; wherein the ultrasonic power is 200W, and the ultrasonic power density is 5W/cm2The frequency is 20 +/-5 kHz.
Comparative example 1
Comparative example 1 is different from example 1 in that ball milling was directly performed in the absence of a step of adjusting the pH with a sodium hydroxide solution, and the remaining steps were the same as example 1.
Comparative example 2
Comparative example 2 is different from example 1 in that the pH of the ball-milled product is adjusted to be neutral by HCl solution, then ultrasonic dispersion is performed, and finally vacuum drying is performed, that is, the procedure of comparative example 2 is the same as example 1 except that the steps of ultrasonic dispersion and vacuum drying are exchanged.
Comparative example 3
The comparative example 3 is different from the example 1 in that ball milling parameters are different, ball milling revolution speed is set to be 250r/min, rotation speed is set to be 900r/min, the ball milling is carried out for 60h in a horizontal planetary ball mill, and the rest process is the same as the example 1.
Comparative example 4
Comparative example 4 differs from example 1 in that the pH adjusted solution was directly subjected to ultrasonic dispersion, absent a ball milling step.
The polymer-coated vanadium-titanium waste residue nanoparticles obtained in example 1 and comparative examples 1 to 4 were examined as follows:
1. particle size
The particle size of the polymer-coated vanadium-titanium waste residue nano particles obtained in example 1 reaches the nanometer level, the average particle size of the nano particles obtained in example 1 is 200nm, the average particle size of the polymer-coated vanadium-titanium waste residue nano particles obtained in comparative examples 1-4 is larger than that of example 1, but is much smaller than that of the vanadium-titanium waste residue before treatment, and the particle size sequence is that comparative example 4 is larger than that of comparative example 1, that of comparative example 2 is larger than that of example 1, and that of the vanadium-titanium waste residue before treatment is larger than that of comparative example 3. When the polymer and the vanadium-titanium waste residue are mixed, the pH value of the solution is adjusted to be alkaline by adopting an alkali solution, the surface of the vanadium-titanium waste residue can be modified with OH < - >, the hydrophilicity of the vanadium-titanium waste residue is improved, and then the vanadium-titanium waste residue is directly subjected to ultrasonic dispersion, although the final nano particles can reach the nano level, the dispersibility of the nano particles is not good, the dispersed particles in the obtained solution are not uniform, contain larger particles and are easy to agglomerate; when the method comprises a ball milling step, ball milling parameters are changed, namely, after the revolution speed, the rotation speed and the ball milling time of the ball milling are increased, the dispersibility of the particles can be improved in order to increase the parameters, but although the obtained particle size is reduced (smaller than that of the embodiment 1), the dispersibility of the particles in the solution is not as good as that of the embodiment 1, the particle size of the nanoparticles is not as small as possible, and when the particle size is very small, the particles are not beneficial to dispersion, and the stability of the particles cannot be ensured; when the surface activity of the vanadium-titanium waste residue is not adjusted by alkali, the particle size of the nano particles can be influenced, and the stability of the nano particles is further influenced; the particle size of the nanoparticles is also not beneficial after the ultrasonic dispersion and vacuum drying sequence is adjusted, because the morphology of the originally formed particles can be damaged by directly carrying out the violent ultrasonic dispersion process again after the ball milling is finished, the morphology of the formed nanoparticles is different from that of the formed nanoparticles in the embodiment 1 after the ultrasonic drying is finished, and the formed nanoparticles are easy to gather together after being dispersed.
2. Index of particle size distribution
The particle size distribution index (PDI) may reflect the degree of uniformity of particle size, with values between 0 and 1, with smaller values indicating better monodispersity of the particles, narrower particle size distributions, and conversely worse. The particle size distribution index detection is carried out on the polymer-coated vanadium-titanium waste residue nano particles obtained in the example 1 and the comparative examples 1 to 4, and the detection results are as follows:
| PDI | example 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| 0.268 | 0.372 | 0.338 | 0.321 | 0.512 |
3. Stability of
The polymer-coated vanadium-titanium waste slag nanoparticles obtained in example 1 and comparative examples 1 to 4 were dissolved in water at a density of 10mg/mL, and left at room temperature for 2 months, 3 months, 4 months, 5 months and 6 months, respectively, and the dissolution was recorded.
After the nanoparticles in example 1 are placed for 6 months, no layering and precipitation phenomena occur, which shows that the nanoparticles have good dispersibility and good stability; whereas comparative examples 1-4 are less stable than example 1, especially comparative example 4, precipitation occurred at 2 months; the stability sequences were example 1 > comparative example 3 > comparative example 2 > comparative example 1 > comparative example 4, consistent with the results described above.
Claims (10)
1. A preparation method of polymer-coated vanadium-titanium waste residue nanoparticles is characterized by comprising the following steps:
mixing vanadium-titanium waste residues with a hydrophilic polymer solution according to a mass ratio of 1-3:200, adjusting the pH value of the solution to 9-13, transferring the mixed solution into a ball mill for ball milling reaction, washing a ball milling product with an acid solution to be neutral, drying, and finally ultrasonically dispersing the dried product in water to obtain the vanadium-titanium composite material.
2. The method for preparing polymer-coated vanadium-titanium waste residue nanoparticles according to claim 1, wherein the concentration of the hydrophilic polymer solution is 1 to 5 wt%.
3. The method for preparing the polymer-coated vanadium-titanium waste residue nanoparticles according to claim 1 or 2, wherein the hydrophilic polymer is polyvinyl alcohol, polyethylene glycol, polyacrylate, polyacrylamide, polystyrene sulfonate, polyvinyl benzyl trimethylamine salt, polyvinylpyrrolidone, poly 2-acrylamide-2-methylpropanesulfonic acid or poly dimethylamino ethyl methacrylate quaternary ammonium salt.
4. The method for preparing the polymer-coated vanadium-titanium waste residue nanoparticles as claimed in claim 3, wherein the hydrophilic polymer solution is prepared by dissolving the hydrophilic polymer in a solvent and mixing the solution uniformly, wherein the solvent for dissolving the polymer is one or a mixture of two of water, N-dimethylformamide, N-methylpyrrolidone, ethyl acetate, tetrahydrofuran, ethanol and isopropanol.
5. The method for preparing the polymer-coated vanadium-titanium waste residue nanoparticles as claimed in claim 1, wherein the pH value of the solution is adjusted to 9-13 by using an alkali solution, and the alkali solution is a sodium hydroxide solution, a potassium hydroxide solution, a sodium bicarbonate solution, a sodium carbonate solution, a potassium bicarbonate solution or a potassium carbonate solution.
6. The preparation method of the polymer-coated vanadium-titanium waste residue nanoparticles as claimed in claim 1, wherein the mass ratio of the ball materials is 50-200:1 in the ball milling reaction process.
7. The method for preparing the polymer-coated vanadium-titanium waste residue nanoparticles as claimed in claim 1 or 6, wherein the revolution speed is 80-200r/min and the rotation speed is 400-800r/min during the ball milling reaction.
8. The method for preparing the polymer-coated vanadium-titanium waste residue nanoparticles as claimed in claim 7, wherein the ball milling reaction time is 12-48 h.
9. The method for preparing the polymer-coated vanadium-titanium waste residue nanoparticles as claimed in claim 1, wherein the ultrasonic power is 180-220W and the ultrasonic power density is 4-6W/cm during ultrasonic dispersion2The frequency is 15-25kHz, and the ultrasonic dispersion time is 1-3 h.
10. Polymer-coated vanadium-titanium waste nanoparticles obtainable by the process according to any one of claims 1 to 9.
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