CN113171761B - Porous electrostatic spraying microsphere for treating antimony-containing wastewater and preparation method thereof - Google Patents
Porous electrostatic spraying microsphere for treating antimony-containing wastewater and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of porous electrostatic spray microspheres for treating antimony-containing wastewater, which specifically comprises the following steps: (1) Dissolving polyacrylonitrile and polyvinylpyrrolidone powder in N, N-dimethylformamide solvent, and stirring at 50-60 deg.C for 2.0-12.0 h to obtain uniform electrostatic spray solution; (2) Placing the electrostatic spraying solution under electrostatic spraying equipment for electrostatic spraying, and collecting a vaporous microsphere precursor by adopting a roller wrapped by aluminum foil paper; (3) Putting the atomized microsphere precursor obtained in the step (2) into distilled water for washing and carrying out ultrasonic treatment; (4) Mixing the washed and ultrasonically treated atomized microsphere precursor with hydroxylamine hydrochloride, anhydrous sodium carbonate and distilled water, stirring, and carrying out in-situ amidoximation reaction to obtain electrostatic spraying microspheres; (5) And taking out the electrostatic spraying microspheres, soaking and washing the electrostatic spraying microspheres by using deionized water, drying the washed products in an oven, and then carrying out vacuum dehydration on the dried products to finally obtain the porous electrostatic spraying microspheres.
Description
Technical Field
The invention belongs to the technical field of preparation of fixed body adsorbents and materials, and particularly relates to a porous electrostatic spray microsphere for treating antimony-containing wastewater and a preparation method thereof.
Background
After the biochemical treatment, the printing and dyeing wastewater still contains a large amount of heavy metal substances, and the pollutants are represented by antimony. In recent years, the content of antimony in printing and dyeing wastewater is seriously exceeded, and the concentration of antimony before treatment can be as high as ten thousand mu g/L. The excessive antimony concentration is proved to have teratogenic and carcinogenic effects on human bodies, and seriously threatens the life and health of local people in the printing and dyeing industry. According to news reports, excessive antimony concentration in printing and dyeing wastewater causes production stoppage and stopping of many printing and dyeing enterprises, and huge economic loss is caused. Studies show that antimony in the printing and dyeing wastewater mainly exists in the form of pentavalent acid radicals (Sb (V)), and the chemical structure of the non-metal cations brings difficulty for antimony treatment. Therefore, the antimony for scientifically and effectively treating the printing and dyeing wastewater becomes a problem to be solved urgently.
At present, methods for removing antimony pollutants in printing and dyeing wastewater are various, and the methods which are researched and used most mainly comprise an adsorption method, a precipitation method and an electrochemical method. Among them, the adsorption method is widely used because of its advantages such as high efficiency, economy, and easy operation. The traditional antimony removal adsorbent mostly adopts inorganic adsorbents such as biomass, metal oxides, ores and the like, the maximum adsorption capacity of the traditional antimony removal adsorbent is generally 20mg/g, and the adsorption capacity is limited because the natural inorganic adsorbents lack a pore channel structure and have insufficient adsorption power; the other type of antimony removal adsorbent is carbon material adsorbents such as activated carbon, carbon nanotubes and graphene, the maximum adsorption capacity of the adsorbent to antimony is generally not more than 80mg/g, and the main reason for limiting the adsorption capacity is that the adsorbent lacks active functional groups as adsorption sites and cannot effectively capture antimony ions. Therefore, there is an important research value in developing an organic adsorbent having a high adsorption capacity.
The organic resin for water treatment has a large number of active functional groups (amino groups, carboxyl groups, sulfenyl groups, oximino groups and the like), is usually used for adsorbing heavy metal pollutants Pb, hg, cu and the like, has good adsorption capacity and has wide application prospect. Chinese patent with publication number CN108794661A discloses amidoximated polyacrylonitrile and a preparation method and application thereof, the amidoximated polyacrylonitrile material prepared by mixing polyacrylonitrile, hydroxylamine material and salt material is used as an adsorbent, the amidoximated polyacrylonitrile material has a porous structure, the pore size distribution is from nanometer to micrometer, and the amidoximated polyacrylonitrile material has chelating adsorption and physical adsorption capacities and can be used for treating heavy metal wastewater; chinese patent with publication number CN109364891A discloses a modified polyacrylonitrile for treating antimony-containing wastewater and a preparation method thereof, wherein the modified polyacrylonitrile particle adsorbent prepared by carrying out in-situ amidoximation on a polyacrylonitrile substrate is specifically disclosed and used for removing antimony in wastewater, the adsorption capacity of the modified polyacrylonitrile particle adsorbent is 90-160 mg/g, but the modified polyacrylonitrile particle adsorbent prepared by the method lacks a pore channel structure, and the maximum adsorption capacity for removing antimony is only 160mg/g. Therefore, increasing the pore structure inside the adsorbent and increasing the adsorption power is one of the ways to improve the adsorption capacity of the adsorbent to antimony.
Disclosure of Invention
In order to solve the problem that an antimony removal adsorbent in the prior art is short of a pore channel structure, the invention provides a porous electrostatic spraying microsphere for treating antimony-containing wastewater and a preparation method thereof.
The technical scheme of the invention is as follows:
the invention discloses a preparation method of porous electrostatic spraying microspheres for treating antimony-containing wastewater, which specifically comprises the following steps:
(1) Dissolving polyacrylonitrile and polyvinylpyrrolidone in N, N-dimethylformamide solvent, and stirring at 50-60 ℃ for 2.0-12.0 h to obtain uniform electrostatic spray solution;
(2) Placing the electrostatic spraying solution under electrostatic spraying equipment for electrostatic spraying, and collecting a vaporous microsphere precursor by adopting a roller wrapped by aluminum foil paper;
(3) Putting the atomized microsphere precursor obtained in the step (2) into distilled water for washing and carrying out ultrasonic treatment;
(4) Adding the washed and ultrasonically treated atomized microsphere precursor, hydroxylamine hydrochloride and anhydrous sodium carbonate into distilled water, mixing, stirring, and carrying out in-situ amidoximation reaction to obtain electrostatic spraying microspheres;
(5) And taking out the electrostatic spraying microspheres, soaking and washing the electrostatic spraying microspheres by using deionized water, drying the washed products in an oven, and then carrying out vacuum dehydration on the dried products to finally obtain the porous electrostatic spraying microspheres.
Further, in the step (1), the mass ratio of polyacrylonitrile to polyvinylpyrrolidone is 0.2-5.0, and the mass percentage of the polymer base material of polyacrylonitrile and polyvinylpyrrolidone in the solvent N, N-dimethylformamide is 0.1-2.5 wt%.
Further, in the step (2), the voltage of electrostatic spraying is 10.0-30.0V, the pushing speed is 0.1-5.0 mL/h, and the distance for collecting the atomized microsphere precursor by the roller is 0.1-0.8 m.
Further, the ultrasonic treatment time in the step (3) is 10.0-60.0 min.
Further, the mass ratio of the atomized microsphere precursor, hydroxylamine hydrochloride and anhydrous sodium carbonate added in the amidoximation reaction in the step (4) is 0.1-5.0; the volume ratio of the total mass of the mist microsphere precursor, the hydroxylamine hydrochloride and the anhydrous sodium carbonate to the distilled water is 11.9-16.8g.
Further, the heating temperature of the water bath for the amidoxime reaction is 60-80 ℃.
Further, the microsphere product washed in the step (5) is dried in a baking oven at 50-60 ℃ for 2-4 h, and then dried in a vacuum atmosphere at 60-70 ℃ for 12-48 h.
The invention also provides the porous electrostatic spraying microsphere prepared by the preparation method for the porous electrostatic spraying microsphere for treating the antimony-containing wastewater, wherein the maximum adsorption capacity of the porous electrostatic spraying microsphere is 300.0-400.0 mg/g.
The invention also provides application of the porous electrostatic spraying microspheres for treating the antimony-containing wastewater in the antimony-containing wastewater.
Compared with the prior art, the invention has the beneficial effects that:
(1) The porous electrostatic spraying microspheres are prepared by taking polyacrylonitrile and polyvinylpyrrolidone as raw materials, utilizing electrostatic spraying to generate a large number of fine pore channel structures on the formed microspheres in a high-voltage mode, and controlling the spraying process conditions to obtain the electrostatic spraying porous microspheres with proper pore channel structures; meanwhile, in combination with the in-situ amidoximation reaction, the in-situ amidoximation reaction not only has a pore-forming effect, but also enables the porous electrostatic spraying microsphere to have chelating adsorption and physical adsorption capacities at the same time, has good ion selectivity and adsorption power, and improves the adsorption performance.
(2) The polyacrylonitrile and the polyvinylpyrrolidone used in the invention have rich raw material sources, are traditional chemical raw materials, have simple preparation method and low energy consumption, and are suitable for industrial production.
(3) The porous electrostatic spray microsphere prepared by the invention has the advantages of high adsorption speed, large maximum adsorption capacity, good desorption effect and repeated recycling.
Drawings
FIG. 1 is a scanning electron micrograph of porous electrostatically sprayed microspheres made according to example 1 of the present invention;
FIG. 2 is a graph showing the adsorption kinetics of antimony ions in wastewater by porous electrostatically-sprayed microspheres prepared in example 1 according to the present invention, wherein qt is the adsorption capacity; t-adsorption time.
Detailed Description
In order to facilitate understanding of the present invention, the technical solutions of the present invention will be further described with reference to the following detailed description and the accompanying drawings, but the present invention is not limited thereto.
Example 1
A preparation method of porous electrostatic spraying microspheres for treating antimony-containing wastewater specifically comprises the following steps:
(1) Dissolving 1g of polyacrylonitrile and 1g of polyvinylpyrrolidone (1:1) in 100mL of N, N-dimethylformamide solvent, wherein the mass percent of polyacrylonitrile and polyvinylpyrrolidone polymer base material in the solvent N, N-dimethylformamide is 2wt%, and stirring at 50 ℃ for 2.0h to obtain uniform electrostatic spraying solution;
(2) Placing the electrostatic spraying solution under electrostatic spraying equipment for electrostatic spraying, and collecting a vaporous microsphere precursor by adopting a roller wrapped by aluminum foil paper; wherein the voltage of electrostatic spraying is 20V, the injection speed is 0.1mL/h, and the distance for collecting the precursor of the atomized microspheres by the roller is 0.1m;
(3) Washing the atomized microsphere precursor obtained in the step (2) in distilled water, and carrying out ultrasonic treatment for 10.0min;
(4) Adding 0.1g of washed and ultrasonically treated atomized microsphere precursor, 6.0g of hydroxylamine hydrochloride and 5.8g of anhydrous sodium carbonate into 100mL of distilled water, mixing, stirring, and carrying out in-situ amidoximation reaction at 60 ℃ to obtain electrostatic spraying microspheres;
(5) And taking out the electrostatic spraying microspheres, soaking and washing the electrostatic spraying microspheres by using deionized water, drying the washed product in a 50 ℃ drying oven for 2.0h, and dehydrating the dried product in a vacuum atmosphere at 70 ℃ for 12.0h to finally obtain the porous electrostatic spraying microspheres.
Example 2
A preparation method of porous electrostatic spraying microspheres for treating antimony-containing wastewater specifically comprises the following steps:
(1) Dissolving 1g of polyacrylonitrile and 0.5g of polyvinylpyrrolidone (2:1) in 100mL of N, N-dimethylformamide solvent, wherein the mass percentage of the polyacrylonitrile and polyvinylpyrrolidone polymer base material in the N, N-dimethylformamide solvent is 1.5wt%, and stirring at 60 ℃ for 12.0h to obtain a uniform electrostatic spraying solution;
(2) Placing the electrostatic spraying solution under electrostatic spraying equipment for electrostatic spraying, and collecting a vaporous microsphere precursor by adopting a roller wrapped by aluminum foil paper; wherein the voltage of electrostatic spraying is 10.0V, the injection speed is 1.0mL/h, and the distance for collecting the precursor of the atomized microspheres by the roller is 0.4m;
(3) Washing the mist microsphere precursor obtained in the step (2) in distilled water, and carrying out ultrasonic treatment for 20.0min;
(4) Adding 5.0g of washed and ultrasonically treated atomized microsphere precursor, 6.0g of hydroxylamine hydrochloride and anhydrous sodium carbonate into distilled water, mixing, stirring, and carrying out in-situ amidoximation reaction at 70 ℃ to obtain electrostatic spraying microspheres;
(5) And taking out the electrostatic spraying microspheres, soaking and washing the electrostatic spraying microspheres by using deionized water, drying the washed product in a 60 ℃ drying oven for 4.0h, and dehydrating the dried product in a 60 ℃ vacuum atmosphere for 48.0h to finally obtain the porous electrostatic spraying microspheres.
Example 3
A preparation method of porous electrostatic spraying microspheres for treating antimony-containing wastewater specifically comprises the following steps:
(1) Dissolving 1g of polyacrylonitrile and 0.2g of polyvinylpyrrolidone (5:1) in 40mL of N, N-dimethylformamide solvent, wherein the mass percent of polyacrylonitrile and polyvinylpyrrolidone polymer base material in the solvent N, N-dimethylformamide is 2.5wt%, and stirring at 55 ℃ for 10.0h to obtain uniform electrostatic spraying solution;
(2) Placing the electrostatic spraying solution under electrostatic spraying equipment for electrostatic spraying, and collecting a vaporous microsphere precursor by adopting a roller wrapped by aluminum foil paper; wherein the voltage of electrostatic spraying is 30.0V, the injection speed is 5.0mL/h, and the distance for collecting the precursor of the atomized microspheres by the roller is 0.8m;
(3) Washing the mist microsphere precursor obtained in the step (2) in distilled water, and carrying out ultrasonic treatment for 60.0min;
(4) Adding 2.0g of the washed and ultrasonically treated atomized microsphere precursor, 6.0g of hydroxylamine hydrochloride and 5.8g of anhydrous sodium carbonate into 100mL of distilled water, mixing, stirring, and carrying out in-situ amidoximation reaction at 80 ℃ to obtain electrostatic spraying microspheres;
(5) And taking out the electrostatic spraying microspheres, soaking and washing the electrostatic spraying microspheres by using deionized water, drying the washed product in an oven at 55 ℃ for 3.0h, and removing the dried product in a vacuum atmosphere at 65 ℃ for 24.0h to finally obtain the porous electrostatic spraying microspheres.
Example 4
A preparation method of porous electrostatic spraying microspheres for treating antimony-containing wastewater specifically comprises the following steps:
(1) Dissolving 0.1g of polyacrylonitrile and 0.5g of polyvinylpyrrolidone (0.2;
(2) Placing the electrostatic spraying solution under electrostatic spraying equipment for electrostatic spraying, and collecting a vaporous microsphere precursor by adopting a roller wrapped by aluminum foil paper; wherein the voltage of electrostatic spraying is 20V, the injection speed is 2.0mL/h, and the distance for collecting the precursor of the atomized microspheres by the roller is 0.2m;
(3) Washing the atomized microsphere precursor obtained in the step (2) in distilled water, and carrying out ultrasonic treatment for 10.0min;
(4) Adding 0.5g of washed and ultrasonically treated atomized microsphere precursor, 6.0g of hydroxylamine hydrochloride and 5.8g of anhydrous sodium carbonate into 100mL of distilled water, mixing, stirring, and carrying out in-situ amidoximation reaction at 60 ℃ to obtain electrostatic spraying microspheres;
(5) And taking out the electrostatic spraying microspheres, soaking and washing the electrostatic spraying microspheres by using deionized water, drying the washed product in a 50 ℃ drying oven for 2.0h, and dehydrating the dried product in a vacuum atmosphere at 70 ℃ for 20.0h to finally obtain the porous electrostatic spraying microspheres.
And (3) performance testing:
1. adsorption Capacity test
In an adsorption experiment, 400mL of antimony-containing wastewater with the concentration of 50mg/L is prepared, then 0.1g of porous electrostatic spray microsphere adsorbent is added, the mixture is put into a shaking table and is shaken at a constant speed at 25 ℃, samples are taken when 0.2,0.5,1.0,1.5,2.0,3.0,6.0 and 12.0 hours respectively, the adsorption capacity is calculated after the concentration of antimony ions is measured, and the specific adsorption capacity is shown in Table 1:
TABLE 1 porous electrostatically sprayed microsphere adsorption capacities
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Adsorption capacity (mg/g) | 380 | 323 | 378 | 355 |
As can be seen from the table above, the maximum adsorption capacity of the porous electrostatic spraying microsphere prepared by the invention is 300.0-400.0 mg/g.
2. Referring to fig. 1, an SEM image of the porous electrostatically-sprayed microspheres prepared according to example 1 of the present invention shows that the porous electrostatically-sprayed microspheres prepared according to the present invention have a particle size of 0.2 to 0.75 μm.
3. Referring to fig. 2, an adsorption kinetics diagram of the porous electrostatic spraying microspheres prepared according to example 1 of the present invention for adsorbing antimony ions in wastewater shows that an adsorption mechanism of the porous electrostatic spraying microspheres for antimony in wastewater conforms to a quasi-second-order adsorption kinetics model, and the adsorption of the porous electrostatic spraying microspheres for antimony in wastewater belongs to chemical adsorption, which relates to electron sharing or electron transfer between an adsorbent and an adsorbate.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. The application of the porous electrostatic spraying microspheres for treating the antimony-containing wastewater in the antimony-containing wastewater is characterized in that the preparation method of the porous electrostatic spraying microspheres specifically comprises the following steps: (1) Dissolving polyacrylonitrile and polyvinylpyrrolidone in an N, N-dimethylformamide solvent, and stirring at 50-60 ℃ for 2.0-12.0 h to form a uniform electrostatic spray solution;
(2) Placing the electrostatic spraying solution under electrostatic spraying equipment for electrostatic spraying, and collecting a vaporous microsphere precursor by adopting a roller wrapped by aluminum foil paper;
(3) Putting the atomized microsphere precursor obtained in the step (2) into distilled water for washing and carrying out ultrasonic treatment;
(4) Adding the washed and ultrasonically treated atomized microsphere precursor, hydroxylamine hydrochloride and anhydrous sodium carbonate into distilled water, mixing, stirring, and carrying out in-situ amidoximation reaction to obtain electrostatic spraying microspheres;
(5) And taking out the electrostatic spraying microspheres, soaking and washing the electrostatic spraying microspheres by using deionized water, drying the washed products in an oven, and then carrying out vacuum dehydration on the dried products to finally obtain the porous electrostatic spraying microspheres.
2. The use of the porous electrostatically-sprayed microspheres for treating antimony-containing wastewater as claimed in claim 1 in antimony-containing wastewater, wherein: in the step (1), the mass ratio of polyacrylonitrile to polyvinylpyrrolidone is 0.2-5.0, and the mass percentage of the polymer base material of polyacrylonitrile and polyvinylpyrrolidone in the solvent N, N-dimethylformamide is 0.1-2.5 wt%.
3. The use of the porous electrostatically-sprayed microspheres for treating antimony-containing wastewater as claimed in claim 1 in antimony-containing wastewater, wherein: in the step (2), the voltage of electrostatic spraying is 10.0-30.0V, the pushing speed is 0.1-5.0 mL/h, and the distance for collecting the precursor of the atomized microspheres in a roller is 0.1-0.8m.
4. The use of the porous electrostatically-sprayed microspheres for treating antimony-containing wastewater as claimed in claim 1 in antimony-containing wastewater, wherein: and (4) in the step (3), the ultrasonic processing time is 10.0-60.0 min.
5. The use of the porous electrostatically-sprayed microspheres for treating antimony-containing wastewater as claimed in claim 1 in antimony-containing wastewater, wherein: the mass ratio of the atomized microsphere precursor, hydroxylamine hydrochloride and anhydrous sodium carbonate added in the amidoximation reaction in the step (4) is 0.1 to 5.0; the volume ratio of the total mass of the atomized microsphere precursor, the hydroxylamine hydrochloride and the anhydrous sodium carbonate to the distilled water is 11.9-16.8g.
6. The use of the porous electrostatically-sprayed microspheres for the treatment of antimony-containing wastewater as claimed in claim 1 in antimony-containing wastewater, wherein: the water bath heating temperature of the amidoxime reaction is 60 to 80 ℃.
7. The use of the porous electrostatically-sprayed microspheres for the treatment of antimony-containing wastewater as claimed in claim 1 in antimony-containing wastewater, wherein: and (3) drying the microsphere product washed in the step (5) in an oven at 50-60 ℃ for 2-4 h, and then drying in a vacuum atmosphere at 60-70 ℃ for 12-48h.
8. The use of the porous electrostatically-sprayed microspheres for treating antimony-containing wastewater as claimed in claim 1 in antimony-containing wastewater, wherein: the maximum adsorption capacity of the porous electrostatic spraying microspheres is 300.0-400.0 mg/g.
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