CN115193421B - Preparation method of sewage treatment adsorbent - Google Patents
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- CN115193421B CN115193421B CN202211125259.XA CN202211125259A CN115193421B CN 115193421 B CN115193421 B CN 115193421B CN 202211125259 A CN202211125259 A CN 202211125259A CN 115193421 B CN115193421 B CN 115193421B
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Abstract
The invention relates to the technical field of water treatment and discloses a preparation method of a sewage treatment adsorbent, wherein mesoporous nano-silica is reacted with 3-aminopropyltriethoxysilane and 4-vinylbenzaldehyde to obtain styryl modified mesoporous silica; carrying out esterification condensation reaction on cysteine-based amide butyric acid monomer and triethanolamine to prepare novel sulfydryl hyperbranched polyester, and carrying out light click reaction on partial sulfydryl and a styrene functional group modified on the surface of mesoporous nano silicon dioxide so as to graft the sulfydryl hyperbranched polyester onto the surface of the silicon dioxide to obtain a sewage treatment adsorbent; the grafted sulfydryl hyperbranched polyester contains functional groups such as sulfydryl, amide groups, carboxyl and the like, has strong coordination chelation and adsorption performance on metal ions such as lead, copper, cadmium and the like, and has wide application prospects in wastewater treatment and marine pollution purification.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a preparation method of a sewage treatment adsorbent.
Background
The pollution of water environment such as oceans is a major problem faced by the present society, and as industrial wastewater, mining wastewater and the like are randomly discharged into natural water body environment such as oceans and the like, the ecological environment of the oceans is seriously damaged, so that the wastewater treatment and the purification of ocean water pollution are in the forefront, and in recent years, various countries in the world are vigorously researched and developed to prepare novel adsorbing materials such as inorganic nano adsorbing materials and polymeric flocculants; the nanometer silica has large specific surface area, is nontoxic and pollution-free, and has wide application prospect in the fields of wastewater treatment, marine water pollution purification and the like, for example, patent CN106861631B entitled functionalized hollow mesoporous silica nanometer microsphere, preparation method thereof and application in heavy metal ion adsorption discloses that hollow mesoporous silica nanometer microspheres are used as raw materials, aminated by silane coupling agent and combined with sodium chloroacetate, so that the nanometer silica is grafted with bidentate functional groups with metal ion adsorption performance, and has great application potential in the field of treating water body heavy metal ion pollution.
The surface modification of the nano-silica can improve the dispersibility and the agglomeration property of the nano-silica, and expand the practical application of the nano-silica in water treatment, for example, a paper, namely hyperbranched modification of mesoporous materials and the adsorption performance research on azo dyes, reports that hyperbranched polyaluminium chloride is grafted on the surface of the mesoporous silica, and has good adsorption performance on dye pollutants; the hyperbranched polymer is used as a three-dimensional macromolecule with multiple branch points and molecular chains which are not easy to tangle, is easy to modify, has rich functional groups, and has wide application prospect in wastewater treatment and ocean water pollution purification; the invention synthesizes novel hyperbranched polyester, and grafts the novel hyperbranched polyester on the surface of mesoporous nano-silica to obtain the sewage treatment adsorbent, which is applied to wastewater treatment and marine pollution purification.
Disclosure of Invention
Technical problem to be solved
The invention provides a preparation method of a sewage treatment adsorbent, which solves the problems of low adsorption performance and low adsorption capacity of a nano-silica adsorption material on metal ions.
(II) technical scheme
In order to realize the purpose, the invention provides the following technical scheme: a preparation method of a sewage treatment adsorbent comprises the following steps:
s1, dispersing amino modified mesoporous silica into an ethanol solvent, adding 4-vinylbenzaldehyde, stirring and refluxing the amino modified mesoporous silica and the 4-vinylbenzaldehyde at the weight ratio of 100-400 for 12-36 h at 70-90 ℃, and filtering and washing after reaction to obtain styryl modified mesoporous silica;
s2, dispersing the styrene-based modified mesoporous silica into N, N-dimethylformamide, adding sulfydryl hyperbranched polyester, wherein the weight ratio of the styrene-based modified mesoporous silica to the sulfydryl hyperbranched polyester is 100-400, adding benzoin dimethyl ether, stirring under an ultraviolet lamp for reaction for 1-2 h, and the illumination intensity of the ultraviolet lamp is 5-20W & lt/EN & gtcm 2 And filtering and washing after reaction to obtain the sewage treatment adsorbent.
Preferably, the preparation method of the amino-modified mesoporous silica in S1 comprises the following steps:
s3, dispersing the nano-silicon powder into 25% ammonia water solution, heating to 80 ℃, stirring, refluxing and reacting for 18 hours, supplementing the ammonia water solution in the reaction process, controlling the pH of the reaction solution to be 11, filtering and washing after the reaction to obtain nano-silicon dioxide; then dispersing the nano-silica into distilled water, adding polyvinylpyrrolidone, heating to 100 ℃, stirring and refluxing for 3 h, cooling, adding 8% aqueous solution of sodium hydroxide, stirring and etching for 2 h, filtering, washing, placing the product in a resistance furnace, and calcining for 3 h at 500 ℃ to obtain mesoporous nano-silica;
s4, dispersing mesoporous nano-silica into a mixed solvent of distilled water and ethanol with the volume ratio of 1.
Preferably, the dosage of benzoin dimethyl ether in S2 is 0.75-2% of the mass of the sulfhydryl hyperbranched polyester.
Preferably, the preparation method of the thiol hyperbranched polyester in S2 comprises the following steps:
s5, adding DL-cysteine into a sodium carbonate aqueous solution, stirring for dissolving, adding succinic anhydride, wherein the weight ratio of DL-cysteine to succinic anhydride is 100-120, stirring for reacting at 15-20 ℃ for 6-8 h, dropwise adding dilute hydrochloric acid after reaction to adjust the pH of the solution to 5-6, uniformly stirring, extracting, drying, filtering, concentrating the filtrate under reduced pressure, and washing to obtain cysteinyl amidobutyric acid;
s6, dissolving cysteinyl amide butyric acid and triethanolamine into a solvent, dropwise adding p-toluenesulfonic acid, wherein the weight ratio of cysteinyl amide butyric acid to triethanolamine to p-toluenesulfonic acid is (100-32-45).
Preferably, the concentration of the aqueous solution of sodium carbonate in S5 is 8-12%.
Preferably, the solvent in S6 comprises N, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide and N-methylpyrrolidone.
Preferably, the reaction in S6 is carried out at 130-150 ℃ for 3-8 h.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the surface of nano-silica generated by nano-silica micropowder in an alkaline ammonia water system contains abundant silicon hydroxyl, and then mesoporous nano-silica is obtained by sodium hydroxide etching, and has high specific surface area and rich pore channel structure; a large amount of silicon hydroxyl on the surface is utilized to react with 3-aminopropyl triethoxysilane, then surface modified amino is subjected to Schiff base reaction with 4-vinylbenzaldehyde, and the styryl modified mesoporous silica is obtained, so that abundant styryl functional groups are modified on the surface of the mesoporous nano silica.
The novel sulfydryl hyperbranched polyester is prepared by performing an anhydride ring-opening reaction on DL-cysteine and succinic anhydride to prepare a cysteinyl amide butyric acid monomer, and performing an esterification condensation reaction on the cysteinyl amide butyric acid monomer and triethanolamine.
Part of sulfydryl in the sulfydryl hyperbranched polyester and a styrene functional group modified on the surface of the mesoporous nano silicon dioxide are subjected to light click reaction, so that the sulfydryl hyperbranched polyester is grafted to the surface of the silicon dioxide to obtain a sewage treatment adsorbent; the hydrophilic hyperbranched polyester improves the dispersibility of the mesoporous nano-silica in a water medium, and is beneficial to reducing the agglomeration of the nano-silica, thereby improving the adsorption performance of the mesoporous nano-silica; meanwhile, the mercapto hyperbranched polyester grafted on the surface of the mesoporous nano-silica contains functional groups such as mercapto, amide groups, carboxyl and the like, and has strong coordination chelation and adsorption performance on metal ions such as lead, copper, cadmium and the like, so that the adsorbent shows excellent adsorption efficiency and adsorption capacity on the metal ions such as lead and the like, and has wide application prospects in wastewater treatment and marine pollution purification.
Drawings
FIG. 1 shows a styryl-modified mesoporous silica SiO 2 -1 infrared spectrum.
FIG. 2 is an infrared spectrum of the mercapto hyperbranched polyester HBPE-1.
FIG. 3 shows a sewage treatment adsorbent SiO 2 -infrared spectrum of HBPE-1.
FIG. 4 is SiO 2 -1 and SiO 2 Scanning electron micrograph of HBPE-1.
FIG. 5 is Pb 2+ Equilibrium capacity adsorption curve.
Detailed Description
Nano silicon powder: model CW-Si-001, average particle size 30 nm, purity >99.9%, shanghai Chaowei nanotechnology Limited.
Polyvinylpyrrolidone: PVPK15, average molecular weight 5500, bubi ke new materials science shanghai ltd.
The present invention provides the following examples:
example 1
(1) Dispersing 5 g of nano silicon powder into 200 mL of 25% ammonia water solution, heating to 80 ℃, stirring, refluxing and reacting for 18 h, supplementing the ammonia water solution in the reaction process, controlling the pH of the reaction solution to be 11, filtering the solvent after the reaction, and washing the product with distilled water to obtain nano silicon dioxide; then dispersing 2 g of nano-silica into 200 mL of distilled water, adding 28 g of polyvinylpyrrolidone, heating to 100 ℃, stirring and refluxing for 3 h, cooling, adding 50mL of 8% sodium hydroxide aqueous solution, stirring and etching for 2 h, filtering the solvent, washing with distilled water, placing the product in a resistance furnace, and calcining for 3 h at 500 ℃ to obtain the mesoporous nano-silica.
(2) Dispersing 2 g of mesoporous nano-silica into a mixed solvent of 50mL of distilled water and 250mL of ethanol, adding 5 mL of 28% ammonia water solution, dropwise adding 2.2 g of 3-aminopropyltriethoxysilane, stirring and reacting at 65 ℃ for 20 h under a nitrogen atmosphere, filtering the solvent after reaction, and washing the product with distilled water and ethanol in sequence to obtain the amino modified mesoporous silica.
(3) Dispersing 1 g of amino modified mesoporous silica into 80 mL of ethanol solvent, adding 1.5 g of 4-vinylbenzaldehyde, stirring and refluxing at 70 ℃ for 36 h, filtering the solvent after reaction, and washing the product with ethanol to obtain the styryl modified mesoporous silica SiO 2 -1。
(4) Adding 0.5 g of DL-cysteine into 10 mL of 12% sodium carbonate aqueous solution, stirring for dissolving, adding 0.52 g of succinic anhydride, stirring for reacting for 6 hours at 15 ℃, dropwise adding dilute hydrochloric acid after the reaction to adjust the pH value of the solution to 6, adding saturated sodium chloride solution and ethyl acetate for extraction after uniformly stirring, adding anhydrous sodium sulfate into an organic layer for drying, filtering, concentrating the filtrate under reduced pressure, washing the product with petroleum ether to obtain cysteinyl amide butyric acid,
；1H NMR (CDCl 3 , 300 MHz) δ:10.65(s, 1H)，10.20(s, 1H)，8.30 (s, 1H)，4.80-4.65 (m, 1H)，3.30-3.06 (m, 2H)，2.86-2.73 (m, 2H)，2.39-2.22 (m, 2H)，1.38(s, 1H)。
(5) Dissolving 1 g of cysteinyl amide butyric acid and 0.32 g of triethanolamine into 50mL of N, N-dimethylformamide solvent, dropwise adding 0.06 g of p-toluenesulfonic acid, stirring and reacting at 130 ℃ for 8 h, cooling, adding methanol for precipitation, filtering the solvent, and washing with distilled water and ethanol in sequence to obtain the sulfydryl hyperbranched polyester HBPE-1.
(6) Dispersing 0.5 g of styrene-based modified mesoporous silica into 50mL of N, N-dimethylformamide, then adding 2 g of sulfydryl hyperbranched polyester and 0.015 g of benzoin dimethyl ether, stirring and reacting for 2 hours under an ultraviolet lamp with the illumination intensity of 5 W/cm 2 Filtering the solvent after the reaction, and washing the product by using N, N-dimethylformamide, distilled water and ethanol in sequence to obtain the sewage treatment adsorbent SiO 2 -HBPE-1。
Example 2
(1) 1 g of the amino modified mesoporous silica prepared in example 1 was dispersed in 80 mL of ethanol solvent, 5 g of 4-vinylbenzaldehyde was added, the mixture was stirred and refluxed at 90 ℃ for 12 hours, and after the reaction, the solvent was filtered, and the product was washed with ethanol to obtain styrene-based modified mesoporous silica.
(2) Adding 0.5 g of DL-cysteine into 15 mL of 10% sodium carbonate aqueous solution, stirring for dissolving, adding 0.6 g of succinic anhydride, stirring for reacting for 8 hours at 20 ℃, dropwise adding dilute hydrochloric acid after the reaction to adjust the pH of the solution to 6, adding a saturated sodium chloride solution and ethyl acetate for extraction after uniformly stirring, adding anhydrous sodium sulfate into an organic layer for drying, filtering, concentrating the filtrate under reduced pressure, and washing the product with petroleum ether to obtain cysteinyl amidobutyric acid.
(3) Dissolving 1 g of cysteinyl amide butyric acid and 0.4 g of triethanolamine into 100 mL of N-methylpyrrolidone solvent, dropwise adding 0.1 g of p-toluenesulfonic acid, stirring and reacting at 150 ℃ for 6 hours, cooling, adding methanol for precipitation, filtering the solvent, and washing with distilled water and ethanol in sequence to obtain the sulfhydryl hyperbranched polyester.
(4) Dispersing 0.5 g of styryl modified mesoporous silica into 100 mL of N, N-dimethylformamide, adding 7.5 g of sulfydryl hyperbranched polyester and 0.15 g of benzoin dimethyl ether, stirring and reacting for 1 h under an ultraviolet lamp with the illumination intensity of 20W/cm 2 Filtering the solvent after the reaction, and washing the product by sequentially using N, N-dimethylformamide, distilled water and ethanol to obtain the sewage treatment adsorbent SiO 2 -HBPE-2。
Example 3
(1) 1 g of the amino-modified mesoporous silica prepared in example 1 was dispersed in 100 mL of an ethanol solvent, 3.2 g of 4-vinylbenzaldehyde was added, the mixture was stirred and refluxed at 80 ℃ for 24 hours, and the solvent was filtered after the reaction, and the product was washed with ethanol to obtain styrene-based modified mesoporous silica.
(2) Adding 0.5 g of DL-cysteine into 10 mL of 8% sodium carbonate aqueous solution, stirring for dissolving, adding 0.45 g of succinic anhydride, stirring for reacting for 8 h at 15 ℃, dropwise adding dilute hydrochloric acid after the reaction to adjust the pH of the solution to 5, adding a saturated sodium chloride solution and ethyl acetate for extraction after uniformly stirring, adding anhydrous sodium sulfate into an organic layer for drying, filtering, concentrating the filtrate under reduced pressure, and washing the product with petroleum ether to obtain cysteinyl amidobutyric acid.
(3) Dissolving 1 g of cysteinyl amide butyric acid and 0.45 g of triethanolamine into 100 mL of N, N-dimethylacetamide solvent, dropwise adding 0.12 g of p-toluenesulfonic acid, stirring and reacting at 130 ℃ for 3 h, cooling, adding methanol for precipitation, filtering the solvent, and washing with distilled water and ethanol in sequence to obtain the sulfhydryl hyperbranched polyester.
(4) Dispersing 0.5 g of styryl modified mesoporous silica into 100 mL of N, N-dimethylformamide, then adding 5.8 g of sulfydryl hyperbranched polyester and 0.1 g of benzoin dimethyl ether, stirring and reacting for 2 hours under an ultraviolet lamp with the illumination intensity of 10W/cm 2 Filtering the solvent after the reaction, and washing the product by using N, N-dimethylformamide, distilled water and ethanol in sequence to obtain the sewage treatment adsorbent SiO 2 -HBPE-3。
Comparative example 1
(1) Dispersing 5 g of nano silicon powder into 200 mL of 25% ammonia water solution, heating to 80 ℃, stirring, refluxing and reacting for 12 h, supplementing the ammonia water solution in the reaction process, controlling the pH of the reaction solution to be 11, filtering the solvent after the reaction, and washing the product with distilled water to obtain nano silicon dioxide; then dispersing 2 g of nano-silica into 400 mL of distilled water, adding 38 g of polyvinylpyrrolidone, heating to 100 ℃, stirring and refluxing for 3 h, cooling, adding 40 mL of 10% sodium hydroxide aqueous solution, stirring and etching for 2 h, filtering the solvent, washing with distilled water, placing the product in a resistance furnace, calcining for 2 h at 500 ℃ to obtain mesoporous nano-silica SiO 2 -4。
Comparative example 2
(1) Adding 0.5 g of DL-cysteine into 15 mL of 8% sodium carbonate aqueous solution, stirring for dissolving, adding 0.48 g of succinic anhydride, stirring for reacting for 4 hours at 30 ℃, dropwise adding dilute hydrochloric acid after the reaction to adjust the pH of the solution to 5, adding a saturated sodium chloride solution and ethyl acetate for extraction after uniformly stirring, adding anhydrous sodium sulfate into an organic layer for drying, filtering, concentrating the filtrate under reduced pressure, and washing the product with petroleum ether to obtain cysteinyl amidobutyric acid.
(2) Dissolving 1 g of cysteinyl amide butyric acid and 0.38 g of triethanolamine into 100 mL of N, N-dimethylformamide solvent, dropwise adding 0.08 g of p-toluenesulfonic acid, stirring and reacting at 120 ℃ for 8 h, cooling, adding methanol for precipitation, filtering the solvent, and washing with distilled water and ethanol in sequence to obtain the sulfydryl hyperbranched polyester HBPE-5.
Dissolving lead nitrate in distilled water to obtain 100 mg/L Pb 2+ The solution was then added to 250mL of Pb using 50 mg of the sewage treatment adsorbent prepared in examples 1 to 3, 50 mg of the mesoporous nano-silica prepared in comparative example 1, and 50 mg of the mercapto hyperbranched polyester prepared in comparative example 2 as adsorbents, respectively 2+ In the solution, controlling the pH value of the solution to be 6, statically adsorbing until the solution is balanced, transferring the adsorption solution in the adsorption process, and measuring Pb by utilizing an atomic absorption spectrophotometry 2+ Absorbance and concentration.
Claims (6)
1. A preparation method of a sewage treatment adsorbent is characterized by comprising the following steps: the preparation method of the sewage treatment adsorbent comprises the following steps:
s1, dispersing amino modified mesoporous silica into an ethanol solvent, and adding 4-vinylbenzaldehyde, wherein the weight ratio of the amino modified mesoporous silica to the 4-vinylbenzaldehyde is 100:150-500, stirring and refluxing at 70-90 ℃ for reaction for 12-36 h, filtering and washing after the reaction to obtain the styryl modified mesoporous silica;
s2, dispersing the styryl modified mesoporous silica into N, N-dimethylformamide, and then adding the sulfydryl hyperbranched polyester, wherein the weight ratio of the styryl modified mesoporous silica to the sulfydryl hyperbranched polyester is 100:400-1500, adding benzoin dimethyl ether, stirring and reacting for 1-2 h under an ultraviolet lamp with the illumination intensity of 5-20W/cm 2 Filtering and washing after reaction to obtain a sewage treatment adsorbent;
the preparation method of the sulfhydryl hyperbranched polyester in S2 comprises the following steps:
s5, adding DL-cysteine into a sodium carbonate aqueous solution, stirring to dissolve, and adding succinic anhydride, wherein the weight ratio of DL-cysteine to succinic anhydride is 100:90-120, stirring and reacting at 15-20 ℃ for 6-8 h, dropwise adding dilute hydrochloric acid after reaction to adjust the pH of the solution to 5-6, uniformly stirring, extracting, drying, filtering, concentrating the filtrate under reduced pressure, and washing to obtain cysteinyl amide butyric acid;
s6, dissolving cysteinyl amide butyric acid and triethanolamine into a solvent, and dropwise adding p-toluenesulfonic acid, wherein the weight ratio of cysteinyl amide butyric acid to triethanolamine to p-toluenesulfonic acid is 100:32-45:6-12, stirring, reacting, cooling, precipitating, filtering and washing to obtain the sulfhydryl hyperbranched polyester.
2. The method for preparing a sewage treatment adsorbent according to claim 1, wherein: the preparation method of the mesoporous silica modified by amino in S1 comprises the following steps:
s3, dispersing the nano-silicon powder into 25% ammonia water solution, heating to 80 ℃, stirring, refluxing and reacting for 18 hours, supplementing the ammonia water solution in the reaction process, controlling the pH of the reaction solution to be 11, filtering and washing after the reaction to obtain nano-silicon dioxide; then dispersing the nano silicon dioxide into distilled water, and adding polyvinylpyrrolidone, wherein the weight ratio of the nano silicon dioxide to the polyvinylpyrrolidone is 100:140, heating to 100 ℃, stirring and refluxing for 3 h, cooling, adding 8% aqueous solution of sodium hydroxide, stirring and etching for 2 h, filtering, washing, placing the product in a resistance furnace, and calcining for 3 h at 500 ℃ to obtain mesoporous nano-silica;
s4, dispersing the mesoporous nano silicon dioxide into a solution with the volume ratio of 1:5, adding 28% ammonia water solution into the mixed solvent of distilled water and ethanol, and dropwise adding 3-aminopropyltriethoxysilane, wherein the weight ratio of the mesoporous nano-silica to the 3-aminopropyltriethoxysilane is 100:110, stirring and reacting for 20 hours at 65 ℃ in the nitrogen atmosphere, filtering the solvent after the reaction, and washing the product by using distilled water and ethanol in sequence to obtain the amino modified mesoporous silica.
3. The method for preparing a sewage treatment adsorbent according to claim 1, wherein: the dosage of benzoin dimethyl ether in S2 is 0.75-2% of the mass of the sulfhydryl hyperbranched polyester.
4. The method for preparing a sewage treatment adsorbent according to claim 1, wherein: the concentration of the aqueous solution of sodium carbonate in S5 is 8-12%.
5. The method for preparing the sewage treatment adsorbent according to claim 1, wherein: the solvent in S6 comprises N, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide and N-methylpyrrolidone.
6. The method for preparing the sewage treatment adsorbent according to claim 1, wherein: the reaction in S6 is carried out at 130-150 ℃ for 3-8 h.
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