CN114130372A - Basalt fiber modified adsorption filler and preparation method thereof - Google Patents
Basalt fiber modified adsorption filler and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a basalt fiber modified adsorption filler and a preparation method thereof, belonging to the technical field of adsorption material preparation, and comprising the following raw materials in parts by weight: 2-3 parts of aniline, 10-15 parts of attapulgite clay, 0.5-0.8 part of functionalized basalt fiber, 10 parts of ammonium persulfate solution, 5 parts of concentrated hydrochloric acid and 100 parts of deionized water; adding concentrated hydrochloric acid into deionized water, stirring, adding attapulgite clay and functionalized basalt fiber, carrying out ultrasonic treatment, adding an aniline monomer, stirring, adding an ammonium persulfate solution, and finishing reaction to obtain the basalt fiber modified adsorption filler, wherein the functionalized basalt fiber is prepared by the following steps: mixing the modified fiber, 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and isopropanol, performing reflux reaction for 6-8h, and performing reduced pressure distillation, washing and drying to obtain the functionalized basalt fiber; the adsorption filler prepared by the invention can effectively remove heavy metal particles and organic pollutants in sewage.
Description
Technical Field
The invention belongs to the technical field of preparation of adsorption materials, and particularly relates to a basalt fiber modified adsorption filler and a preparation method thereof.
Background
With the rapid development of industrialization and urbanization, industrial wastewater and domestic sewage are discharged wantonly, and industries such as metal mining, steel and nonferrous metal smelting, metal processing and electroplating discharge a large amount of wastewater containing heavy metal ions to the environment every year, so that the pollution of various water bodies is more serious. The heavy metal ions have durability, high toxicity and harmfulness, so that the heavy metal ions become one of the most biohazard and toxic components in the wastewater, and pose a potential threat to the life safety of human beings. The existing printing and dyeing wastewater has high content of organic wastewater and is characterized by large discharge amount, complex components, high organic matter content, deep chromaticity, high chemical oxygen demand (CODcr) and poor biodegradability, and besides dye, auxiliary agent and slurry, the wastewater also contains toxic organic pollutants containing groups such as heavy metal ions, aniline, nitrobenzene, phthalic acid and the like, such as benzene ring, amino, azo and the like, and is difficult to biodegrade and seriously pollutes the environment. The existing treatment methods are more, including an adsorption method, a redox method and a flocculation method, wherein the adsorption method is widely applied, but the existing adsorption filler has strong pertinence, cannot adsorb heavy metal ions and organic pollutants at the same time, has poor universality, and has higher requirements (temperature, concentration and pH) on the adsorption environment, so that the technical problem to be solved is to provide the adsorption filler with good adsorption performance and wide application range.
Disclosure of Invention
The invention aims to provide a basalt fiber modified adsorption filler and a preparation method thereof, and aims to solve the technical problems in the background.
The purpose of the invention can be realized by the following technical scheme:
the basalt fiber modified adsorption filler comprises the following raw materials in parts by weight: 2-3 parts of aniline, 10-15 parts of attapulgite clay, 0.5-0.8 part of functionalized basalt fiber, 10 parts of ammonium persulfate solution, 5 parts of concentrated hydrochloric acid and 100 parts of deionized water;
the basalt fiber modified adsorption filler is prepared by the following steps:
adding concentrated hydrochloric acid into deionized water, uniformly stirring, adding attapulgite clay and functionalized basalt fiber, performing ultrasonic treatment for 30min at the frequency of 40-50kHz to obtain a suspension, then adding an aniline monomer into the suspension, uniformly stirring, adding an ammonium persulfate solution, stirring and reacting at room temperature for 4-6h, after the reaction is finished, performing suction filtration, washing a filter cake with deionized water for 3-5 times, and finally drying at 80 ℃ to constant weight to obtain the basalt fiber modified adsorption filler.
Further, the ammonium persulfate solution is prepared by mixing ammonium persulfate and deionized water according to the weight ratio of 1.8-2.2 g: 10mL of concentrated hydrochloric acid is mixed, and the mass fraction of the concentrated hydrochloric acid is 37 percent.
Further, the attapulgite clay is prepared by the following steps: drying commercially available attapulgite at the temperature of 110-120 ℃ for 2h, transferring to a muffle furnace for calcining at the temperature of 750 ℃ for 3h, and grinding and sieving with a 80-mesh sieve to obtain the attapulgite clay.
Further, the functionalized basalt fiber is prepared by the following steps:
step A1, sequentially adding trimethylolpropane-tris (3-mercaptopropionate) and carbon tetrachloride into a three-neck flask provided with a stirrer and a condenser, stirring and reacting at the temperature of-2-0 ℃ under the protection of nitrogen, slowly dripping mixed liquid a of KH-570, allyl dimethyldithiocarbamate and carbon tetrachloride through a constant-pressure dropping funnel, stirring and reacting at the temperature of-2-0 ℃ for 12 hours, and after the reaction is finished, distilling under reduced pressure to remove the carbon tetrachloride to obtain a macromolecular coupling agent;
wherein the dosage ratio of trimethylolpropane-tri (3-mercaptopropionate), carbon tetrachloride and mixed liquid a is 0.05 mol: 200-250 mL: 150mL, wherein the mixed solution a is prepared from KH-570, allyl dimethyldithiocarbamate and carbon tetrachloride according to the molar ratio of 0.05 mol: 0.05 mol: 150mL of the modified starch is prepared by mixing trimethylolpropane-tris (3-mercaptopropionate) -SH and KH-570, and carrying out chemical reaction on unsaturated C ═ C double bonds in dimethyl allyl dithiocarbamate to obtain a macromolecular coupling agent, wherein the macromolecular coupling agent contains terminal tertiary amino groups, dithiocarbamate groups and siloxane bonds;
step A2, mixing the deposited basalt fiber with an ethanol solution with the mass fraction of 50%, heating to 60 ℃ under magnetic stirring, dropwise adding the ethanol solution of the macromolecular coupling agent through a constant-pressure dropping funnel under the stirring state, protecting the whole reaction process by using argon atmosphere, finishing dropwise adding within 1h, performing reflux reaction for 24h, finishing the reaction, performing suction filtration, washing a filter cake with distilled water for 3-5 times, and then placing the filter cake in a vacuum drying oven for vacuum drying at 50 ℃ for 10h to obtain the modified fiber;
wherein the dosage ratio of the deposited basalt fiber to the ethanol solution of the ethanol solution and the macromolecular coupling agent is 5.5-6.1 g: 80-90 mL: 10mL, the ethanol solution of the macromolecular coupling agent is prepared by mixing the macromolecular coupling agent and absolute ethanol according to the weight ratio of 1.3-1.5 g: 10mL of the modified basalt fiber is mixed, a silicon-oxygen bond of a macromolecular coupling agent is hydrolyzed to obtain a silanol bond, and the silanol bond and a hydroxyl group on the surface of the deposited basalt fiber are subjected to condensation reaction to obtain modified fiber;
step A3, sequentially adding modified fibers, 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and isopropanol into a three-neck flask, heating to reflux reaction for 6-8 hours while stirring, and removing the isopropanol by reduced pressure distillation after the reaction is finished to obtain the functionalized basalt fibers;
wherein the dosage ratio of the modified fiber, the 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride and the isopropanol is 5 g: 1.2-1.3 g: and (3) performing quaternization reaction on 50-70mL of the modified fiber by using terminal tertiary amino and 3-chloro-2-hydroxypropyl trimethyl ammonium chloride to obtain the functional basalt fiber.
Further, the sedimentary basalt fiber is made by the following steps:
b1, cutting the basalt fiber to the length of 20-30mm, then soaking in a nitric acid solution with the concentration of 1mol/L for 8-10h, then taking out, washing with deionized water until the washing liquid is neutral, and then drying at 80 ℃ to constant weight to obtain an acidified fiber;
wherein the dosage ratio of the basalt fiber to the nitric acid solution is 5.8-6.1 g: 60-70 mL;
step B2, mixing ethyl orthosilicate, ethanol and water according to a molar ratio of 2: 3: 2, mixing, adding ammonia water with the mass fraction of 28% under the stirring condition at the temperature of 70 ℃, adjusting the pH value to 8, stirring and reacting for 1-2h to obtain silica sol, adding acidified fibers into the silica sol, soaking for 30-60min, taking out, and roasting in a muffle furnace at the temperature of 450 ℃ for 2h to obtain the deposited basalt fibers;
wherein the dosage ratio of the silica sol to the acidified fiber is 80 mL: 5.8-6.1 g.
The invention has the beneficial effects that:
the method comprises the steps of firstly shearing the existing basalt fiber, then treating the basalt fiber with a nitric acid solution to enable the surface of the basalt fiber to be rich in oxygen-containing groups, then depositing silicon dioxide particles on the surface of the basalt fiber by taking ethyl orthosilicate as a silicon source and ammonia water as a catalyst to increase the surface roughness of the basalt fiber to obtain a deposited basalt fiber, then carrying out a chemical reaction on-SH of trimethylolpropane-tris (3-mercaptopropionate) and KH-570 and terminal unsaturated C-C double bonds in allyl dimethyldithiocarbamate to obtain a macromolecular coupling agent, and modifying the deposited basalt fiber by using the macromolecular coupling agent to obtain a modified fiber; then the modified fiber reacts with 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride to obtain the functional basalt fiber, the surface of the functional basalt fiber is rich in a plurality of functional groups, including dithiocarbamate group, quaternary ammonium salt structure, alcoholic hydroxyl and mercaptan bond, on one hand, the groups can be combined with heavy metal ions and organic pollutants in the wastewater through electrostatic adsorption and coordination, on the other hand, the functionalized basalt fiber has larger specific surface area and physical adsorption performance and can play a role in purification, and the polyaniline molecule contains a large amount of amidogen and imino which have good coordination function to heavy metal ions, and the amino and imino also have reducibility, can be subjected to oxidation-reduction reaction with some heavy metal ions with higher oxidation potential for adsorption, and meanwhile, the polyaniline adsorbent is used for adsorbing Pb.2+、Hg2+The heavy metal ions have an ion exchange function, and the polyaniline has good solvent resistance, so that the polyaniline can be widely applied to various complex adsorption environments.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a functional basalt fiber which is prepared by the following steps:
step A1, sequentially adding 0.05mol of trimethylolpropane-tri (3-mercaptopropionate) and 200mL of carbon tetrachloride into a three-neck flask provided with a stirrer and a condenser, stirring and reacting at the temperature of minus 2 ℃ under the protection of nitrogen, slowly dropwise adding 150mL of mixed solution a through a constant-pressure dropping funnel, stirring and reacting for 12 hours at the temperature of minus 2 ℃, and after the reaction is finished, removing the carbon tetrachloride through reduced pressure distillation to obtain a macromolecular coupling agent, wherein the mixed solution a is prepared from KH-570, dimethyl allyl dithiocarbamate and carbon tetrachloride according to the mol of 0.05: 0.05 mol: 150mL of the mixture is obtained;
step A2, mixing 5.5g of deposited basalt fiber with 80mL of ethanol solution with the mass fraction of 50%, heating to 60 ℃ under magnetic stirring, dropwise adding 10mL of ethanol solution of macromolecular coupling agent through a constant-pressure dropping funnel under the stirring state, using argon atmosphere for protection in the whole reaction process, finishing dropwise adding within 1h, carrying out reflux reaction for 24h, finishing the reaction, carrying out suction filtration, washing a filter cake for 3 times by using distilled water, placing the filter cake in a vacuum drying oven, carrying out vacuum drying for 10h at 50 ℃ to obtain modified fiber, wherein the ethanol solution of the macromolecular coupling agent is prepared from the macromolecular coupling agent and absolute ethyl alcohol according to the weight ratio of 1.3 g: 10mL of the mixture is mixed;
and A3, adding 5g of modified fiber, 1.2g of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and 50mL of isopropanol into a three-neck flask in sequence, heating to reflux reaction for 6 hours while stirring, and removing the isopropanol by reduced pressure distillation after the reaction is finished to obtain the functionalized basalt fiber.
The basalt fiber sediment is prepared by the following steps:
b1, cutting 5.8g of basalt fibers to the length of 20mm, then soaking in 60mL of 1mol/L nitric acid solution for 8h, taking out, washing with deionized water until the washing liquid is neutral, and drying at 80 ℃ to constant weight to obtain acidified fibers;
step B2, mixing ethyl orthosilicate, ethanol and water according to a molar ratio of 2: 3: 2, mixing, adding ammonia water with the mass fraction of 28% under the stirring condition at the temperature of 70 ℃, adjusting the pH value to 8, stirring and reacting for 1h to obtain silica sol, adding 5.8g of acidified fibers into 80mL of silica sol, soaking for 30min, taking out, and roasting in a muffle furnace at the temperature of 450 ℃ for 2h to obtain the deposited basalt fibers.
Example 2
The embodiment provides a functional basalt fiber which is prepared by the following steps:
step A1, sequentially adding 0.05mol of trimethylolpropane-tri (3-mercaptopropionate) and 220mL of carbon tetrachloride into a three-neck flask provided with a stirrer and a condenser, stirring and reacting at the temperature of-1 ℃ under the protection of nitrogen, slowly dropwise adding 150mL of mixed solution a through a constant-pressure dropping funnel, stirring and reacting for 12 hours at the temperature of-1 ℃, after the reaction is finished, distilling under reduced pressure to remove the carbon tetrachloride to obtain a macromolecular coupling agent, wherein the mixed solution a is prepared from KH-570, dimethyl allyl dithiocarbamate and carbon tetrachloride according to the mol of 0.05: 0.05 mol: 150mL of the mixture is obtained;
step A2, mixing 5.8g of deposited basalt fiber with 85mL of ethanol solution with the mass fraction of 50%, heating to 60 ℃ under magnetic stirring, dropwise adding 10mL of ethanol solution of macromolecular coupling agent through a constant-pressure dropping funnel under the stirring state, using argon atmosphere for protection in the whole reaction process, finishing dropwise adding within 1h, carrying out reflux reaction for 24h, finishing the reaction, carrying out suction filtration, washing a filter cake for 4 times by using distilled water, placing the filter cake in a vacuum drying oven, carrying out vacuum drying for 10h at 50 ℃ to obtain modified fiber, wherein the ethanol solution of the macromolecular coupling agent is prepared from the macromolecular coupling agent and absolute ethyl alcohol according to the weight ratio of 1.4 g: 10mL of the mixture is mixed;
and A3, sequentially adding 5g of modified fiber, 1.2g of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and 60mL of isopropanol into a three-neck flask, heating to reflux while stirring for 7h, and after the reaction is finished, removing the isopropanol by reduced pressure distillation to obtain the functionalized basalt fiber.
The basalt fiber sediment is prepared by the following steps:
b1, cutting 5.9g of basalt fibers to a length of 25mm, soaking in 65mL of 1mol/L nitric acid solution for 9h, taking out, washing with deionized water until the washing liquid is neutral, and drying at 80 ℃ to constant weight to obtain acidified fibers;
step B2, mixing ethyl orthosilicate, ethanol and water according to a molar ratio of 2: 3: 2, mixing, adding ammonia water with the mass fraction of 28% under the stirring condition at the temperature of 70 ℃, adjusting the pH value to 8, stirring and reacting for 1.5h to obtain silica sol, adding 5.9g of acidified fibers into 80mL of silica sol, soaking for 45min, taking out, and roasting in a muffle furnace at the temperature of 450 ℃ for 2h to obtain the deposited basalt fibers.
Example 3
The embodiment provides a functional basalt fiber which is prepared by the following steps:
step A1, sequentially adding 0.05mol of trimethylolpropane-tris (3-mercaptopropionate) and 250mL of carbon tetrachloride into a three-neck flask provided with a stirrer and a condenser, stirring and reacting at 0 ℃ under the protection of nitrogen, slowly dropwise adding 150mL of mixed solution a through a constant-pressure dropping funnel, stirring and reacting at 0 ℃ for 12 hours, after the reaction is finished, distilling under reduced pressure to remove carbon tetrachloride to obtain a macromolecular coupling agent, wherein the mixed solution a is prepared from KH-570, dimethyl allyl dithiocarbamate and carbon tetrachloride according to 0.05 mol: 0.05 mol: 150mL of the mixture is obtained;
step A2, mixing 6.1g of deposited basalt fiber with 90mL of ethanol solution with the mass fraction of 50%, heating to 60 ℃ under magnetic stirring, dropwise adding 10mL of ethanol solution of macromolecular coupling agent through a constant-pressure dropping funnel under the stirring state, using argon atmosphere for protection in the whole reaction process, finishing dropwise adding within 1h, carrying out reflux reaction for 24h, finishing the reaction, carrying out suction filtration, washing a filter cake for 5 times by using distilled water, placing the filter cake in a vacuum drying oven, carrying out vacuum drying for 10h at 50 ℃ to obtain modified fiber, wherein the ethanol solution of the macromolecular coupling agent is prepared from the macromolecular coupling agent and absolute ethyl alcohol according to the weight of 1.5 g: 10mL of the mixture is mixed;
and A3, sequentially adding 5g of modified fiber, 1.3g of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and 70mL of isopropanol into a three-neck flask, heating to reflux reaction for 8 hours while stirring, and after the reaction is finished, removing the isopropanol by reduced pressure distillation to obtain the functionalized basalt fiber.
The basalt fiber sediment is prepared by the following steps:
b1, cutting 6.1g of basalt fibers to a length of 30mm, soaking in 70mL of 1mol/L nitric acid solution for 10 hours, taking out, washing with deionized water until the washing liquid is neutral, and drying at 80 ℃ to constant weight to obtain acidified fibers;
step B2, mixing ethyl orthosilicate, ethanol and water according to a molar ratio of 2: 3: 2, mixing, adding 28 mass percent of ammonia water under the stirring condition at the temperature of 70 ℃, adjusting the pH value to 8, stirring and reacting for 2 hours to obtain silica sol, adding 6.1g of acidified fiber into 80mL of silica sol, soaking for 60 minutes, taking out, and roasting in a muffle furnace at the temperature of 450 ℃ for 2 hours to obtain the deposited basalt fiber.
Example 4
The basalt fiber modified adsorption filler comprises the following raw materials in parts by weight: 2 parts of aniline, 10 parts of attapulgite clay, 0.5 part of functionalized basalt fiber in example 1, 10 parts of ammonium persulfate solution, 5 parts of concentrated hydrochloric acid and 100 parts of deionized water;
the basalt fiber modified adsorption filler is prepared by the following steps:
adding concentrated hydrochloric acid into deionized water, uniformly stirring, adding attapulgite clay and functionalized basalt fiber, performing ultrasonic treatment for 30min at the frequency of 40kHz to obtain a suspension, then adding an aniline monomer into the suspension, uniformly stirring, adding an ammonium persulfate solution, stirring at room temperature for reaction for 4h, after the reaction is finished, performing suction filtration, washing a filter cake with deionized water for 3 times, and finally placing at 80 ℃ for drying to constant weight to obtain the basalt fiber modified adsorption filler.
Wherein the ammonium persulfate solution is prepared from ammonium persulfate and deionized water according to the weight ratio of 1.8 g: 10mL of the attapulgite clay is mixed, the mass fraction of the concentrated hydrochloric acid is 37 percent, and the attapulgite clay is prepared by the following steps: drying commercially available attapulgite at 110 deg.C for 2h, transferring to muffle furnace, calcining at 750 deg.C for 3h, grinding, and sieving with 80 mesh sieve to obtain attapulgite clay.
Example 5
The basalt fiber modified adsorption filler comprises the following raw materials in parts by weight: 2.5 parts of aniline, 12 parts of attapulgite clay, 0.7 part of functionalized basalt fiber in example 2, 10 parts of ammonium persulfate solution, 5 parts of concentrated hydrochloric acid and 100 parts of deionized water;
the basalt fiber modified adsorption filler is prepared by the following steps:
adding concentrated hydrochloric acid into deionized water, uniformly stirring, adding attapulgite clay and functionalized basalt fiber, performing ultrasonic treatment for 30min at the frequency of 45kHz to obtain a suspension, then adding an aniline monomer into the suspension, uniformly stirring, adding an ammonium persulfate solution, stirring at room temperature for reaction for 5h, after the reaction is finished, performing suction filtration, washing a filter cake with deionized water for 4 times, and finally drying at 80 ℃ to constant weight to obtain the basalt fiber modified adsorption filler.
Wherein the ammonium persulfate solution is prepared from ammonium persulfate and deionized water according to the weight ratio of 2 g: 10mL of the attapulgite clay is mixed, the mass fraction of the concentrated hydrochloric acid is 37 percent, and the attapulgite clay is prepared by the following steps: drying commercially available attapulgite at 115 deg.C for 2h, transferring to muffle furnace, calcining at 750 deg.C for 3h, grinding, and sieving with 80 mesh sieve to obtain attapulgite clay.
Example 6
The basalt fiber modified adsorption filler comprises the following raw materials in parts by weight: 3 parts of aniline, 15 parts of attapulgite clay, 0.8 part of functionalized basalt fiber in example 3, 10 parts of ammonium persulfate solution, 5 parts of concentrated hydrochloric acid and 100 parts of deionized water;
the basalt fiber modified adsorption filler is prepared by the following steps:
adding concentrated hydrochloric acid into deionized water, uniformly stirring, adding attapulgite clay and functionalized basalt fiber, performing ultrasonic treatment for 30min at the frequency of 50kHz to obtain a suspension, then adding an aniline monomer into the suspension, uniformly stirring, adding an ammonium persulfate solution, stirring at room temperature for reaction for 6h, after the reaction is finished, performing suction filtration, washing a filter cake with deionized water for 5 times, and finally placing at 80 ℃ for drying to constant weight to obtain the basalt fiber modified adsorption filler.
Wherein the ammonium persulfate solution is prepared from ammonium persulfate and deionized water according to the weight ratio of 2.2 g: 10mL of the attapulgite clay is mixed, the mass fraction of the concentrated hydrochloric acid is 37 percent, and the attapulgite clay is prepared by the following steps: drying commercially available attapulgite at 120 deg.C for 2h, transferring to muffle furnace, calcining at 750 deg.C for 3h, grinding, and sieving with 80 mesh sieve to obtain attapulgite clay.
Comparative example 1
The functional basalt fiber in the embodiment 4 is removed, and the rest of the raw materials and the preparation process are unchanged.
Comparative example 2
The functional basalt fiber in the embodiment 4 is replaced by the basalt fiber sold by Chongqing Hetai building materials Co.
Comparative example 3
This comparative example is the product of example 1 of the invention patent publication No. CN 107970881A.
The same sewage treatment test was performed on the adsorbing fillers of examples 4 to 6 and comparative examples 1 to 3, and the COD removal rate was calculated, and the test results are shown in table 1:
TABLE 1
As can be seen from Table 1, the adsorptive fillers of examples 4-6 have better COD removal than those of comparative examples 1-3.
The same Congo red dye of 10mL/L was treated with the same adsorptive filler of examples 4-6 and comparative examples 1-3 at an amount of 0.5g/L and the decolorization ratio (%) was calculated as shown in Table 2:
TABLE 2
As can be seen from Table 2, the adsorptive fillers of examples 4-6 have better decolorization ratios for organic dyes than comparative examples 1-3.
The same heavy metal wastewater containing Pb was treated with the adsorbing fillers of examples 4 to 6 and comparative examples 1 to 32+、Hg2+、Cd2+And Cr6+The addition amount was 0.4g/L, and the metal ion removal rate was calculated, and the results are shown in Table 3:
TABLE 3
| Example 4 | Example 5 | Example 6 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Pb2+Removal rate | 98.89 | 98.83 | 98.91 | 81.44 | 85.21 | 87.17 |
| Hg2+Removal rate | 98.75 | 99.23 | 99.15 | 83.52 | 84.67 | 86.12 |
| Cd2+Removal rate | 99.14 | 99.24 | 99.25 | 82.11 | 84.23 | 85.18 |
| Cr6+Removal rate | 97.71 | 97.9 | 98.14 | 81.25 | 83.85 | 86.12 |
As can be seen from Table 3, the metal ion removal rates of examples 4 to 6 are better than those of comparative examples 1 to 3, and in conclusion, the adsorption filler prepared by the invention has better sewage purification effect.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (6)
1. The basalt fiber modified adsorption filler is characterized by comprising the following raw materials in parts by weight: 2-3 parts of aniline, 10-15 parts of attapulgite clay, 0.5-0.8 part of functionalized basalt fiber, 10 parts of ammonium persulfate solution, 5 parts of concentrated hydrochloric acid and 100 parts of deionized water;
the functional basalt fiber is prepared by the following steps:
adding modified fiber, 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and isopropanol into a three-neck flask in sequence, heating to reflux reaction for 6-8h while stirring, and removing the isopropanol by reduced pressure distillation after the reaction is finished to obtain the functionalized basalt fiber.
2. The basalt fiber-modified adsorptive filler according to claim 1, wherein the modified fiber is prepared by the steps of:
mixing the deposited basalt fiber with an ethanol solution, heating to 60 ℃ under magnetic stirring, dripping the ethanol solution of the large molecular coupling agent under stirring, protecting the whole reaction process by using argon atmosphere, finishing dripping within 1h, performing reflux reaction for 24h, finishing the reaction, performing suction filtration, washing a filter cake, and drying to obtain the modified fiber.
3. The basalt fiber-modified adsorptive filler according to claim 2, wherein the ethanol solution of the macromolecular coupling agent is prepared from the macromolecular coupling agent and absolute ethanol in a weight ratio of 1.3 to 1.5 g: 10mL of the above-mentioned components were mixed.
4. The basalt fiber-modified adsorptive filler according to claim 3, wherein the macromolecular coupling agent is prepared by:
sequentially adding trimethylolpropane-tri (3-mercaptopropionate) and carbon tetrachloride into a three-neck flask, stirring and reacting at the temperature of-2-0 ℃ under the protection of nitrogen, dropwise adding a mixed solution a of KH-570, allyl dimethyldithiocarbamate and carbon tetrachloride, stirring and reacting at the temperature of-2-0 ℃ for 12 hours, and carrying out reduced pressure distillation to obtain the macromolecular coupling agent.
5. The basalt fiber-modified adsorptive filler according to claim 4, wherein mixed liquor a is prepared from KH-570, allyl dimethyldithiocarbamate and carbon tetrachloride in an amount of 0.05 mol: 0.05 mol: 150mL of the mixture.
6. The preparation method of the basalt fiber modified adsorption filler according to claim 1, characterized by comprising the following steps:
adding concentrated hydrochloric acid into deionized water, uniformly stirring, adding attapulgite clay and functionalized basalt fiber, performing ultrasonic treatment for 30min at the frequency of 40-50kHz to obtain a suspension, then adding an aniline monomer into the suspension, uniformly stirring, adding an ammonium persulfate solution, stirring and reacting at room temperature for 4-6h, after the reaction is finished, performing suction filtration, washing a filter cake with deionized water for 3-5 times, and finally drying at 80 ℃ to constant weight to obtain the basalt fiber modified adsorption filler.
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| CN116199460A (en) * | 2023-02-27 | 2023-06-02 | 浙江新都水泥有限公司 | High-crack-resistance wear-resistant cement and preparation method thereof |
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