CN111254701B - Aramid nanofiber composite material, preparation method thereof and application of aramid nanofiber composite material in adsorption of Hg ions in solution - Google Patents
Aramid nanofiber composite material, preparation method thereof and application of aramid nanofiber composite material in adsorption of Hg ions in solution Download PDFInfo
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- CN111254701B CN111254701B CN202010170475.0A CN202010170475A CN111254701B CN 111254701 B CN111254701 B CN 111254701B CN 202010170475 A CN202010170475 A CN 202010170475A CN 111254701 B CN111254701 B CN 111254701B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
Abstract
The invention relates to the field of preparation and application of composite materials, in particular to an aramid nanofiber composite material, a preparation method thereof and application thereof in adsorbing Hg ions in a solution. The preparation method of the aramid nano-fiber composite material is simple to operate, less in material consumption, uniform in obtained appearance, and uniform in dispersion of nano-metal particles in the porous structure of the aramid fiber; the aramid nano-fiber and Ag composite material obtained by the invention can be applied to heavy metal adsorption, particularly has the adsorption rate of Hg ions in a solution as high as more than 90%, and has the saturated adsorption capacity of 298mg/g at 25 ℃.
Description
Technical Field
The invention relates to the field of preparation and application of composite materials, in particular to an aramid nanofiber composite material, a preparation method thereof and application thereof in adsorbing Hg ions in a solution.
Background
The aramid nano-fiber has a special molecular structure, inherits and exceeds the good performance of a macroscopic PPTA fiber. The composite material is easy to disperse, is convenient to be compounded with other materials, has good heat insulation and oxidation resistance, and has wide application prospect in the fields of supercapacitors, diaphragm materials, high temperature resistant filtering materials and the like.
Aramid nanofibers are chosen because of their large surface area and surface energy. Because adjacent atoms are lacked around the surface atoms, the unsaturated degree of the modified epoxy resin is higher, the modified epoxy resin can form stable bonding force with other atoms, can be bonded with various atoms, and has high chemical activity and large modification space. The special molecular structure, the larger porosity and the metal ions of the nano composite material are synthesized into the nano composite material, and the nano composite material is used for adsorbing the metal ions in the wastewater or used for catalysts, material fillers and the like. Many methods for compounding aramid nano-fiber with other materials exist, but most of the methods are complex in operation, harsh in experimental conditions and extremely high in cost, and are difficult to be used for large-scale production.
In the field of adsorption of heavy metal ions, such as Hg ions, Ag nanoparticles can form silver amalgam metal compounds with Hg ions, and silver amalgam is commonly used for filling tooth bodies and is a safe and good adsorbent for removing mercury in wastewater. At present, researchers commonly use graphene as a silver-loaded material, and the large surface area of the graphene provides a good carrier for mercury adsorbents, but the graphene adsorption often has the limitations of high cost and difficulty in secondary recovery.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an aramid nano-fiber composite material, a preparation method thereof and application thereof in adsorbing Hg ions in a solution.
The technical scheme for solving the technical problems is as follows: a preparation method of an aramid nanofiber composite material comprises the following steps:
1) adding para-aramid into DMSO (dimethylsulfoxide) dissolved with KOH (potassium hydroxide), and deprotonating to prepare an aramid nanofiber ANFs solution;
2) adding soluble metal salt into DMSO solvent at 20-25 deg.C, and performing ultrasonic treatment for 30min to completely dissolve the soluble metal salt to obtain DMSO solution of the soluble metal salt;
3) dripping the ANFs solution obtained in the step 1) into the DMSO solution of the soluble metal salt obtained in the step 2) by using an injector at the temperature of 20-25 ℃, standing at room temperature, reacting for 5 hours, putting the reactant into a DMF solvent, and stirring at the temperature of 60 ℃ and at the speed of 400r/min for 3-6 hours;
4) and (3) taking out the product stirred in the step 3), repeatedly washing the product with distilled water, and drying the product in a vacuum drying oven at 60 ℃ to obtain the product.
Wherein the mass ratio of KOH to para-aramid in the step 1) is (1-1.5) to 1, and the concentration of the obtained ANFs solution is 2-2.5 mg/mL; in the step 2), the soluble metal salt is any one of silver nitrate, calcium sulfate, barium chloride, copper sulfate, nickel sulfate or lead chloride, and the concentration of metal ions in the DMSO solution of the obtained soluble metal salt is 2-10 mg/mL; in the step 3), the volume ratio of the ANFs solution to the DMSO solution of the soluble metal salt is 1 (2-5).
The second purpose of the invention is to provide the aramid nano-fiber composite material prepared by the preparation method.
The third purpose of the invention is to provide the application of the aramid nano-fiber composite material in the field of heavy metal adsorption, in particular to the application of the aramid nano-fiber and Ag composite material in adsorbing Hg ions in a solution.
Specifically, the aramid nano-fiber and Ag composite material is added into a solution containing mercury ions, the pH value of the solution is adjusted to be 4-6, the temperature of the solution is 25 ℃, the solution is placed into a constant-temperature shaking box for adsorption for 12 hours, and the concentration of the Hg ions in the solution is measured by a flame atomic absorption method.
The invention has the beneficial effects that: the preparation method of the aramid nano-fiber composite material is simple to operate, less in material consumption, uniform in obtained appearance, and uniform in dispersion of nano-metal particles in the porous structure of the aramid fiber; the aramid nano-fiber and Ag composite material obtained by the invention can be applied to heavy metal adsorption, particularly has the adsorption rate of Hg ions in a solution as high as more than 90%, and has the saturated adsorption capacity of 298mg/g at 25 ℃.
Drawings
FIG. 1 is a scanning electron microscope of the composite material of aramid nanofibers and Ag obtained in example 1;
FIG. 2 is a scanning electron microscope of the aramid nanofiber and Cu composite obtained in example 2;
fig. 3 is a scanning electron microscope of the composite material of aramid nanofibers and Ba obtained in example 3;
FIG. 4 is a scanning electron microscope of the composite of the aramid nanofibers and Ca obtained in example 4;
FIG. 5 is a scanning electron microscope of the aramid nanofiber and Ni composite obtained in example 5;
FIG. 6 is a scanning electron microscope of the composite material of aramid nanofibers and Pb obtained in example 6;
FIG. 7 is a schematic diagram showing the effect of pH on adsorption effect;
FIG. 8 is a graph of adsorption kinetics at different temperatures;
FIGS. 9 and 10 are fitted curves of adsorption kinetics at different temperatures;
FIG. 11 is a thermodynamic curve of adsorption at different temperatures;
FIG. 12 is a Lqngmuir adsorption thermodynamics fit curve;
figure 13 is a Freundlich adsorption thermodynamic fit curve.
Detailed Description
The present invention is described below with reference to examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1
A preparation method of an aramid nanofiber composite material comprises the following steps:
(1) adding 0.6g of para-aramid into 50mL of DMSO solvent dissolved with 0.9g of potassium hydroxide, and preparing nanofiber ANFs solution through deprotonation;
(2) adding 0.5g of silver nitrate into 50mL of DMSO solvent at the temperature of 20-25 ℃, and carrying out ultrasonic treatment for 15-30min to completely dissolve the silver nitrate;
(3) dripping the ANFs solution into 50mL of DMSO solvent dissolved with 0.5g of silver nitrate, fully reacting for 5h, placing the reactant in DMF solvent, and stirring for 3h at the temperature of 60 ℃ and at the speed of 400 r/min;
(4) and taking out the materials, repeatedly washing the materials by using distilled water, and drying the materials to obtain the composite material.
Example 2
A preparation method of an aramid nanofiber composite material comprises the following steps:
(1) adding 0.6g of para-aramid into 50mL of DMSO solvent dissolved with 0.9g of potassium hydroxide, and preparing nanofiber ANFs solution through deprotonation;
(2) adding 0.5g of copper sulfate into 50mL of DMSO solvent at the temperature of 20-25 ℃, and carrying out ultrasonic treatment for 15-30min to completely dissolve the copper sulfate;
(3) dripping the ANFs solution into 50mL of DMSO solvent dissolved with 0.5g of copper sulfate, fully reacting for 5h, placing the reactant in DMF solvent, and stirring for 4h at the temperature of 60 ℃ and at the speed of 400 r/min;
(4) and taking out the materials, repeatedly washing the materials by using distilled water, and drying the materials to obtain the composite material.
Example 3
A preparation method of an aramid nanofiber composite material comprises the following steps:
(1) adding 0.6g of para-aramid into 50mL of DMSO solvent dissolved with 0.9g of potassium hydroxide, and preparing nanofiber ANFs solution through deprotonation;
(2) adding 0.5g of barium sulfate into 50mL of DMSO solvent at the temperature of 20-25 ℃, and carrying out ultrasonic treatment for 15-30min to completely dissolve the barium sulfate;
(3) dripping the ANFs solution into 50mL DMSO solvent containing 0.5g barium sulfate, fully reacting for 5h, placing the reactant in DMF solvent, stirring for 5h at 60 ℃ under the condition of 400 r/min;
(4) and taking out the materials, repeatedly washing the materials by using distilled water, and drying the materials to obtain the composite material.
Example 4
A preparation method of an aramid nanofiber composite material comprises the following steps:
(1) adding 0.6g of para-aramid into 50mL of DMSO solvent dissolved with 0.9g of potassium hydroxide, and preparing nanofiber ANFs solution through deprotonation;
(2) adding 0.5g of calcium chloride into 50mL of DMSO solvent at the temperature of 20-25 ℃, and carrying out ultrasonic treatment for 15-30min to completely dissolve the calcium chloride;
(3) dripping the ANFs solution into 50mL of DMSO solvent containing 0.5g of calcium chloride, fully reacting for 5h, placing the reactant in DMF solvent, and stirring for 6h at the temperature of 60 ℃ and at the speed of 400 r/min;
(4) and taking out the materials, repeatedly washing the materials by using distilled water, and drying the materials to obtain the composite material.
Example 5
A preparation method of an aramid nanofiber composite material comprises the following steps:
(1) adding 0.6g of para-aramid into 50mL of DMSO solvent dissolved with 0.9g of potassium hydroxide, and preparing nanofiber ANFs solution through deprotonation;
(2) adding 0.5g of nickel sulfate into 50mL of DMSO solvent at the temperature of 20-25 ℃, and carrying out ultrasonic treatment for 15-30min to completely dissolve the nickel sulfate;
(3) dripping the ANFs solution into 50mL of DMSO solvent containing 0.5g of nickel sulfate, fully reacting for 5h, placing the reactant in DMF solvent, and stirring for 3h at the temperature of 60 ℃ and at the speed of 400 r/min;
(4) and taking out the materials, repeatedly washing the materials by using distilled water, and drying the materials to obtain the composite material.
Example 6
A preparation method of an aramid nanofiber composite material comprises the following steps:
(1) adding 0.6g of para-aramid into 50mL of DMSO solvent dissolved with 0.9g of potassium hydroxide, and preparing nanofiber ANFs solution through deprotonation;
(2) adding 0.5g of lead sulfate into 50mL of DMSO solvent at the temperature of 20-25 ℃, and carrying out ultrasonic treatment for 15-30min to completely dissolve the lead sulfate;
(3) dripping the ANFs solution into 50mL of DMSO solvent containing 0.5g of lead sulfate, fully reacting for 5h, placing the reactant in DMF solvent, and stirring for 3h at the temperature of 60 ℃ and at the speed of 400 r/min;
(4) and taking out the materials, repeatedly washing the materials by using distilled water, and drying the materials to obtain the composite material.
Fig. 1 to fig. 6 are scanning electron microscopes of the aramid nanofibers and the metal composite material obtained in examples 1 to 6, respectively, and it can be seen that the nano metal particles are loaded in the reticular aramid nanofibers, and the nano metal particles are uniformly distributed in the porous structure of the aramid nanofibers and have uniform size.
Applications of
Adding 25mg of the aramid nanofiber and Ag composite material of example 1 into 100mL of 100 mg-
And (3) respectively adjusting the pH values of the solutions to be 1, 2, 3, 4, 5 and 6 in the L mercuric nitrate solution, respectively adjusting the temperatures of the solutions to be 15 ℃, 25 ℃ and 35 ℃, putting the solutions into a constant-temperature shaking box for adsorption for 12 hours, and measuring the concentration of Hg ions in the solutions by a flame atomic absorption method to obtain the adsorption capacity.
By controlling the single variable of the reaction, the optimum adsorption pH of 4-6 and the optimum adsorption temperature of 25 ℃ can be selected from FIGS. 7-13. FIG. 7 is a drawing showingThe effect of pH on adsorption is shown schematically, and it can be seen that the adsorption is better at pH 4-6, with the best adsorption amount of 298 mg/g. FIG. 8 is a graph of adsorption kinetics at different temperatures, with adsorption equilibrium reached at 11 hours of adsorption. FIG. 9 and FIG. 10 are fitting curves of adsorption kinetics at different temperatures, and it can be seen from the fitting data in Table 1 that the fitting R of the second order kinetics 2 2 All reach more than 0.99, and are greater than first-order kinetic fitting R 1 2 And determining to accord with the second-order kinetic adsorption. Fig. 11 is a thermodynamic adsorption curve at different temperatures, fig. 12 and fig. 13 are a thermodynamic adsorption fit curve of Lqngmuir and a thermodynamic adsorption fit curve of Freundlich, and it can be seen from the fit data in table 2 that the Lqngmuir adsorption is satisfied.
TABLE 1
TABLE 2
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (1)
1. The preparation method of the aramid nanofiber composite material is characterized by comprising the following steps of:
1) adding para-aramid into DMSO (dimethylsulfoxide) dissolved with KOH (potassium hydroxide), and deprotonating to prepare an aramid nanofiber ANFs solution;
2) adding soluble metal salt into DMSO solvent at 20-25 deg.C, and performing ultrasonic treatment for 30min to completely dissolve the soluble metal salt to obtain DMSO solution of the soluble metal salt;
3) dripping the ANFs solution obtained in the step 1) into the DMSO solution of the soluble metal salt obtained in the step 2) by using an injector at the temperature of 20-25 ℃, standing at room temperature, reacting for 5 hours, putting the reactant into a DMF solvent, and stirring at the temperature of 60 ℃ and at the speed of 400r/min for 3-6 hours;
4) taking out the product after stirring in the step 3), repeatedly washing the product with distilled water, and drying the product in a vacuum drying oven at 60 ℃ to obtain the product;
in the step 1), the mass ratio of KOH to para-aramid is (1-1.5) to 1; the concentration of the obtained ANFs solution is 2-2.5 mg/mL;
in the step 2), the soluble metal salt is any one of silver nitrate, calcium sulfate, barium chloride, copper sulfate, nickel sulfate or lead chloride; the concentration of metal ions in the DMSO solution of the obtained soluble metal salt is 2-10 mg/mL;
in the step 3), the volume ratio of the ANFs solution to the DMSO solution of the soluble metal salt is 1 (2-5).
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| JP2010255140A (en) * | 2009-04-27 | 2010-11-11 | Teijin Techno Products Ltd | Aramid fiber |
| US10160833B2 (en) * | 2012-04-26 | 2018-12-25 | The Regents Of The University Of Michigan | Synthesis and use of aramid nanofibers |
| CN103042225B (en) * | 2012-11-05 | 2015-05-13 | 中科院广州化学有限公司 | Linear nano silver and preparation method and application thereof |
| CN103937237A (en) * | 2014-04-16 | 2014-07-23 | 鲁东大学 | P-aramid nanofiber solution and preparation method thereof |
| CN104532553A (en) * | 2014-12-19 | 2015-04-22 | 东华大学 | Method for chemical silver-plating of aramid conductive fibers |
| CN105749865A (en) * | 2016-04-12 | 2016-07-13 | 中国科学院合肥物质科学研究院 | Preparation method and application of three-dimensional graphene/silver composite |
| CN106179497B (en) * | 2016-07-08 | 2019-04-09 | 上海电力学院 | A kind of preparation method of metal nanoparticles loaded nano-fiber composite film |
| CN108285540B (en) * | 2018-02-11 | 2020-09-29 | 陕西科技大学 | Preparation method of water-dispersible aramid nanofiber and aramid nano paper |
| CN108912350B (en) * | 2018-06-13 | 2021-05-07 | 中科广化（重庆）新材料研究院有限公司 | Spherical aramid fiber nano material and preparation method thereof |
| CN110055797B (en) * | 2019-04-25 | 2021-08-10 | 陕西科技大学 | Method for preparing aramid nano-fiber |
| CN110258170A (en) * | 2019-06-26 | 2019-09-20 | 陕西科技大学 | A kind of Nano silver grain modification hexagonal boron nitride/aramid nano-fiber heat-conductive composite material preparation method |
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