CN108043362B - Aerogel type heavy metal adsorbent and preparation method thereof - Google Patents
Aerogel type heavy metal adsorbent and preparation method thereof Download PDFInfo
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- CN108043362B CN108043362B CN201711382881.8A CN201711382881A CN108043362B CN 108043362 B CN108043362 B CN 108043362B CN 201711382881 A CN201711382881 A CN 201711382881A CN 108043362 B CN108043362 B CN 108043362B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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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
Abstract
The invention discloses an aerogel type heavy metal adsorbent with large adsorption capacity and high adsorption efficiency and a preparation method thereof, wherein the aerogel type heavy metal adsorbent is prepared by compounding an aerogel material and an organic matter containing a chelating group; the dopamine is used as a bridging substance, the aerogel and the chelating agent are combined together through chemical bonds, the stability is good, and the preparation is convenient.
Description
Technical Field
The invention relates to a heavy metal adsorbent, in particular to a heavy metal adsorbent prepared by compounding an aerogel material and an organic matter containing a chelating group and a preparation method thereof.
Background
Heavy metals in water mainly comprise As, Cu, Cr, Zn, Cd, Pb, Hg and the like, and generally enter water environment through mining, metal smelting, electroplating, chemical wastewater and domestic sewage. Heavy metals are characterized by high toxicity, difficult metabolism in the environment, easy biological enrichment, biological amplification effect and the like, and can cause great harm to human bodies through various ways. Therefore, how to effectively solve the problem of heavy metal pollution and control the potential health risks of heavy metals to human bodies has become a focus of attention of people. The adsorption method is a common method for removing heavy metals in water, and at present, adsorption materials for removing heavy metals comprise activated carbon, bentonite, zeolite, a biological adsorbent, activated alumina, natural or synthetic metal oxides, hydrated oxides thereof and the like. However, the adsorption capacity and the adsorption efficiency of the existing adsorption material are still to be further improved, and the development of a novel adsorption material with large adsorption capacity and high adsorption efficiency becomes an important research direction.
The aerogel is a high-dispersion solid material which is formed by mutually gathering nano-scale microstructures to form a nano-porous network structure, and gaseous dispersion media are filled in pores, and has the characteristics of a nano-porous structure, low density, low dielectric constant, low thermal conductivity coefficient, high porosity, high specific surface area and the like, so that the aerogel shows unique properties in the aspects of mechanics, acoustics, thermal, optics and the like, has wide and huge application value in numerous fields of aerospace, military, petroleum, chemical industry, mineral products, communication, medical use, building materials, electronics, metallurgy and the like, and is called as a magic material for changing the world. By utilizing the characteristics of the nano porous structure, high porosity, high specific surface area and the like of the aerogel material, the aerogel material is expected to be applied to the heavy metal adsorbent material.
Disclosure of Invention
The invention aims to: provides an aerogel type heavy metal adsorbent with large adsorption capacity and high adsorption efficiency and a preparation method thereof.
The object of the invention is achieved by:
an aerogel type heavy metal adsorbent is prepared by compounding aerogel materials and organic matters containing chelating groups;
the aerogel material comprises at least one of silica aerogel, titania aerogel, carbon aerogel, graphene aerogel, and composites thereof;
the aerogel material can be in the forms of powder, granules, blocks and the like; the aerogel material has an average pore diameter of 1-100 nm and a specific surface area of 100-1500 m 2/g;
the preparation method of the organic matter containing the chelating group comprises the following steps:
(1) dissolving chelating agent in deionized water, adding N-hydroxysuccinimide (NHS) and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDS), adjusting pH to 5-7, and performing activation reaction at 20-50 deg.C to obtain intermediate liquid;
(2) adding dopamine into the intermediate solution, adjusting pH to 3-7, and stirring at room temperature for 10-40h to obtain reaction solution;
(3) adding ether into the reaction solution to generate a precipitate, centrifugally collecting, and drying in vacuum to obtain an organic matter containing a chelating group;
the chelating agent is at least one of ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), diethylenetriaminepentaacetic acid (DTPA), ethyleneglycol bistetraacetic acid (EGTA), ethylenediamine diacetic acid (EDDHA), cyclohexanediaminetetraacetic acid (CDTA), S-ethylenediamine disuccinic acid (S, S-EDDS), diethyltriacetic acid (NTA), glutamic acid N, N-diacetic acid tetrasodium (GLDA), methylglycinediacetic acid (MGDA), hydroxyethylethylenediamine triacetic acid (HEDTA), Dihydroxyethylglycine (DEG), and salts thereof;
the mass ratio of the chelating agent to the deionized water to the NHS to the EDS is 1: (1-200): (0.1-10): (0.1-10);
the mass ratio of the intermediate solution to the dopamine is 1: (0.001-1);
the preparation method of the aerogel type heavy metal adsorbent comprises the following steps:
(1) mixing aerogel material with alcohol solvent and deionized water, soaking completely, and adjusting pH to 7-11 to obtain aerogel solution;
the aerogel material, the alcohol solvent and the deionized water are mixed according to a mass ratio of 1: (0.1-100): (0.1-200);
the alcohol solvent is at least one of ethanol, methanol, isopropanol and n-butanol;
(2) dissolving organic matter containing chelating group in deionized water to obtain organic matter solution containing chelating group in 0.1-10 wt%;
(3) dropwise adding the organic matter solution containing the chelating group into the aerogel solution, and reacting for 1-24h at 20-60 ℃ to obtain aerogel reaction liquid;
the mass ratio of the organic matter solution containing the chelating group to the aerogel solution is 1: (0.1-100);
(4) filtering, washing and drying the aerogel reaction solution to obtain an aerogel type heavy metal adsorbent;
the filtration is to remove the liquid in the aerogel reaction liquid by adopting a filtration mode;
the washing is to remove unreacted organic matters containing chelating groups by adopting an organic solvent or water;
the drying is at least one of normal pressure drying or supercritical drying;
the atmospheric drying can be carried out under atmospheric conditions and at 40-200 deg.C.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. according to the project, the aerogel material and the chelating agent are combined, and the prepared adsorbent has the characteristics of large adsorption capacity and high adsorption efficiency by utilizing the large specific surface area and pore volume of the aerogel material and the heavy metal combination effect of the chelating agent.
2. The project utilizes dopamine as a bridging substance, combines the aerogel and the chelating agent together through chemical bonds, and has good stability and convenient preparation.
Detailed Description
The following describes in detail specific embodiments of the present invention with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Preparation of organic matter containing chelating group
Dissolving 10g of chelating agent in 100g of deionized water, adding 5g of N-hydroxysuccinimide (NHS) and 10g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDS), adjusting the pH value to 5, and carrying out an activation reaction at 30 ℃ to obtain an intermediate solution; adding 10g of dopamine into 100g of intermediate solution, adjusting the pH value to 4, and stirring at normal temperature for reaction for 24 hours to obtain reaction solution; adding ether into the reaction solution to generate a precipitate, centrifugally collecting, and drying in vacuum to obtain an organic matter containing a chelating group;
(2) preparation of gel type heavy metal adsorbent
Mixing 10g of aerogel material, 200g of ethanol solvent and deionized water, and after completely soaking, adjusting the pH value to 7 to obtain aerogel solution; dissolving organic matters containing chelating groups into deionized water to obtain organic matter solution containing chelating groups, wherein the organic matters containing chelating groups account for 10% by mass; dropwise adding 10g of organic matter solution containing chelating groups into the aerogel solution, and reacting for 12h at 40 ℃ to obtain aerogel reaction liquid; and filtering the aerogel reaction solution to remove the liquid in the aerogel reaction solution, washing to remove unreacted chelate groups, and drying at the normal pressure and the temperature of 80 ℃ to obtain the aerogel-type heavy metal adsorbent. Wherein the aerogel material is silicon dioxide aerogel powder with the grain diameter of 20-100 μm and the specific surface area of 800m 2/g.
The prepared heavy metal adsorbent is placed in 150mL of water containing Cu, Cr, Zn, Cd and Pb ions for desorption
Removing metal ions, wherein the contents of Cu, Cr, Zn, Cd and Pb ions in water are respectively 0.05mg/L, adding 2g of adsorbent, oscillating for 40 minutes (the temperature is 25 ℃, the oscillation rate is 130r/min) on a constant temperature oscillator under the condition of pH5.5,
collecting supernatant, filtering with 0.45 μm filter membrane, and analyzing the concentration of residual heavy metal ions in the supernatant with ICP-OES
The removal rate of heavy metal ions can reach more than 96%; the adsorption kinetics performance detection shows that the adsorbent can reach adsorption balance in about 10 min.
Example 2
(1) Preparation of organic matter containing chelating group
Dissolving 10g of chelating agent in 500g of deionized water, adding 10g of N-hydroxysuccinimide (NHS) and 5g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDS), adjusting the pH value to 7, and carrying out an activation reaction at 30 ℃ to obtain an intermediate solution; adding 5g of dopamine into 100g of intermediate solution, adjusting the pH value to 8, and stirring at normal temperature for reacting for 40 hours to obtain reaction solution; adding ether into the reaction solution to generate a precipitate, centrifugally collecting, and drying in vacuum to obtain an organic matter containing a chelating group;
(2) preparation of gel type heavy metal adsorbent
Mixing 10g of aerogel material, 600g of methanol solvent and deionized water, and after completely soaking, adjusting the pH value to 10 to obtain aerogel solution; dissolving organic matters containing chelating groups into deionized water to obtain a chelating group-containing organic matter solution with the chelating group-containing organic matters accounting for 0.1 mass percent; dropwise adding 10g of organic matter solution containing chelating groups into the aerogel solution, and reacting for 12h at 60 ℃ to obtain aerogel reaction liquid; and filtering the aerogel reaction solution to remove the liquid in the aerogel reaction solution, washing to remove unreacted chelate groups, and performing supercritical drying to obtain the aerogel-type heavy metal adsorbent. Wherein the aerogel material adopts silicon dioxide aerogel microspheres, the particle size is 3mm, and the specific surface area is 1200m 2/g.
The prepared heavy metal adsorbent is placed in 150mL of water containing Cu, Cr, Zn, Cd and Pb ions for desorption
Removing metal ions, wherein the contents of Cu, Cr, Zn, Cd and Pb ions in water are respectively 0.05mg/L, adding 2g of adsorbent, oscillating for 40 minutes (the temperature is 25 ℃, the oscillation rate is 130r/min) on a constant temperature oscillator under the condition of pH5.5,
collecting supernatant, filtering with 0.45 μm filter membrane, and analyzing the concentration of residual heavy metal ions in the supernatant with ICP-OES
The removal rate of heavy metal ions can reach more than 99 percent; the adsorption kinetics performance detection shows that the adsorbent can reach adsorption balance in about 8 min.
Example 3
(1) Preparation of organic matter containing chelating group
Dissolving 10g of chelating agent in 2000g of deionized water, adding 20g of N-hydroxysuccinimide (NHS) and 30g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDS), adjusting the pH value to 6, and carrying out an activation reaction at 30 ℃ to obtain an intermediate solution; adding 20g of dopamine into 100g of intermediate solution, adjusting the pH value to 4.5, and stirring at normal temperature for reaction for 10 hours to obtain reaction solution; adding ether into the reaction solution to generate a precipitate, centrifugally collecting, and drying in vacuum to obtain an organic matter containing a chelating group;
(2) preparation of gel type heavy metal adsorbent
Mixing 10g of aerogel material, 1000g of isopropanol solvent and deionized water, and after completely soaking, adjusting the pH value to 8 to obtain aerogel solution; dissolving organic matters containing chelating groups into deionized water to obtain a chelating group-containing organic matter solution with the chelating group-containing organic matters accounting for 2 mass percent; dropwise adding 30g of organic matter solution containing chelating groups into the aerogel solution, and reacting for 2h at 40 ℃ to obtain aerogel reaction liquid; and filtering the aerogel reaction solution to remove the liquid in the aerogel reaction solution, washing to remove unreacted chelate groups, and drying at 120 ℃ under normal pressure to obtain the aerogel-type heavy metal adsorbent. Wherein the aerogel material adopts carbon aerogel blocks with the size of about 2-100 mm and the specific surface area of 700m 2/g.
The prepared heavy metal adsorbent is placed in 150mL of water containing Cu, Cr, Zn, Cd and Pb ions for desorption
Removing metal ions, wherein the contents of Cu, Cr, Zn, Cd and Pb ions in water are respectively 0.05mg/L, adding 2g of adsorbent, oscillating for 40 minutes (the temperature is 25 ℃, the oscillation rate is 130r/min) on a constant temperature oscillator under the condition of pH5.5,
collecting supernatant, filtering with 0.45 μm filter membrane, and analyzing the concentration of residual heavy metal ions in the supernatant with ICP-OES
The removal rate of heavy metal ions can reach more than 98 percent; the adsorption kinetics performance detection shows that the adsorbent can reach adsorption balance within 15 min.
Example 4
(1) Preparation of organic matter containing chelating group
Dissolving 10g of chelating agent in 1000g of deionized water, adding 50g of N-hydroxysuccinimide (NHS) and 20g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDS), adjusting the pH value to 6, and carrying out an activation reaction at 45 ℃ to obtain an intermediate solution; adding 80g of dopamine into 100g of intermediate solution, adjusting the pH value to 4.5, and stirring at normal temperature for reaction for 32 hours to obtain reaction solution; adding ether into the reaction solution to generate a precipitate, centrifugally collecting, and drying in vacuum to obtain an organic matter containing a chelating group;
(2) preparation of gel type heavy metal adsorbent
Mixing 10g of aerogel material, 800g of ethanol solvent and deionized water, and after completely soaking, adjusting the pH value to 8 to obtain aerogel solution; dissolving organic matters containing chelating groups into deionized water to obtain a chelating group-containing organic matter solution with the chelating group-containing organic matters accounting for 0.1 mass percent; dropwise adding 100g of organic matter solution containing chelating groups into the aerogel solution, and reacting for 1h at 40 ℃ to obtain aerogel reaction liquid; and filtering the aerogel reaction solution to remove the liquid in the aerogel reaction solution, washing to remove unreacted chelate groups, and performing supercritical drying to obtain the aerogel-type heavy metal adsorbent. The aerogel material is a graphene aerogel block with the size of about 2-100 mm and the specific surface area of 1300m 2/g.
The prepared heavy metal adsorbent is placed in 150mL of water containing Cu, Cr, Zn, Cd and Pb ions for desorption
Removing metal ions, wherein the contents of Cu, Cr, Zn, Cd and Pb ions in water are respectively 0.05mg/L, adding 2g of adsorbent, oscillating for 40 minutes (the temperature is 25 ℃, the oscillation rate is 130r/min) on a constant temperature oscillator under the condition of pH5.5,
collecting supernatant, filtering with 0.45 μm filter membrane, and analyzing the concentration of residual heavy metal ions in the supernatant with ICP-OES
The removal rate of heavy metal ions can reach more than 99 percent; the adsorption kinetics performance detection shows that the adsorbent can reach adsorption balance within 5 min.
Claims (1)
1. The aerogel type heavy metal adsorbent is characterized by being prepared by compounding aerogel materials and organic matters containing chelating groups;
the aerogel material comprises at least one of silica aerogel, titania aerogel, carbon aerogel, and composites thereof;
the preparation method of the organic matter containing the chelating group comprises the following steps:
(1) dissolving a chelating agent in deionized water, adding N-hydroxysuccinimide (NHS) and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDS), adjusting the pH value to 5-7, and performing an activation reaction at 20-50 ℃ to obtain an intermediate solution;
(2) adding dopamine into the intermediate solution, adjusting the pH value to 3-7, and stirring at normal temperature for reaction for 10-40h to obtain a reaction solution;
(3) adding ether into the reaction solution to generate a precipitate, centrifugally collecting, and drying in vacuum to obtain an organic matter containing a chelating group;
the chelating agent is at least one of ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), diethylenetriaminepentaacetic acid (DTPA), ethyleneglycol bistetraacetic acid (EGTA), ethylenediamine diacetic acid (EDDHA), cyclohexanediaminetetraacetic acid (CDTA), S-ethylenediamine disuccinic acid (S, S-EDDS), diethyltriacetic acid (NTA), glutamic acid N, N-diacetic acid tetrasodium (GLDA), methylglycinediacetic acid (MGDA), hydroxyethylethylenediamine triacetic acid (HEDTA), Dihydroxyethylglycine (DEG), and salts thereof;
the mass ratio of the chelating agent to the deionized water to the NHS to the EDS is 1: (1-200): (0.1-10): (0.1-10);
the mass ratio of the intermediate solution to the dopamine is 1: (0.001-1);
the preparation method of the aerogel type heavy metal adsorbent comprises the following steps:
(1) mixing the aerogel material with an alcohol solvent and deionized water, and adjusting the pH value to 7-11 after completely soaking to obtain an aerogel solution; the aerogel material, the alcohol solvent and the deionized water are mixed according to a mass ratio of 1: (0.1-100): (0.1-200); the alcohol solvent is at least one of ethanol, methanol, isopropanol and n-butanol;
(2) dissolving organic matters containing chelating groups in deionized water to obtain organic matter solution containing chelating groups, wherein the mass percent of the organic matters containing chelating groups is 0.1-10%;
(3) dropwise adding the organic matter solution containing the chelating group into the aerogel solution, and reacting for 1-24h at the temperature of 20-60 ℃ to obtain aerogel reaction liquid; the mass ratio of the organic matter solution containing the chelating group to the aerogel solution is 1: (0.1-100);
(4) filtering, washing and drying the aerogel reaction solution to obtain an aerogel type heavy metal adsorbent; the drying is at least one of normal pressure drying or supercritical drying.
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