CN107915803B - Method for preparing nano composite gel for removing divalent cadmium in wastewater - Google Patents
Method for preparing nano composite gel for removing divalent cadmium in wastewater Download PDFInfo
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- CN107915803B CN107915803B CN201710992186.7A CN201710992186A CN107915803B CN 107915803 B CN107915803 B CN 107915803B CN 201710992186 A CN201710992186 A CN 201710992186A CN 107915803 B CN107915803 B CN 107915803B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0069—Post treatment
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic 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
- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a method for preparing nano composite gel for removing divalent cadmium in wastewater, which comprises the following steps: taking hydroxyethyl chitosan and clinoptilolite as raw materials, grafting acrylamide to hydroxyethyl chitosan macromolecules through a free radical graft copolymerization reaction, mixing the hydroxyethyl chitosan macromolecules and the clinoptilolite, cleaning and drying a resultant, and performing ball milling to obtain the nano-scale clinoptilolite/hydroxyethyl chitosan graft copolymer composite gel; the nano composite gel adsorbent obtained by the method is in a grey white powder shape, can efficiently remove divalent cadmium ions in wastewater, has no pollution to the environment, is green and environment-friendly, and not only can improve the comprehensive utilization efficiency of natural macromolecules such as chitosan derivatives and clinoptilolite, but also can improve the comprehensive utilization efficiency of Cd in heavy metal wastewater2+The efficient adsorption and removal provides a feasible scheme, and the application prospect is wide.
Description
Technical Field
The invention relates to a method for preparing selectively adsorbed divalent cadmium ions (Cr)2+) The method of clinoptilolite/hydroxyethyl chitosan grafted copolymer nanometer composite gel belongs to the field of natural polymer modified material technology.
Background
With the rapid development of industry, wastewater containing many potentially toxic metals is released in large quantities in surface and underground water, and the problem of water pollution is receiving increasing attention. Among these industries, the mineral and metallurgical industries play a major role in water pollution, not only directly discharging waste liquid containing heavy metal ions into the river system, but also discarding untreated solid waste containing residual metals into the environment. Solid waste such as slag and the like is dumped in the environment, and heavy metal ions are still continuously migrated to surface water and underground water as time goes on. Some heavy metal ions, e.g. Pb2+And Cd2+Even at relatively low concentrations, can have negative effects on aquatic flora and human health. The removal of these heavy metal ions from the environment requires the development of effective and sustainable technical solutions. Several techniques for removing heavy metal ions have been available for many years, such as chemical precipitation, redox, osmosis, electrolysis, etc., but the success is not obvious. Since these processes either cost expensive removal or form new solid waste byproducts. Among the numerous treatment methods, adsorption techniques have become heavy metal removalOne of the research hotspots of (1).
Many adsorbents have been successfully applied to remove metal ions in wastewater, but biomass adsorbents are often preferred due to their unique properties such as biodegradability, low cost and abundant availability. The biomass adsorbent has the characteristics of rich raw material sources, multiple varieties, low cost, good treatment effect under low concentration, large adsorption capacity, high speed, good selectivity, simple adsorption equipment, easy operation and the like, and has wide application prospect in the aspect of removing heavy metals in water. Raw materials for biomass adsorbents include gums, collagen, cellulose, alginate, carrageenan, and chitosan. Hydrogels made based on biomass polymers whose adsorption behavior can be improved by incorporating nanoparticles of any other foreign material such as metal oxides, zeolites or clays. The natural zeolite has low price, large resource reserve, large specific surface area and excellent ion exchange adsorption performance, and has wide application prospect in the field of wastewater treatment. Some natural zeolites and clays such as bentonite and clinoptilolite are inexpensive and widely used for water purification applications.
Zeolite can be considered as a zeolite made up of a certain amount of Al3+Substituted Si4+The porous aluminosilicate mineral with an aqueous structure is formed. Typically the zeolite is a silicon-oxygen tetrahedron and Al3+Substituted Si4+The aluminum tetrahedron structure formed later, i.e. with silicon atom or aluminum atom as tetrahedron center, surrounded by 4 oxygen atoms. Since the aluminum atom has a +3 valence, the valence electron of one oxygen atom in the alundum is not neutralized, so that it is in a-1 valence state. In order to keep the overall electrical property of the electrolyte neutral, a positive cation (usually Na) must be around the four sides+、K+、1/2Ca2+). These cations are relatively weakly bound to the aluminosilicate and therefore have a high mobility and are very susceptible to ion exchange with cations in the surrounding aqueous solution. This structure of the zeolite determines its large electrostatic attraction and strong ion exchange, and thus the removal of heavy metals by the zeolite may involve multiple effects. Jenne et al showed that: zeolite pairThe removal mechanism of heavy metal ions mainly comprises ion exchange and chemical adsorption. Wherein the ion exchange may comprise 2 forms: the metal ions exchange with protons in hydroxyl functional groups on the surface of the zeolite; metal ion and cation (Na) with stronger fluidity on zeolite surface+、K+、Ca2+Etc.) exchange occurs. The complexation reaction of heavy metal ions with hydroxyl groups on the surface of zeolite has chemisorption, which generally comprises surface complexation and internal complexation. Internal complexation is generally considered to be more stable and the binding between the zeolite and the heavy metal ions to be tighter than surface complexation. The sieving molecular nature of zeolites and the strong active sites present on its surface make them well suited for adsorbing different types of wastewater contaminants. Clinoptilolite is a natural mineral composed of aluminosilicates that can incorporate a variety of metal oxides and metal matrix cations commonly used to adsorb dyes and heavy metal ions from various waste waters.
Chitosan is a natural high molecular alkaline polysaccharide, has the characteristics of no toxicity, no irritation, no immune antigenicity and the like, has good biocompatibility and biodegradability, and is widely applied to the fields of food, medicine and the like. However, due to strong hydrogen bonding between molecules and in molecules, chitosan can only be dissolved in a few dilute acid solutions such as dilute acetic acid; meanwhile, the degradation speed of the material is slow, the material is difficult to match with the tissue regeneration speed, and tissue defects are easily caused, so that the application of the material is greatly limited. The hydroxyethyl group is properly introduced into the hydroxyl or amino position on the chitosan sugar ring, so that the hydrogen bond effect between or in the chitosan molecule is effectively weakened, the solubility of the chitosan is improved, and the subsequent modification capability of the chitosan is enhanced.
Since heavy metal adsorption type gels mainly depend on synthetic or semisynthetic polymers, there is not enough foundation and technical support for the development of all-natural material based gels, and thus, environmentally-friendly and selective adsorption gels have not been industrially utilized and developed on a large scale.
Disclosure of Invention
The invention aims to provide a preparation methodThe invention relates to a method for removing nano composite gel of bivalent cadmium in waste water, which can remove bivalent cadmium ions in the waste water with high efficiency and selectivity2+The method not only can improve the comprehensive utilization efficiency of natural polymers such as chitosan derivatives, clinoptilolite and the like, but also can be used for preparing Cd in heavy metal wastewater2+The efficient adsorption and removal provides a feasible scheme.
The technical scheme of the invention is as follows: adding deionized water into clinoptilolite powder, uniformly oscillating by ultrasonic waves to obtain clinoptilolite dispersion liquid, sequentially adding the clinoptilolite dispersion liquid, potassium persulfate (KPS for short) and N, N-methylene bisacrylamide (MBA for short) into hydroxyethyl chitosan solution, uniformly mixing, introducing nitrogen, then adding acrylamide (AAm for short), uniformly stirring, carrying out graft copolymerization at 45-80 ℃, cooling the generated reactant to room temperature, repeatedly washing with hot water and acetone, drying, and carrying out ball milling and crushing to obtain the nano composite gel.
The method for preparing the nano composite gel for removing the divalent cadmium in the wastewater comprises the following specific operations:
(1) weighing clinoptilolite powder, adding deionized water, and then carrying out ultrasonic oscillation to uniformly disperse the clinoptilolite powder in the deionized water to obtain clinoptilolite dispersion liquid, wherein the power of the ultrasonic oscillation is 500-2000W, the oscillation time is 0.5-5.0 h, and the concentration of the clinoptilolite dispersion liquid is 0.1-10 mg/mL;
(2) weighing hydroxyethyl chitosan solid, adding deionized water to prepare a hydroxyethyl chitosan solution, sequentially adding clinoptilolite dispersion liquid, potassium persulfate (KPS) and N, N-methylene bisacrylamide to the hydroxyethyl chitosan solution, stirring and mixing uniformly, introducing nitrogen, introducing the nitrogen for 10-30 min, adding acrylamide, and carrying out graft copolymerization at 45-80 ℃, wherein the concentration of the hydroxyethyl chitosan solution is 0.01-0.1 g/mL, the volume ratio of the clinoptilolite dispersion liquid to the hydroxyethyl chitosan solution is 1: 10-10: 1, the mass ratio of the potassium persulfate to the N, N-methylene bisacrylamide to the hydroxyethyl chitosan solution is 0.05-0.5, the mass ratio of the acrylamide to the hydroxyethyl chitosan solid is 0.03-0.1 and 0.5-5, and the graft copolymerization time is 1-10 h;
(3) and (3) cooling the reaction product obtained in the step (2) to room temperature, sequentially and repeatedly cleaning and drying the reaction product by using hot water and acetone, and then performing ball milling and crushing to obtain the nanoscale composite gel for removing the divalent cadmium in the wastewater, wherein the drying temperature is 35-55 ℃, trimethylbenzene is added as a solvent during ball milling and crushing, and the ball milling and crushing time is 24-120 hours.
The nano composite gel adsorbent prepared by the method is in a grey white powder shape.
The invention has the advantages and technical effects that:
(1) the invention takes hydroxyethyl chitosan and clinoptilolite as raw materials to prepare the selective adsorption Cd2+The ionic nano-blending composite gel can efficiently remove divalent cadmium ions in wastewater, and has no pollution to the environment and environmental protection;
(2) the method not only can improve the comprehensive utilization efficiency of natural polymers such as chitosan derivatives, clinoptilolite and the like, but also can improve the comprehensive utilization efficiency of Cd in heavy metal wastewater2+The efficient adsorption and removal provides a feasible scheme.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not limited to the examples.
Example 1: the method for preparing the nano composite gel for removing the divalent cadmium in the wastewater comprises the following specific operations:
(1) process for dispersing clinoptilolite
Weighing 0.1mg clinoptilolite powder, adding 1mL of deionized water, preparing 0.1mg/mL clinoptilolite dispersion, then putting the clinoptilolite dispersion into an ice water bath, and carrying out ultrasonic treatment for 0.5h under the power of 500W by using an ultrasonic generator to uniformly disperse clinoptilolite in the deionized water;
(2) implementation process of composite hydrogel
Dissolving 1g of hydroxyethyl chitosan in 100mL of deionized water to prepare a hydroxyethyl chitosan solution with the concentration of 0.01g/mL, sequentially adding clinoptilolite dispersion, 0.05g of potassium persulfate and 0.03g of N, N-methylene bisacrylamide into the hydroxyethyl chitosan solution, dissolving and uniformly mixing, introducing nitrogen, introducing the nitrogen for 10min, adding 0.5g of acrylamide, and carrying out graft copolymerization reaction at 45 ℃ for 1h, wherein the volume ratio of the clinoptilolite dispersion to the hydroxyethyl chitosan solution is 10:1, and the mass ratios of the potassium persulfate to the N, N-methylene bisacrylamide to the acrylamide to the hydroxyethyl chitosan solid are respectively 0.05, 0.03 and 0.5;
(3) process for preparing nano adsorption gel
And (3) cooling the reactant generated in the step (2) to 23 ℃, repeatedly washing the reactant for 3 times by using hot water and acetone in sequence, drying the reactant in a drying oven at 35 ℃, and grinding the dried product for 24 hours by using a ball mill by using trimethylbenzene as a solvent to obtain the clinoptilolite/hydroxyethyl chitosan grafted copolymer nano composite gel.
(4) Properties of nanocomposite gel
Placing the gel sample in Cr with the concentration of 1000mg/L2+Oscillating and adsorbing the sample in the solution for 24 hours, and measuring the adsorption capacity of the sample to be 9.98mg/g by using a plasma photoelectric direct-reading spectrometer.
(5) Desorption and recycling of hydrogels
The adsorption-desorption experiment was initially carried out for 5 cycles, with the metal ions adsorbed on the adsorbent and then desorbed in 50ml of 0.1mol/L HCl solution for 24 h. After desorption, the active sites of the adsorbent were regenerated using a 1mol/L NaOH solution and then used again for the next adsorption cycle. After 5 times of recycling, the adsorption capacity of the gel is 5.83 mg/g.
Example 2: the method for preparing the nano composite gel for removing the divalent cadmium in the wastewater comprises the following specific operations:
(1) process for dispersing clinoptilolite
Weighing 10mg clinoptilolite powder, adding 1mL of deionized water, preparing a clinoptilolite dispersion liquid with the concentration of 10mg/mL, then putting the clinoptilolite dispersion liquid into an ice-water bath, and carrying out ultrasonic treatment for 5 hours at the power of 2000W by using an ultrasonic wave generating device to uniformly disperse the clinoptilolite in the deionized water;
(2) implementation process of composite hydrogel
Dissolving 1g of hydroxyethyl chitosan in 10mL of deionized water to prepare a 0.1g/mL hydroxyethyl chitosan solution, sequentially adding clinoptilolite dispersion, 0.5g of potassium persulfate and 0.1g of N, N-methylene bisacrylamide to the hydroxyethyl chitosan solution, dissolving and uniformly mixing, introducing nitrogen for 30min, adding 5g of acrylamide, and carrying out graft copolymerization at 60 ℃ for 10h, wherein the volume ratio of the clinoptilolite dispersion to the hydroxyethyl chitosan solution is 5:1, and the mass ratios of the potassium persulfate to the N, N-methylene bisacrylamide to the acrylamide to the hydroxyethyl chitosan solid are 0.5, 0.1 and 5 respectively;
(3) process for preparing nano adsorption gel
And (3) cooling the reactant generated in the step (2) to 25 ℃, repeatedly washing the reactant for 6 times by using hot water and acetone in sequence, drying the reactant in an oven at 55 ℃, and crushing and grinding the dried product for 120 hours by using a ball mill by using trimethylbenzene as a solvent to obtain the clinoptilolite/hydroxyethyl chitosan grafted copolymer nano composite gel.
(4) Properties of nanocomposite gel
Placing the gel sample in Cr with the concentration of 1000mg/L2+Oscillating and adsorbing the sample in the solution for 24 hours, and measuring the adsorption capacity of the sample to be 27.38mg/g by using a plasma photoelectric direct-reading spectrometer.
(5) Desorption and recycling of hydrogels
The adsorption-desorption experiment was initially performed for 5 cycles; the metal ions were adsorbed on the adsorbent and then desorbed in 50ml of 0.1mol/L HCl solution for 24 h. After desorption, the active sites of the adsorbent were regenerated using a 1mol/L NaOH solution and then used again for the next adsorption cycle. After 5 times of recycling, the adsorption capacity of the gel is 20.36 mg/g.
Example 3: the method for preparing the nano composite gel for removing the divalent cadmium in the wastewater comprises the following specific operations:
(1) process for dispersing clinoptilolite
Weighing 5mg clinoptilolite powder, adding 1mL of deionized water, preparing clinoptilolite dispersion liquid with the concentration of 5mg/mL, then putting the clinoptilolite dispersion liquid into ice-water bath, and carrying out ultrasonic treatment for 2.5h at the power of 1500W by using an ultrasonic wave generating device to uniformly disperse clinoptilolite in the deionized water;
(2) implementation process of composite hydrogel
Dissolving 1g of hydroxyethyl chitosan in 20mL of deionized water to prepare a hydroxyethyl chitosan solution with the concentration of 0.05g/mL, sequentially adding 1mL of clinoptilolite dispersion, 0.25g of potassium persulfate and 0.05g of N, N-methylene bisacrylamide to the hydroxyethyl chitosan solution, dissolving and uniformly mixing, introducing nitrogen, introducing the nitrogen for 15min, adding 2.5g of acrylamide, and carrying out graft copolymerization reaction at 80 ℃ for 5h, wherein the volume ratio of the clinoptilolite dispersion to the hydroxyethyl chitosan solution is 1:10, and the mass ratios of the potassium persulfate, the N, N-methylene bisacrylamide and the acrylamide to the hydroxyethyl chitosan solid are respectively 0.25, 0.05 and 2.5;
(3) process for preparing nano adsorption gel
And (3) cooling the reactant generated in the step (2) to 24 ℃, washing the reactant for 5 times by using hot water and acetone in sequence, drying the reactant in a drying oven at the temperature of 45 ℃, and grinding the dried product for 60 hours by using a ball mill by using trimethylbenzene as a solvent to obtain the clinoptilolite/hydroxyethyl chitosan grafted copolymer nano composite gel.
(4) Properties of nanocomposite gel
Placing the gel sample in Cr with the concentration of 1000mg/L2+Oscillating and adsorbing the sample in the solution for 24 hours, and measuring the adsorption capacity of the sample to be 21.57mg/g by using a plasma photoelectric direct-reading spectrometer.
(5) Desorption and recycling of hydrogels
The adsorption-desorption experiment was initially carried out for 5 cycles, and the metal ions were adsorbed on the adsorbent and then desorbed in 50ml of 0.1mol/L HCl solution for 24 hours. After desorption, the active sites of the adsorbent were regenerated using a 1mol/L NaOH solution and then used again for the next adsorption cycle. After 5 times of recycling, the adsorption capacity of the gel is 16.19 mg/g.
Claims (7)
1. A method for preparing nano composite gel for removing bivalent cadmium in wastewater is characterized by comprising the following steps:
(1) weighing clinoptilolite powder, adding deionized water, and then performing ultrasonic oscillation to uniformly disperse the clinoptilolite powder in the deionized water to obtain clinoptilolite dispersion liquid;
(2) weighing hydroxyethyl chitosan solid, adding deionized water to prepare a hydroxyethyl chitosan solution, then sequentially adding clinoptilolite dispersion liquid, potassium persulfate and N, N-methylene bisacrylamide into the hydroxyethyl chitosan solution, uniformly stirring and mixing, introducing nitrogen, introducing the nitrogen for 10-30 min, adding acrylamide, and carrying out graft copolymerization at 45-80 ℃, wherein the concentration of the hydroxyethyl chitosan solution is 0.01-0.1 g/mL, the volume ratio of the clinoptilolite dispersion liquid to the hydroxyethyl chitosan solution is 1: 10-10: 1, and the mass ratios of the potassium persulfate, the N, N-methylene bisacrylamide and the acrylamide to the hydroxyethyl chitosan solid are 0.05-0.5, 0.03-0.1 and 0.5-5 respectively;
(3) and (3) cooling the reaction product obtained in the step (2) to room temperature, sequentially washing and drying the reaction product by using hot water and acetone, then carrying out ball milling and crushing, and adding trimethylbenzene as a solvent during ball milling and crushing to obtain the nano-scale composite gel for removing the divalent cadmium in the wastewater.
2. The method for preparing a nanocomposite gel for removing divalent cadmium from wastewater according to claim 1, wherein: the concentration of the clinoptilolite dispersion liquid in the step (1) is 0.1-10 mg/mL.
3. The method for preparing a nanocomposite gel for removing divalent cadmium from wastewater according to claim 1, wherein: the power of ultrasonic oscillation in the step (1) is 500-2000W, and the oscillation time is 0.5-5.0 h.
4. The method for preparing a nanocomposite gel for removing divalent cadmium from wastewater according to claim 1, wherein: the graft copolymerization reaction time in the step (2) is 1-10 h.
5. The method for preparing a nanocomposite gel for removing divalent cadmium from wastewater according to claim 1, wherein: in the step (3), the drying temperature is 35-55 ℃.
6. The method for preparing a nanocomposite gel for removing divalent cadmium from wastewater according to claim 1, wherein: and (4) ball milling and crushing time in the step (3) is 24-120 h.
7. The method for preparing a nanocomposite gel for removing divalent cadmium from wastewater according to claim 1, wherein: the number of cleaning in the step (3) is 3-6.
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