CN107913677B - Nano heavy metal wastewater ion adsorption microspheres and preparation method thereof - Google Patents
Nano heavy metal wastewater ion adsorption microspheres and preparation method thereof Download PDFInfo
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- 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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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a preparation method of nano heavy metal wastewater ion adsorption microspheres, which comprises the following steps: 1) preparing porous graphene microspheres, 2) modifying the surfaces of the porous graphene microspheres, and 3) carrying out ion exchange; the invention also discloses the nano heavy metal ion adsorption microspheres prepared by the preparation method; according to the nano heavy metal ion adsorption microsphere disclosed by the invention, triazine compounds are modified on the surface of the porous graphene microsphere, and are fixedly connected with hematoporphyrin through ionic bonds, and the adsorption microsphere has good heavy metal ion adsorption effect, low cost, large adsorption capacity and easiness in desorption due to more amino groups and carboxyl groups on the surface.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a nano heavy metal wastewater ion adsorption microsphere and a preparation method thereof.
Background
With the rapid development of modern industry, a large amount of wastewater rich in heavy metal ions comes from the wastewater, the heavy metal ions cannot be degraded by self, water and soil pollution is easily caused, the heavy metal ions are enriched in organisms through food chains, great threat is formed to the living environment, ecology and health of human beings, and economic development and social progress are restricted. The effective control and treatment of the wastewater containing heavy metal ions and the high-efficiency recycling of valuable metals are the problems facing and urgently waiting to be solved in the current environmental protection field.
The adsorption method is a method for treating heavy metal ions, which is most applied, simplest in operation and most ideal in treatment effect at present, and is a method for removing the heavy metal ions by adhering the heavy metal ions to the surfaces of active sites of an adsorbent by a physical or chemical method.
Therefore, it is imperative to develop a novel adsorption material which has good adsorption effect on heavy metal ions, low cost, large adsorption capacity and easy desorption.
Disclosure of Invention
The invention aims to solve the problems and provides a nano heavy metal wastewater ion adsorption microsphere and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solution, a method for preparing nano heavy metal wastewater ion adsorption microspheres, comprising the steps of:
1) preparing porous graphene microspheres: uniformly mixing graphene oxide and deionized water, performing ultrasonic dispersion for 15-20 minutes, adding a pore-forming agent to uniformly disperse the pore-forming agent in the graphene oxide, then adding glucose, uniformly mixing, performing electrostatic spraying, collecting by a wet method, adding the mixture into an organic solvent, soaking for 5-6 hours, and treating for 6-10 hours by using a near point drying method under a humid condition to obtain porous nano graphene microspheres;
2) surface modification of porous graphene microspheres: dispersing the porous graphene microspheres prepared in the step 1) in ethanol, adding 1,3, 5-tris [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring for 3-5 hours at 40-50 ℃, then adding halogenated alkane, stirring for 4-6 hours at a constant temperature, then centrifuging, sequentially washing for 3-5 times by using ethyl acetate and diethyl ether, and then drying in a vacuum drying oven at 50-70 ℃ for 10-12 hours;
3) ion exchange: soaking the surface-modified porous graphene microspheres prepared in the step 2) in a hematoporphyrin aqueous solution with the mass fraction of 10-20% for 60-72 hours, carrying out ion exchange, filtering, washing with water for 3-5 times, and drying in a vacuum drying oven at 50-70 ℃ for 10-12 hours;
wherein the mass ratio of the graphene oxide, the deionized water, the pore-forming agent and the glucose in the step 1) is 1:10 (0.2-0.7) to 1;
the pore-forming agent is selected from one or more of polystyrene microspheres, polymethyl methacrylate microspheres and polybutyl acrylate microspheres;
the organic solvent is selected from one or more of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone;
the mass ratio of the porous graphene microspheres, the ethanol, the 1,3, 5-tris [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione and the halogenated alkane in the step 2) is (3-5): (10-15): 1: (1-2);
the halogenated alkane is selected from one or more of chloroethane, chloropropane, bromopropane and bromoethane;
a nanometer heavy metal wastewater ion adsorption microsphere is prepared by adopting the preparation method of the nanometer heavy metal ion adsorption microsphere.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) the preparation method of the nano heavy metal ion adsorption microspheres provided by the invention is simple and easy to implement, has low requirements on equipment, easily available raw materials and low price.
(2) According to the nano heavy metal ion adsorption microsphere provided by the invention, the porous graphene microsphere has higher adsorbability and desorption capacity to heavy metal ions due to the porous structure, and can be repeatedly utilized for a plurality of times.
(3) According to the nano heavy metal ion adsorption microsphere provided by the invention, triazine compounds are modified on the surface of the microsphere and fixedly connected with hematoporphyrin through ionic bonds, and the adsorption capacity of the adsorption microsphere on heavy metal ions is further enhanced by amino and carboxyl on the surface.
(4) The molecular chain of the nano heavy metal ion adsorption microsphere provided by the invention contains a conjugated structure, so that the nano heavy metal ion adsorption microsphere has visible light catalysis effect while maintaining high-efficiency adsorption, thereby effectively treating other organic pollutants in sewage.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the following provides a detailed description of the product of the present invention with reference to the examples.
Example 1
A preparation method of nano heavy metal wastewater ion adsorption microspheres comprises the following steps:
1) preparing porous graphene microspheres: uniformly mixing 100g of graphene oxide and 1000g of deionized water, performing ultrasonic dispersion for 15 minutes, adding 20g of polystyrene microspheres to uniformly disperse the polystyrene microspheres in the graphene oxide, then adding 100g of glucose, uniformly mixing, performing electrostatic spraying, collecting by a wet method, adding the polystyrene microspheres into dimethyl sulfoxide, soaking for 5 hours, and then treating for 6 hours by using a near point drying method under a humid condition to obtain porous nano-graphene microspheres;
2) surface modification of porous graphene microspheres: dispersing 90g of the porous graphene microspheres prepared in the step 1) in 300g of ethanol, adding 30g of 1,3, 5-tris [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring for 3 hours at 40 ℃, then adding 30g of chloroethane, stirring for 4 hours at the temperature, then centrifuging, sequentially washing for 3 times by using ethyl acetate and diethyl ether, and then drying for 10 hours at 50 ℃ in a vacuum drying oven;
3) ion exchange: soaking the surface-modified porous graphene microspheres prepared in the step 2) in a hematoporphyrin aqueous solution with the mass fraction of 10% for 60 hours, carrying out ion exchange, filtering, washing with water for 3 times, and drying in a vacuum drying oven at 50 ℃ for 10 hours;
a nanometer heavy metal wastewater ion adsorption microsphere is prepared by adopting the preparation method of the nanometer heavy metal ion adsorption microsphere.
Example 2
A preparation method of nano heavy metal wastewater ion adsorption microspheres comprises the following steps:
1) preparing porous graphene microspheres: uniformly mixing 100g of graphene oxide and 1000g of deionized water, performing ultrasonic dispersion for 17 minutes, adding 40g of polymethyl methacrylate microspheres to uniformly disperse the polymethyl methacrylate microspheres in the graphene oxide, then adding 100g of glucose, uniformly mixing, performing electrostatic spraying, collecting by a wet method, adding the polymethyl methacrylate microspheres into N, N-dimethylformamide to soak for 5.5 hours, and then treating for 7 hours by using a near point drying method under a humid condition to obtain porous nano graphene microspheres;
2) surface modification of porous graphene microspheres: dispersing 120g of the porous graphene microspheres prepared in the step 1) in 360g of ethanol, adding 30g of 1,3, 5-tris [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring for 4 hours at 45 ℃, then adding bromopropane, stirring for 5 hours at a constant temperature, then centrifuging, sequentially washing for 4 times by using ethyl acetate and diethyl ether, and then drying for 11 hours at 60 ℃ in a vacuum drying oven;
3) ion exchange: soaking the surface-modified porous graphene microspheres prepared in the step 2) in a hematoporphyrin aqueous solution with the mass fraction of 14% for 66 hours, carrying out ion exchange, filtering, washing with water for 5 times, and drying in a vacuum drying oven at 60 ℃ for 11 hours;
a nanometer heavy metal wastewater ion adsorption microsphere is prepared by adopting the preparation method of the nanometer heavy metal ion adsorption microsphere.
Example 3
A preparation method of nano heavy metal wastewater ion adsorption microspheres comprises the following steps:
1) preparing porous graphene microspheres: uniformly mixing 100g of graphene oxide and 1000g of deionized water, performing ultrasonic dispersion for 18 minutes, adding 60g of polybutyl acrylate microspheres to uniformly disperse the polybutyl acrylate microspheres in the graphene oxide, then adding 100g of glucose, uniformly mixing, performing electrostatic spraying, collecting by a wet method, adding the polybutyl acrylate microspheres into N-methylpyrrolidone, soaking for 5.8 hours, and then treating for 9 hours by using a near point drying method under a humid condition to obtain porous nano graphene microspheres;
2) surface modification of porous graphene microspheres: dispersing 140g of the porous graphene microspheres prepared in the step 1) in 400g of ethanol, adding 30g of 1,3, 5-tris [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring for 5 hours at 47 ℃, then adding 50g of bromoethane, stirring for 6 hours at a constant temperature, then centrifuging, sequentially washing for 5 times by using ethyl acetate and diethyl ether, and then drying for 12 hours at 70 ℃ in a vacuum drying oven;
3) ion exchange: soaking the surface-modified porous graphene microspheres prepared in the step 2) in a hematoporphyrin aqueous solution with the mass fraction of 18% for 68 hours, carrying out ion exchange, filtering, washing with water for 5 times, and drying in a vacuum drying oven at 64 ℃ for 12 hours;
a nanometer heavy metal wastewater ion adsorption microsphere is prepared by adopting the preparation method of the nanometer heavy metal ion adsorption microsphere.
Example 4
A preparation method of nano heavy metal wastewater ion adsorption microspheres comprises the following steps:
1) preparing porous graphene microspheres: uniformly mixing 100g of graphene oxide and 1000g of deionized water, performing ultrasonic dispersion for 20 minutes, adding 70g of polystyrene microspheres to uniformly disperse the polystyrene microspheres in the graphene oxide, then adding 100g of glucose, uniformly mixing, performing electrostatic spraying, collecting by a wet method, adding the polystyrene microspheres into dimethyl sulfoxide, soaking for 6 hours, and then treating for 10 hours by using a near point drying method under a humid condition to obtain porous nano-graphene microspheres;
2) surface modification of porous graphene microspheres: dispersing 150g of the porous graphene microspheres prepared in the step 1) in 450g of ethanol, adding 30g of 1,3, 5-tris [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring for 5 hours at 50 ℃, then adding 60g of chloropropane, stirring for 6 hours at the temperature of heat preservation, then centrifuging, sequentially washing for 5 times by using ethyl acetate and diethyl ether, and then drying for 12 hours at 70 ℃ in a vacuum drying oven;
3) ion exchange: soaking the surface-modified porous graphene microspheres prepared in the step 2) in a hematoporphyrin aqueous solution with the mass fraction of 20% for 72 hours, carrying out ion exchange, filtering, washing with water for 5 times, and drying in a vacuum drying oven at 70 ℃ for 12 hours;
a nanometer heavy metal wastewater ion adsorption microsphere is prepared by adopting the preparation method of the nanometer heavy metal ion adsorption microsphere.
Comparative example 1
Commercially available activated carbon granules;
the heavy metals prepared by the embodiment of the invention are as follows: the examples and comparative examples of the present invention were carried out by measuring the adsorption capacity of heavy metal ions by the following method: placing a certain mass of adsorption material in a conical flask with a plug, respectively adding a certain volume of heavy metal ion solution, vibrating in a constant-temperature oscillator at a constant temperature of 25 ℃ for a certain time, and calculating adsorption capacity according to the change of the concentration of heavy metal ions in the feed liquid; the concentration of heavy metal ions is measured by using a UV2450 type ultraviolet-visible spectrophotometer and calculated according to the adsorption capacity formula (1):
qeq-adsorption capacity of heavy metal ions, mg/g; cO-initial concentration of feed solution, mg/mL;
Ct-concentration of feed liquid at time t, mg/mL; vfVolume of feed liquid, mL; w-weight of adsorbent, g.
In this example, the desorption rate was measured by the following method: washing the adsorption material after adsorption balance with distilled water until no metal ions exist in the filtrate, then mixing with a certain volume of 2% sulfuric acid solution, oscillating for a certain time at constant temperature in a constant temperature oscillator, measuring the concentration of heavy metal ions in the solution, and calculating the desorption rate according to the formula (2):
wherein η represents the desorption rate, and C represents the concentration of metal ions in the eluate (mg. L)-1) V is the volume of the eluent (L), Q is the adsorption capacity of the membrane adsorbent before elution (mg. g)-1) And m is the mass (g) of the adsorbent.
This example selects Pb2+、Cu2+、Cd3+The adsorption capacity and desorption rate were determined and the test results are shown in table 1.
As can be seen from table 1, compared with the conventional commercially available activated carbon particles, the nano heavy metal ion adsorption beads prepared in this example have high adsorption and desorption capabilities for heavy metal ions.
TABLE 1 test results of adsorption and desorption properties of samples of inventive examples and comparative examples
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those of ordinary skill in the art can readily implement the present invention as described herein; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (7)
1. A preparation method of nanometer heavy metal wastewater ion adsorption microspheres is characterized by comprising the following steps:
1) preparing porous graphene microspheres: uniformly mixing graphene oxide and deionized water, performing ultrasonic dispersion for 15-20 minutes, adding a pore-forming agent to uniformly disperse the pore-forming agent in the graphene oxide, then adding glucose, uniformly mixing, performing electrostatic spraying, collecting by a wet method, adding the mixture into an organic solvent, soaking for 5-6 hours, and treating for 6-10 hours by using a near point drying method under a humid condition to obtain porous nano graphene microspheres;
2) surface modification of porous graphene microspheres: dispersing the porous graphene microspheres prepared in the step 1) in ethanol, adding 1,3, 5-tris [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring for 3-5 hours at 40-50 ℃, then adding halogenated alkane, stirring for 4-6 hours at a constant temperature, then centrifuging, sequentially washing for 3-5 times by using ethyl acetate and diethyl ether, and then drying in a vacuum drying oven at 50-70 ℃ for 10-12 hours;
3) ion exchange: soaking the surface-modified porous graphene microspheres prepared in the step 2) in a hematoporphyrin aqueous solution with the mass fraction of 10-20% for 60-72 hours, carrying out ion exchange, filtering, washing with water for 3-5 times, and drying in a vacuum drying oven at 50-70 ℃ for 10-12 hours.
2. The preparation method of the nano heavy metal wastewater ion adsorption microspheres according to claim 1, wherein the mass ratio of the graphene oxide, the deionized water, the pore-forming agent and the glucose in the step 1) is 1:10 (0.2-0.7) to 1.
3. The preparation method of the nano heavy metal wastewater ion adsorption microsphere of claim 1, wherein the pore-forming agent is selected from one or more of polystyrene microsphere, polymethyl methacrylate microsphere and polybutyl acrylate microsphere.
4. The preparation method of the nano heavy metal wastewater ion adsorption microspheres according to claim 1, wherein the organic solvent is one or more selected from dimethylsulfoxide, N-dimethylformamide and N-methylpyrrolidone.
5. The method for preparing nano heavy metal wastewater ion adsorption microspheres according to claim 1, wherein the mass ratio of the porous graphene microspheres, ethanol, 1,3, 5-tris [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, and halogenated alkane in step 2) is (3-5): (10-15): 1: (1-2).
6. The preparation method of the nano heavy metal wastewater ion adsorption microspheres according to claim 1, wherein the halogenated alkane is one or more selected from chloroethane, chloropropane, bromopropane and bromoethane.
7. A nano heavy metal wastewater ion adsorption microsphere which is characterized by being prepared by the preparation method of the nano heavy metal ion adsorption microsphere of any one of claims 1 to 6.
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| CN113171761B (en) * | 2021-04-26 | 2022-11-22 | 福建省环境保护设计院有限公司 | Porous electrostatic spraying microsphere for treating antimony-containing wastewater and preparation method thereof |
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