CN112844062A - Preparation method of graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material - Google Patents
Preparation method of graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material Download PDFInfo
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- CN112844062A CN112844062A CN202011554874.3A CN202011554874A CN112844062A CN 112844062 A CN112844062 A CN 112844062A CN 202011554874 A CN202011554874 A CN 202011554874A CN 112844062 A CN112844062 A CN 112844062A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/08—Thickening liquid suspensions by filtration
- B01D17/085—Thickening liquid suspensions by filtration with membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2323/08—Specific temperatures applied
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2323/00—Details relating to membrane preparation
- B01D2323/10—Specific pressure applied
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/12—Specific ratios of components used
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention relates to the field of inorganic materials, in particular to a preparation method of a graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material, which comprises the following steps: preparing cerium and yttrium modified zinc oxide; the preparation method comprises the steps of modifying cerium and yttrium modified zinc oxide with graphene to obtain graphene-rare earth doped zinc oxide, and mixing the graphene modified cerium and yttrium modified zinc oxide to obtain graphene-rare earth doped zinc oxide and a ceramic substrate to be pressed into a film. The invention widens the application field of the graphene-cerium and yttrium codoped zinc oxide ceramic microfiltration membrane nanocomposite, and the graphene-cerium and yttrium codoped zinc oxide ceramic microfiltration membrane is assembled by a simple and easy method; and (3) a method of photodegradation. Solves the technical problem of secondary pollution of the ceramic microfiltration membrane. The composite material has wide application value in the fields of oil field water treatment, sewage treatment, oil-water separation and the like.
Description
Technical Field
The invention relates to the field of inorganic materials, in particular to a preparation method of a graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material.
Technical Field
The rapid development of modern industry generates increasingly serious water pollution problems. Among various pollutants in water, the water environment destruction caused by petroleum and other organic matters is particularly serious, and huge economic loss is caused. Therefore, the oily wastewater is timely and efficiently treated so as to be recycled. At present, the main methods for treating oily wastewater at home and abroad comprise: biodegradation, chemical treatment, physical treatment, and the like.
The membrane materials for oil-water separation can be mainly divided into organic membranes and ceramic membranes. In the process of oil-water separation, the organic membrane is easily affected by swelling and is reduced, and once organic pollutants are adsorbed, the performance of the membrane material is easily damaged, so that the application range of the organic membrane has certain limitation; compared with organic membranes, ceramic membranes have the outstanding advantages of high strength, high temperature resistance, good chemical stability and the like, can be used for long-term stable separation operation under severe conditions, are widely applied to the fields of metallurgy, chemical engineering, medicine, food processing and the like, and the material characteristics of the ceramic membranes are favorable for inhibiting the adsorption of organic pollutants on the surfaces of the membranes. Therefore, the advantages are obvious in the oil-water separation process.
Certainly, in the filtering process of the ceramic microfiltration membrane, organic pollutants are bred and adhered on the surface and in the pore channel of the membrane to cause secondary pollution, and the use effect and the service life of the ceramic membrane are seriously influenced.
Disclosure of Invention
The invention aims to solve the problem that secondary pollution is easily caused in the process of a ceramic microfiltration membrane in the prior art, and provides a preparation method of a graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material comprises the following steps:
s1, adding cerium acetate into ethylene glycol to obtain an ethylene glycol solution of cerium acetate with the concentration of 0.03-0.6 mol/L, and marking as a solution A;
s2, dissolving zinc acetate and ethanolamine in equal molar amounts in ethylene glycol to obtain a zinc acetate ethylene glycol solution, wherein the concentration of the zinc acetate is 0.25-5 mol/L;
s3, adding yttrium acetate in the step S2, and marking the obtained mixed solution as a solution B, wherein the concentration of yttrium acetate is 0.007-0.14 mol/L;
s4, dropwise adding the solution A obtained in the step S1 into the solution B obtained in the step S3 according to the volume ratio of 1 (5-20), and stirring the obtained mixed solution at 50-70 ℃ for 1-2 hours;
s5, after the reaction in the step S4 is finished, adding graphene into the mixed solution obtained in the step S4, stirring at the temperature of 50-70 ℃ for 1-2 hours, and then drying at the temperature of 70-100 ℃ for 10-60 min;
s6, transferring the product dried in the step S5 to a muffle furnace, heating to 400-600 ℃ under the protection of inert gas, preserving heat for 1-2 h, cooling to room temperature to obtain a graphene-cerium and yttrium co-doped zinc oxide nano material, then performing dry pressing forming under 16-25 MPa, and then drying, sintering, grinding and forming a film;
s7, mixing the graphene-cerium and yttrium co-doped zinc oxide nano material obtained in the step S6 with a ceramic microfiltration membrane substrate, and pressing to form a film;
s8, heating the film pressed in the step S7 to 500 ℃ at a heating rate of 1-3 ℃/min in an inert atmosphere; and then heating to 500-1400 ℃ at the heating rate of 5-8 ℃/min, preserving the heat for 1-2 h, and then cooling to raise the temperature.
Preferably, in the step S5, the mass ratio of the added graphene to the zinc oxide is (1-8): 90-99.
Preferably, in the step S1, cerium acetate is dissolved in ethylene glycol and stirred for 1-2 hours at 60-80 ℃ to obtain a solution A.
Preferably, in the step S2, zinc acetate and ethanolamine are dissolved in ethylene glycol and stirred for 1-2 hours at 50-70 ℃.
Preferably, in the step S3, after the yttrium acetate is added in the step S22, the mixture is stirred for 1 to 2 hours at 50 to 70 ℃ and then is kept still for 6 to 12 hours.
Preferably, in the step S6, the product dried in the step S5 is transferred to a muffle furnace, heated to 200 ℃ at a heating rate of 5-10 ℃/min, heated to 500-600 ℃ at a heating rate of 1-3 ℃/min, and then kept at the temperature for 1-2 h.
Preferably, in the step S7, a ball milling blending is adopted to mix the graphene-cerium and yttrium co-doped zinc oxide nano material with the ceramic microfiltration membrane substrate, wet ball milling is carried out at a rotation speed of 100-250 r/min for 1-2 hours, and then drying is carried out at 80-100 ℃ for 1-3 hours; the mass ratio of the graphene-cerium-yttrium codoped zinc oxide nano material to the ceramic microfiltration membrane substrate is as follows: (0.01-2) and (98-99.9).
Compared with the prior art, the invention has the following technical effects:
the invention discloses a preparation method of a graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material. The zinc oxide introduces electron holes through cerium and yttrium modification to improve the photoelectric efficiency of the zinc oxide. In order to further improve and widen the application field of the graphene-cerium and yttrium codoped zinc oxide ceramic microfiltration membrane nanocomposite, the graphene-cerium and yttrium codoped zinc oxide ceramic microfiltration membrane is assembled by a simple and easy method; and (3) a method of photodegradation. Solves the technical problem of secondary pollution of the ceramic microfiltration membrane. The composite material has wide application value in the fields of oil field water treatment, sewage treatment, oil-water separation and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below with reference to specific examples and comparative examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Unless otherwise specified, the devices used in this example are all conventional experimental devices, the materials and reagents used are commercially available, and the experimental methods without specific descriptions are also conventional experimental methods.
Example 1
A graphene-cerium and yttrium co-doped zinc oxide ceramic microfiltration membrane composite material comprises:
(1) preparing cerium and yttrium codoped zinc oxide: in the experiment, 9.3 g of zinc acetate is dissolved in 50 ml of ethylene glycol and a stabilizer ethanolamine solution which is equimolar with the zinc acetate, the mixture is heated and stirred at 70 ℃ for 1 hour to form a uniform transparent solution, 0.5 g of yttrium acetate is added, the mixture is continuously and fully stirred for 2 hours and stands for 12 hours for standby application, 0.2 g of cerium acetate is dissolved in 10 ml of ethylene glycol, the mixture is heated and stirred at 80 ℃ for 1 hour to prepare a solution A, a required certain amount of solution A is dropwise added into the solution B, the solution A is stirred at 70 ℃ for 1 hour to obtain a cerium-yttrium-codoped zinc oxide solution, the cerium-yttrium-codoped zinc oxide solution is dried in a 100 ℃ drying oven for 10-60 minutes and then is placed in a muffle furnace to be slowly heated to 400-600 ℃ and is kept for 2 hours, and then the solution is naturally cooled to room temperature to obtain cerium-yttrium-codoped zinc oxide.
(2) Preparing a cerium and yttrium co-doped zinc oxide/graphene nano material: and grinding the cerium and yttrium codoped zinc oxide powder and the graphene for half an hour, then placing the ground material into a muffle furnace, slowly heating the ground material to 400-600 ℃, keeping the temperature for 2 hours, and naturally cooling the ground material to obtain the graphene-cerium and yttrium codoped zinc oxide nano material.
(3) Preparing a graphene-cerium-yttrium co-doped zinc oxide nano ceramic microfiltration membrane composite material: ball-milling and blending the graphene-cerium and yttrium co-doped zinc oxide and the ceramic microfiltration membrane substrate, carrying out wet ball milling for 1-2 h at the rotating speed of 100-250 r/min, and then drying for 1-3 h at the temperature of 80-100 ℃; the mass ratio of the graphene-cerium-yttrium codoped zinc oxide nano material to the ceramic microfiltration membrane substrate is as follows: 0.01-2: 98-99.9; putting the prepared graphene-cerium and yttrium codoped zinc oxide ceramic microfiltration membrane substrate into a muffle furnace, introducing nitrogen for 30 minutes, slowly heating to 400-600 ℃, keeping the temperature for 1-2 hours, naturally cooling to room temperature to obtain the graphene-cerium and yttrium codoped zinc oxide ceramic microfiltration membrane substrate, performing dry pressing forming under 16-25 MPa, and then drying, sintering and lapping; the temperature of the pressed film sample is raised to 500 ℃ at the rate of 1-3 ℃/min under the nitrogen atmosphere; and (3) heating at 500-1400 ℃ at a heating rate of 5-8 ℃/min, preserving heat for 1-2 h, and naturally cooling to room temperature.
Comparative example 1
In comparison to example 1, this comparative example uses only cerium doped zinc oxide, with no yttrium added.
Comparative example 2
Compared with example 1, this comparative example uses yttrium-doped zinc oxide only, without the addition of cerium.
Comparative example 3
In contrast to example 1, no graphene was added in this comparative example.
Experimental example 1
And observing the SEM (figure 1) and TEM (figure 2) morphology of the prepared graphene-cerium and yttrium co-doped zinc oxide. It can be seen that the cerium and yttrium co-doped zinc oxide is uniformly distributed on the surface of the graphene.
Experimental example 2
The microfiltration membranes obtained in the examples and comparative examples were used to filter water from the same source. The content of E.coli in the water after filtration was measured before and after 1 month, and the filtration effect of the filter membrane was judged from the E.coli content, and the results are shown in the following table.
As can be seen from the above table, the filtration levels of the various groups of membranes were comparable one month before. After 1 month of sun exposure, the control group showed a higher degree of reduction in the E.coli filtration effect than the example group. The experiment shows that the graphene/rare earth doped zinc oxide has strong photocatalytic degradation sterilization effect in the filter membrane, so that secondary pollution can not be generated, and the residual organic matter in the comparative example degrades to generate secondary pollution on the filter membrane.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. A preparation method of a graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material is characterized by comprising the following steps:
s1, adding cerium acetate into ethylene glycol to obtain an ethylene glycol solution of cerium acetate with the concentration of 0.03-0.6 mol/L, and marking as a solution A;
s2, dissolving zinc acetate and ethanolamine in equal molar amounts in ethylene glycol to obtain a zinc acetate ethylene glycol solution, wherein the concentration of the zinc acetate is 0.25-5 mol/L;
s3, adding yttrium acetate in the step S2, and marking the obtained mixed solution as a solution B, wherein the concentration of yttrium acetate is 0.007-0.14 mol/L;
s4, dropwise adding the solution A obtained in the step S1 into the solution B obtained in the step S3 according to the volume ratio of 1 (5-20), and stirring the obtained mixed solution at 50-70 ℃ for 1-2 hours;
s5, after the reaction in the step S4 is finished, adding graphene into the mixed solution obtained in the step S4, stirring at the temperature of 50-70 ℃ for 1-2 hours, and then drying at the temperature of 70-100 ℃ for 10-60 min;
s6, transferring the product dried in the step S5 to a muffle furnace, heating to 400-600 ℃ under the protection of inert gas, preserving heat for 1-2 h, cooling to room temperature to obtain a graphene-cerium and yttrium co-doped zinc oxide nano material, then performing dry pressing forming under 16-25 MPa, and then drying, sintering, grinding and forming a film;
s7, mixing the graphene-cerium and yttrium co-doped zinc oxide nano material obtained in the step S6 with a ceramic microfiltration membrane substrate, and pressing to form a film;
s8, heating the film pressed in the step S7 to 500 ℃ at a heating rate of 1-3 ℃/min in an inert atmosphere; and then heating to 500-1400 ℃ at the heating rate of 5-8 ℃/min, preserving the heat for 1-2 h, and then cooling to raise the temperature.
2. The preparation method of the graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material as claimed in claim 1, wherein in the step S5, the mass ratio of the added graphene to the added zinc oxide is (1-8) to (90-99).
3. The preparation method of the graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material as claimed in claim 1, wherein in the step S1, cerium acetate is dissolved in ethylene glycol and stirred for 1-2 h at 60-80 ℃ to obtain a solution A.
4. The preparation method of the graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material according to claim 1, wherein in the step S2, zinc acetate and ethanolamine are dissolved in ethylene glycol and stirred for 1-2 h at 50-70 ℃.
5. The preparation method of the graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material as claimed in claim 1, wherein in the step S3, after yttrium acetate is added in the step S22, the mixture is stirred at 50-70 ℃ for 1-2 hours and then is kept still for 6-12 hours.
6. The preparation method of the graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material according to claim 1, wherein in the step S6, the dried product obtained in the step S5 is transferred to a muffle furnace, heated to 200 ℃ at a heating rate of 5-10 ℃/min, heated to 500-600 ℃ at a heating rate of 1-3 ℃/min, and then kept warm for 1-2 hours.
7. The preparation method of the graphene-rare earth doped zinc oxide nano ceramic microfiltration membrane composite material according to claim 1, wherein in the step S7, the graphene-cerium and yttrium co-doped zinc oxide nano material and the ceramic microfiltration membrane substrate are mixed by ball milling and blending, and are subjected to wet ball milling for 1-2 hours at a rotation speed of 100-250 r/min, and then are dried for 1-3 hours at a temperature of 80-100 ℃; the mass ratio of the graphene-cerium-yttrium codoped zinc oxide nano material to the ceramic microfiltration membrane substrate is as follows: (0.01-2) and (98-99.9).
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