CN111036082B - Graphene oxide/TiO2Method for preparing composite membrane - Google Patents

Graphene oxide/TiO2Method for preparing composite membrane Download PDF

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CN111036082B
CN111036082B CN202010027468.5A CN202010027468A CN111036082B CN 111036082 B CN111036082 B CN 111036082B CN 202010027468 A CN202010027468 A CN 202010027468A CN 111036082 B CN111036082 B CN 111036082B
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graphene oxide
tio
membrane
preparation
mxene quantum
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CN111036082A (en
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黄瑞芳
陈德志
曾珍
吕文彦
胡笑笑
杨欣楼
叶雯茜
曾繁瑞
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Nanchang Hangkong University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/021—Carbon
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/024—Oxides
    • 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
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
    • 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 relates to graphene oxide/TiO2The preparation method of the composite membrane comprises the steps of oxidizing GO solution and Ti3C2Mixing MXene quantum dot solution in proportion to obtain mixed solution, ultrasonically pouring into a filter flask with a microfiltration membrane under the condition of continuously introducing air, and oxidizing MXene quantum dots to obtain TiO by a vacuum filtration method2Loading the graphene oxide and the graphene oxide on the surface of the microfiltration membrane in a composite manner to obtain the graphene oxide/TiO2A composite membrane. The graphene oxide/TiO of the invention2The pure water flux of the composite membrane is far greater than that of a pure graphene oxide membrane, and the pure water flux is along with Ti3C2The MXene quantum dot solution is increased in proportion, and the flux presentation is increased; meanwhile, the retention rate of heavy metal is also obviously improved. The preparation method is simple, easy to operate, easy for large-scale production and use and beneficial to popularization.

Description

Graphene oxide/TiO2Method for preparing composite membrane
Technical Field
The invention relates to graphene oxide/TiO2A preparation method of a composite membrane belongs to the technical field of composite membrane materials.
Background
The membrane separation technology utilizes the selective permeability of the membrane to each substance component in the mixed fluid to realize the separation, purification and concentration of each substance component. Due to the advantages of high separation efficiency, energy conservation, environmental protection, simple operation and the like, the method becomes one of common support technologies for solving the important problems of global energy, environment, water resources and the like. The single separation membrane can cause membrane pollution in the separation process due to the inherent properties (general hydrophilicity and the like), so that the problems of reduced membrane separation performance, increased energy consumption, short service life and the like are caused. Therefore, the development of composite membranes with excellent performance is the focus of research in the field of membrane separation materials at present. The composite membrane is composed of a base membrane and a skin layer which are supported by mechanics, and common base membrane materials comprise polysulfone, polyethersulfone, cellulose acetate, polyvinylidene fluoride and the like. The performance of the composite membrane can be improved by optimizing the materials and the structure of the surface layer, common surface layer materials comprise carbon nanotubes, silicon dioxide and the like, the composite membrane has the characteristics of high metal ion interception efficiency, strong antibacterial property, functional modification of a base membrane and the like, but the composite membrane also has the defects of poor dispersibility and stability and the like. The graphene oxide is used as a two-dimensional nano carbon material with a large specific surface area, is rich in oxygen-containing functional groups such as hydroxyl and carboxyl, has the advantages of strong hydrophilicity, easiness in dispersion, strong pollution resistance, easiness in functional design and the like, and is an ideal epidermis layer material. However, since the retention rate and the membrane flux of the pure graphene oxide are difficult to meet the requirements of practical application, it is necessary to introduce other nano materials to perform functional design on the graphene oxide, and change the interlayer distance and the pore diameter, thereby improving the retention rate and the membrane flux of the graphene oxide composite membrane.
Nano TiO 22The graphene oxide film is widely used for modifying the graphene oxide film due to the characteristics of no toxicity, no harm, abundant hydroxyl on the surface, good thermal stability and the like. Compared with a pure graphene oxide film, the prepared graphene oxide/TiO2The composite membrane has higher retention rate and membrane flux to water pollutants, however, due to the problem of easy agglomeration of nano materials and nano TiO2Surface with negative charge, nano TiO2The flaky graphene oxide with the same negative charge on the surface is difficult to uniformly disperse, so that the prepared graphene oxide/TiO is greatly reduced2The retention rate of the composite membrane to water pollutants. Therefore, to ensure nano TiO2The uniform dispersion on the surface of the flaky graphene oxide requires the nano TiO2The surface is modified necessarily, the modification process not only increases the preparation process of the composite membrane, but also changes the nano TiO2Greatly reduces the original physicochemical property of the surface of the nano TiO2The surface has the adsorption performance on water pollutants.
Disclosure of Invention
The invention aims at the graphene oxide/TiO prepared by the existing literature2The problem that the retention rate of the composite membrane to water pollutants is low is solved by utilizing Ti3C2Preparation of graphene oxide/TiO with high rejection rate by compounding MXene quantum dots and graphene oxide2A method of composite membrane. The method comprises the steps of mixing a graphene oxide solution and Ti3C2Mixing MXene quantum dot solution, and ultrasonic treating in air atmosphere at certain temperature with Ti in ultrasonic process3C2MXene quantum dots are oxidized to TiO2Nanoparticles, and finally vacuum filtering the nascent TiO2The nano particles and the graphene oxide are uniformly and compositely loaded on the surface of the filter membrane and are used for intercepting and adsorbing heavy metal ions in water.
In order to achieve the purpose, the invention provides graphene oxide/TiO2The preparation method of the composite film comprises the following steps of Ti3C2Preparation of MXene quantum dot solution, graphene oxide and Ti3C2Preparation of MXene quantum dot mixed solution and Ti3C2Oxidation of MXene quantum dots and graphene oxide/TiO2Preparing the composite membrane;
step 1: ti3C2Preparation of MXene quantum dot solution
The Ti after being intercalated, processed and dried by N, N dimethyl sulfoxide3C2Mixing MXene and deionized water in a mass ratio of 1: 100, crushing for 6 hours by using an ultrasonic crusher, and carrying out ice bath in the whole process; centrifuging the suspension at 10000 r/min, filtering the supernatant with 0.22 μm filter membrane to obtain the final productBlackish green Ti3C2MXene quantum dot solution;
step 2: graphene oxide and Ti3C2Preparation of MXene quantum dot mixed solution
According to graphene oxide and Ti3C2The mass ratio of MXene quantum dots is 10: 1-2: 1, and graphene oxide solution and Ti are mixed3C2Mixing MXene quantum dot solution in proportion to obtain mixed solution;
and step 3: ti3C2Oxidation of MXene quantum dots
Controlling the air flow rate to be 100-400 mL/min, continuously charging air into the mixed solution obtained in the step (2), and carrying out ultrasonic treatment at the temperature of 35-55 ℃ for 30 min to obtain Ti3C2MXene quantum dots are oxidized to TiO2A nanoparticle;
and 4, step 4: graphene oxide/TiO2Preparation of composite membranes
Pouring the product obtained in the step 3 into a filter flask with a microfiltration membrane, and filtering TiO by vacuum2The nano particles and the graphene oxide are loaded on the surface of the micro-filtration membrane in a composite way to obtain the graphene oxide/TiO2A composite membrane.
The graphene oxide is prepared by a Hummer chemical oxidation method.
The invention has the beneficial effects that:
1. the flux of the graphene oxide membrane is small, and the heavy metal removing effect is general, by newly generating TiO2The nano-particles are introduced, so that the interlayer distance of the membrane is enlarged, and the flux of the membrane is increased; simultaneous formation of TiO2The surface is rich in hydroxyl, and can effectively adsorb heavy metal cations in a water body, so that the removal rate of the heavy metal ions by the membrane is obviously improved.
2. The graphene oxide/TiO of the invention2The pure water flux of the composite membrane is far greater than that of a pure graphene oxide membrane, and along with TiO2The doping proportion is increased, the flux presents an increasing trend, and the maximum doping proportion can reach 83L m-2 h-1 bar-16.4 times that of a pure graphene oxide film.
3. The graphene oxide/TiO of the invention2Composite membrane for Pb in water2+，Cd2+Has high removal rate to Pb in water2+The retention rate of the graphene oxide membrane can reach 100 percent, which is far higher than 86 percent of that of a pure graphene oxide membrane.
4. The method has simple process and is easy to industrially popularize and apply.
Drawings
FIG. 1 shows the graphene oxide/TiO prepared in example 1 of the present invention2Scanning electron microscope images of the composite films;
FIG. 2 shows the graphene oxide/TiO prepared according to the present invention2Pure water membrane flux diagram of the composite membrane;
FIG. 3 shows the graphene oxide/TiO prepared according to the present invention2The composite membrane can be used for treating lead ions (Pb) in drinking water2+) Retention diagram of (c).
Detailed Description
The following is a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements are also considered to be within the scope of the present invention.
Example 1
Mixing graphene oxide solution and Ti3C2Mixing MXene quantum dot solution at a ratio of 10:1 to obtain mixed solution, and subjecting to ultrasonic treatment at 35 deg.C for 6 hr under continuous air flow (flow 100 mL/min), and adding Ti3C2MXene quantum dots are oxidized to TiO2Nano-particles, then pouring the mixed solution into a filter flask with a microfiltration membrane, and filtering the newly-generated TiO by vacuum2The nano particles and the graphene oxide are loaded on the surface of the micro-filtration membrane in a composite way to obtain the graphene oxide/TiO2A composite membrane. The membrane flux of the composite membrane is 15L m-2 h-1 bar-1For lead ion (Pb) in water2+) The retention of (a) was 92%.
Example 2
Mixing graphene oxide solution and Ti3C2Mixing MXene quantum dot solution at a ratio of 8:1 to obtain mixed solution, and introducing air (flow rate 125 mL/min) continuously and performing ultrasonic treatment at 40 deg.C to obtain 6Hour of Ti3C2MXene quantum dots are oxidized to TiO2Nano-particles, then pouring the mixed solution into a filter flask with a microfiltration membrane, and filtering the newly-generated TiO by vacuum2The nano particles and the graphene oxide are loaded on the surface of the micro-filtration membrane in a composite way to obtain the graphene oxide/TiO2A composite membrane. The membrane flux of the composite membrane is 20L m-2 h-1 bar-1For lead ion (Pb) in water2+) The retention rate of (D) was 94.2%.
Example 3
Mixing graphene oxide solution and Ti3C2Mixing MXene quantum dot solution at a ratio of 6:1 to obtain mixed solution, and subjecting to ultrasonic treatment at 45 deg.C for 6 hr under continuous air flow (flow 175 mL/min), and adding Ti3C2MXene quantum dots are oxidized to TiO2Nano-particles, then pouring the mixed solution into a filter flask with a microfiltration membrane, and filtering the newly-generated TiO by vacuum2The nano particles and the graphene oxide are loaded on the surface of the micro-filtration membrane in a composite way to obtain the graphene oxide/TiO2A composite membrane. The membrane flux of the composite membrane is 31.5L m-2 h-1 bar-1For lead ion (Pb) in water2+) The retention rate of (a) was 98.6%.
Example 4
Mixing graphene oxide solution and Ti3C2Mixing MXene quantum dot solution at a ratio of 4:1 to obtain mixed solution, and subjecting to ultrasonic treatment at 50 deg.C for 6 hr under continuous air (flow rate of 250 mL/min) to obtain Ti3C2MXene quantum dots are oxidized to TiO2Nano-particles, then pouring the mixed solution into a filter flask with a microfiltration membrane, and filtering the newly-generated TiO by vacuum2And (3) carrying the nano particles and the graphene oxide on the surface of the microfiltration membrane in a composite way to obtain the composite membrane. The membrane flux of the composite membrane is 42L m-2h-1 bar-1For lead ion (Pb) in water2+) The rejection of (a) was 100%.
Example 5
Mixing graphene oxide solution and Ti3C2Mixing MXene quantum dot solution according to the proportion of 3:1Mixing the solution, continuously introducing air (flow rate 325 mL/min) and performing ultrasonic treatment at 55 ℃ for 6 hours, and obtaining Ti3C2MXene quantum dots are oxidized to TiO2Nano-particles, then pouring the mixed solution into a filter flask with a microfiltration membrane, and filtering the newly-generated TiO by vacuum2The nano particles and the graphene oxide are loaded on the surface of the micro-filtration membrane in a composite way to obtain the graphene oxide/TiO2A composite membrane. The membrane flux of the composite membrane is 59L m-2 h-1 bar-1For lead ion (Pb) in water2+) The retention rate of (a) was 99.5%.
Example 6
Mixing graphene oxide solution and Ti3C2Mixing MXene quantum dot solution at a ratio of 2:1 to obtain mixed solution, and subjecting to ultrasonic treatment at 55 deg.C for 6 hr under continuous air flow (400 mL/min), and adding Ti3C2MXene quantum dots are oxidized to TiO2Nano-particles, then pouring the mixed solution into a filter flask with a microfiltration membrane, and filtering the newly-generated TiO by vacuum2The nano particles and the graphene oxide are loaded on the surface of the micro-filtration membrane in a composite way to obtain the graphene oxide/TiO2A composite membrane. The membrane flux of the composite membrane is 83L m-2 h-1 bar-1For lead ion (Pb) in water2+) The retention rate of (D) was 97.5%.

Claims (2)

1. Graphene oxide/TiO2The preparation method of the composite membrane is characterized by comprising the following steps: the preparation method comprises Ti3C2Preparation of MXene quantum dot solution, graphene oxide and Ti3C2Preparation of MXene quantum dot mixed solution and Ti3C2Oxidation of MXene quantum dots and graphene oxide/TiO2Preparing the composite membrane;
step 1: ti3C2Preparation of MXene quantum dot solution
The Ti after being intercalated, processed and dried by N, N dimethyl sulfoxide3C2Mixing MXene and deionized water in a mass ratio of 1: 100, crushing for 6 hours by using an ultrasonic crusher, and carrying out ice bath in the whole process; subjecting to ultrasonic waveCentrifuging at 10000 r/min, filtering the supernatant with 0.22 μm filter membrane to obtain dark green Ti3C2MXene quantum dot solution;
step 2: graphene oxide and Ti3C2Preparation of MXene quantum dot mixed solution
According to graphene oxide and Ti3C2The mass ratio of MXene quantum dots is 10: 1-2: 1, and graphene oxide solution and Ti are mixed3C2Mixing MXene quantum dot solution in proportion to obtain mixed solution;
and step 3: ti3C2Oxidation of MXene quantum dots
Controlling the air flow rate to be 100-400 mL/min, continuously charging air into the mixed solution obtained in the step (2), and carrying out ultrasonic treatment at the temperature of 35-55 ℃ for 30 min to obtain Ti3C2MXene quantum dots are oxidized to TiO2A nanoparticle;
and 4, step 4: graphene oxide/TiO2Preparation of composite membranes
Pouring the product obtained in the step 3 into a filter flask with a microfiltration membrane, and filtering TiO by vacuum2The nano particles and the graphene oxide are loaded on the surface of the micro-filtration membrane in a composite way to obtain the graphene oxide/TiO2A composite membrane.
2. Graphene oxide/TiO according to claim 12The preparation method of the composite membrane is characterized by comprising the following steps: the graphene oxide is prepared by a Hummer chemical oxidation method.
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CN115849861A (en) * 2022-11-22 2023-03-28 安徽宇航派蒙健康科技股份有限公司 Composite graphene heat-conducting film and preparation method thereof

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