CN111495220A - Preparation method of modified MXene two-dimensional layered material, modified microfiltration membrane and application - Google Patents
Preparation method of modified MXene two-dimensional layered material, modified microfiltration membrane and application Download PDFInfo
- Publication number
- CN111495220A CN111495220A CN202010327667.8A CN202010327667A CN111495220A CN 111495220 A CN111495220 A CN 111495220A CN 202010327667 A CN202010327667 A CN 202010327667A CN 111495220 A CN111495220 A CN 111495220A
- Authority
- CN
- China
- Prior art keywords
- modified
- layered material
- mxene
- dimensional layered
- microfiltration membrane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/78—Graft polymers
-
- 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
- B01D67/0002—Organic 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
-
- 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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
本发明属于过滤膜技术领域，具体是一种改性MXene二维层状材料的制备方法、改性微滤膜及应用，将氨基改性MXene二维层状材料分散在第一极性有机溶剂中，加入缚酸剂搅拌溶解，加入蒽醌‑2‑磺酰氯，在40～60℃以下搅拌1～8小时，过滤，清洗，干燥，获得所述改性MXene二维层状材料；再将所述改性MXene二维层状材料超声分散在第二极性有机溶剂中形成分散液，倒入放置有所述微滤膜的抽滤瓶中，真空抽滤，获得所述改性微滤膜。本发明的改性微滤膜可用于含偶氮染料、硝酸盐等的污水处理。
The invention belongs to the technical field of filtration membranes, in particular to a preparation method of a modified MXene two-dimensional layered material, a modified microfiltration membrane and application thereof. The amino-modified MXene two-dimensional layered material is dispersed in a first polar organic solvent , adding an acid binding agent, stirring and dissolving, adding anthraquinone-2-sulfonyl chloride, stirring for 1-8 hours below 40-60° C., filtering, cleaning, and drying to obtain the modified MXene two-dimensional layered material; The modified MXene two-dimensional layered material is ultrasonically dispersed in a second polar organic solvent to form a dispersion, poured into a suction filtration bottle on which the microfiltration membrane is placed, and vacuum filtered to obtain the modified microfiltration membrane. The modified microfiltration membrane of the present invention can be used for the treatment of sewage containing azo dyes, nitrates and the like.
Description
技术领域technical field
本发明属于过滤膜技术领域，涉及一种改性MXene二维层状材料的制备方法、改性微滤膜及应用。The invention belongs to the technical field of filtration membranes, and relates to a preparation method of a modified MXene two-dimensional layered material, a modified microfiltration membrane and applications.
背景技术Background technique
以醌类化合物为主的氧化还原介体在偶氮染料、硝酸盐等含氮污水的处理中具有广泛的应用。氧化还原介体作为电子的传递体提高了偶氮染料、硝酸盐等的厌氧生物降解速率，可提高1至几个数量级。Redox mediators dominated by quinone compounds are widely used in the treatment of nitrogen-containing sewage such as azo dyes and nitrates. Redox mediators act as electron transporters to increase the anaerobic biodegradation rates of azo dyes, nitrates, etc., by 1 to several orders of magnitude.
将醌类化合物固定在膜上是一种提高醌类化合物可回收使用、减少或避免醌类化合物溶解在水中造成二次污染的一种方法，CN103936146B公开了在尼龙膜上修饰固定醌类化合物的方法。但人们期望偶氮染料、硝酸盐等能有更高的促进生物降解速率。Fixing quinones on the membrane is a method for improving the recyclability of quinones, reducing or avoiding secondary pollution caused by dissolving quinones in water. CN103936146B discloses the modification and immobilization of quinones on nylon membranes. method. However, it is expected that azo dyes, nitrates, etc. can have a higher accelerated biodegradation rate.
发明内容SUMMARY OF THE INVENTION
本发明的一个目的在于克服现有技术缺陷，提供一种改性MXene二维层状材料的制备方法。One object of the present invention is to overcome the defects of the prior art and provide a preparation method of a modified MXene two-dimensional layered material.
本发明的另一个目的在于提供一种改性微滤膜。Another object of the present invention is to provide a modified microfiltration membrane.
本发明还有一个目的在于提供一种改性微滤膜的应用。Another object of the present invention is to provide an application of the modified microfiltration membrane.
本发明的技术方案如下：The technical scheme of the present invention is as follows:
一种改性MXene二维层状材料的制备方法，将氨基改性MXene二维层状材料分散在第一极性有机溶剂中，加入缚酸剂搅拌溶解，加入蒽醌-2-磺酰氯，在40～60℃以下搅拌1～8小时，过滤，清洗，干燥，获得所述改性MXene二维层状材料。A method for preparing a modified MXene two-dimensional layered material, the amino-modified MXene two-dimensional layered material is dispersed in a first polar organic solvent, an acid binding agent is added to stir and dissolve, an anthraquinone-2-sulfonyl chloride is added, The modified MXene two-dimensional layered material is obtained by stirring at below 40-60° C. for 1-8 hours, filtering, washing and drying.
优选的，所述氨基改性MXene二维层状材料为氨基硅烷偶联剂改性MXene二维层状材料。所用氨基硅烷偶联剂选自3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、3-氨基丙基甲基二甲氧基硅烷、3-氨基丙基甲基二乙氧基硅烷、N-(2-氨乙基)-3-氨丙基甲基二甲氧基硅烷、N-(2-氨乙基)-3-氨丙基三甲氧基硅烷、N-(2-氨乙基)-3-氨丙基三乙氧基硅烷和N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷中的至少一种。Preferably, the amino-modified MXene two-dimensional layered material is an aminosilane coupling agent-modified MXene two-dimensional layered material. The aminosilane coupling agent used is selected from 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-aminopropylmethyldimethoxysilane, 3-aminopropylmethyldimethoxysilane Ethoxysilane, N-(2-aminoethyl)-3-aminopropylmethyldimethoxysilane, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, N- At least one of (2-aminoethyl)-3-aminopropyltriethoxysilane and N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane.
更优选的，所述MXene二维层状材料的层数不超过5层，横向尺寸不超过5μm。More preferably, the number of layers of the MXene two-dimensional layered material does not exceed 5 layers, and the lateral dimension does not exceed 5 μm.
MXene二维层状材料表面含有末端O基团、羟基等活性基团，因此可以与硅烷偶联剂反应，在表面接枝有机官能团。一种氨基改性MXene二维层状材料的方法为：将5重量份氨基硅烷偶联剂加入到100重量份醇水溶液(无水乙醇和水体积比95:5)中，搅拌均匀，加入20重量份MXene二维层状材料，超声分散均匀，常温下搅拌12h或者升温至60℃反应3小时，过滤，清洗，干燥，即获得氨基改性MXene二维层状材料。本发明所使用的MXene二维层状材料为薄层状，层数不超过5层，横向尺寸不超过5μm，可以选自Ti3C2-MXene、Ti2C-MXene、Ti4C3-MXene、V3C2-MXene、Ti3ZnC2-MXene和Ti2ZnC-MXene中的一种或几种。The surface of MXene two-dimensional layered material contains terminal O groups, hydroxyl groups and other active groups, so it can react with silane coupling agents to graft organic functional groups on the surface. A method for an amino-modified MXene two-dimensional layered material is as follows: adding 5 parts by weight of an amino silane coupling agent to 100 parts by weight of an alcohol aqueous solution (volume ratio of absolute ethanol and water: 95:5), stirring evenly, adding 20 parts by weight of an amino silane coupling agent. The MXene two-dimensional layered material in parts by weight is uniformly dispersed by ultrasonic, stirred for 12 hours at room temperature or heated to 60° C. for 3 hours, filtered, washed, and dried to obtain an amino-modified MXene two-dimensional layered material. The MXene two-dimensional layered material used in the present invention is thin-layered, the number of layers does not exceed 5, and the lateral dimension does not exceed 5 μm, and can be selected from Ti 3 C 2 -MXene, Ti 2 C-MXene, Ti 4 C 3 - One or more of MXene, V 3 C 2 -MXene, Ti 3 ZnC 2 -MXene and Ti 2 ZnC-MXene.
所述第一有机溶剂并无特别限制，优选乙酸丁酯、四氢呋喃、乙酸乙酯、丙酮、丁酮和1,4-二氧六环中的至少一种。The first organic solvent is not particularly limited, preferably at least one of butyl acetate, tetrahydrofuran, ethyl acetate, acetone, butanone and 1,4-dioxane.
优选的，所述氨基改性MXene二维层状材料和蒽醌-2-磺酰氯的重量比为1:0.1～0.3。Preferably, the weight ratio of the amino-modified MXene two-dimensional layered material to anthraquinone-2-sulfonyl chloride is 1:0.1-0.3.
优选的，所述缚酸剂选自三乙胺、三乙醇胺、碳酸钠、碳酸钾、碳酸氢钠、碳酸氢钾、N-乙基二乙醇胺、二甲基乙醇胺和N-甲基二乙醇胺中的至少一种。Preferably, the acid binding agent is selected from triethylamine, triethanolamine, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, N-ethyldiethanolamine, dimethylethanolamine and N-methyldiethanolamine at least one of.
优选的，所述缚酸剂和蒽醌-2-磺酰氯的摩尔比为1:0.5～0.9。Preferably, the molar ratio of the acid binding agent and anthraquinone-2-sulfonyl chloride is 1:0.5-0.9.
一种改性微滤膜，包含上述任一实施方案所述的制备方法获得的改性MXene二维层状材料和微滤膜，所述改性MXene二维层状材料负载在所述微滤膜的表面。A modified microfiltration membrane, comprising a modified MXene two-dimensional layered material and a microfiltration membrane obtained by the preparation method described in any of the above embodiments, wherein the modified MXene two-dimensional layered material is supported on the microfiltration membrane. the surface of the membrane.
一种上述实施方案所述的改性微滤膜的制备方法，将所述改性MXene二维层状材料超声分散在第二极性有机溶剂中形成分散液，倒入放置有所述微滤膜的抽滤瓶中，真空抽滤，获得所述改性微滤膜。A method for preparing a modified microfiltration membrane according to the above embodiment, ultrasonically dispersing the modified MXene two-dimensional layered material in a second polar organic solvent to form a dispersion, pouring the The modified microfiltration membrane is obtained by vacuum filtration in the suction filtration bottle of the membrane.
优选的，所述第二极性有机溶剂选自丙酮、四氢呋喃、无水乙醇、DMF、DMSO、异丙醇、乙酸乙酯和乙酸丁酯中的一种。Preferably, the second polar organic solvent is selected from one of acetone, tetrahydrofuran, absolute ethanol, DMF, DMSO, isopropanol, ethyl acetate and butyl acetate.
优选的，所述分散液的浓度为5～50mg/ml。Preferably, the concentration of the dispersion liquid is 5-50 mg/ml.
MXene二维层状材料具有高的导电性能，同时比表面积高、表面拥有羟基等活性基团，可进一步进行化学反应，在其表面接枝有机官能团，而且有机官能团的密度较高。The MXene two-dimensional layered material has high electrical conductivity, high specific surface area, and active groups such as hydroxyl on the surface, which can further undergo chemical reactions and graft organic functional groups on its surface, and the density of organic functional groups is high.
本发明的有益效果是：The beneficial effects of the present invention are:
(1)本发明采用氨基硅烷偶联剂改性MXene，使得MXene表面拥有较高密度的氨基，再与含酰氯的蒽醌化合物反应，氨基和酰氯的反应活性很高，因此在MXene表面接枝上较高密度的蒽醌化合物。(1) The present invention uses aminosilane coupling agent to modify MXene, so that the surface of MXene has higher density of amino groups, and then reacts with the anthraquinone compound containing acid chloride, the reactivity of amino group and acid chloride is very high, so grafting on the surface of MXene higher density anthraquinone compounds.
(2)MXene的高导电性进一步提升了蒽醌化合物在水环境中传递电子的能力。因此本发明的改性MXene二维材料可以更快的促进偶氮染料、硝酸盐等的生物降解。(2) The high conductivity of MXene further enhances the ability of anthraquinone compounds to transfer electrons in aqueous environment. Therefore, the modified MXene two-dimensional material of the present invention can accelerate the biodegradation of azo dyes, nitrates and the like.
(3)本发明将改性MXene二维材料负载在微滤膜上，在过滤含偶氮染料和/或硝酸盐的污水时可以对其中的偶氮染料、硝酸盐等进行生物降解，还可以将成膜的蒽醌改性MXene二维材料单独用于含偶氮染料和/或硝酸盐的污水处理，处理效率高，而且回收方便。(3) In the present invention, the modified MXene two-dimensional material is loaded on the microfiltration membrane, and the azo dyes, nitrates, etc. can be biodegraded when filtering the sewage containing azo dyes and/or nitrates. The film-forming anthraquinone-modified MXene two-dimensional material is used alone for the treatment of sewage containing azo dyes and/or nitrates, with high treatment efficiency and convenient recovery.
附图说明Description of drawings
图1为不同膜材料对酸性红B溶液的降解速率对比。Figure 1 is a comparison of the degradation rates of different membrane materials to acid red B solution.
图2为不同膜材料对硝酸盐溶液的降解速率对比。Figure 2 is a comparison of the degradation rates of different membrane materials to nitrate solutions.
图3为不同膜材料对酸性红B溶液降解循环测试对比。Figure 3 is a comparison of the degradation cycle test of different membrane materials on acid red B solution.
图4为不同膜材料对硝酸盐溶液降解循环测试对比。Figure 4 is a comparison of the degradation cycle test of different membrane materials on nitrate solution.
图5为不同微滤膜对酸性红B溶液过滤中的降解性能对比。Figure 5 is a comparison of the degradation performance of different microfiltration membranes in the filtration of acid red B solution.
图6为不同微滤膜对硝酸盐溶液过滤中的降解性能对比。Figure 6 is a comparison of the degradation performance of different microfiltration membranes in the filtration of nitrate solution.
具体实施方式Detailed ways
以下通过具体实施方式对本发明的技术方案进行进一步的说明和描述。The technical solutions of the present invention will be further illustrated and described below through specific embodiments.
实施例1Example 1
按氨基改性MXene二维层状材料、四氢呋喃和蒽醌-2-磺酰氯重量比1:5:0.1以及三乙胺和蒽醌-2-磺酰氯摩尔比1:0.5配料，将氨基改性MXene二维层状材料分散在四氢呋喃中，加入三乙胺搅拌溶解，加入蒽醌-2-磺酰氯，在40℃以下搅拌8小时，过滤，清洗，干燥，获得改性MXene二维层状材料，记为M-1。Amino-modified MXene two-dimensional layered material, tetrahydrofuran and anthraquinone-2-sulfonyl chloride in a weight ratio of 1:5:0.1, and triethylamine and anthraquinone-2-sulfonyl chloride in a molar ratio of 1:0.5 were prepared. The MXene two-dimensional layered material was dispersed in tetrahydrofuran, added with triethylamine and stirred to dissolve, added with anthraquinone-2-sulfonyl chloride, stirred at below 40 °C for 8 hours, filtered, washed and dried to obtain a modified MXene two-dimensional layered material , denoted as M-1.
实施例2Example 2
按氨基改性MXene二维层状材料、1,4-二氧六环和蒽醌-2-磺酰氯重量比1:20:0.3以及三乙醇胺和蒽醌-2-磺酰氯摩尔比1:0.9配料，将氨基改性MXene二维层状材料分散在1,4-二氧六环中，加入三乙醇胺搅拌溶解，加入蒽醌-2-磺酰氯，在60℃以下搅拌3小时，过滤，清洗，干燥，获得改性MXene二维层状材料，记为M-2。According to the amino-modified MXene two-dimensional layered material, the weight ratio of 1,4-dioxane and anthraquinone-2-sulfonyl chloride is 1:20:0.3 and the molar ratio of triethanolamine and anthraquinone-2-sulfonyl chloride is 1:0.9 Ingredients, disperse the amino-modified MXene two-dimensional layered material in 1,4-dioxane, add triethanolamine and stir to dissolve, add anthraquinone-2-sulfonyl chloride, stir at below 60 ° C for 3 hours, filter, wash , and dried to obtain a modified MXene two-dimensional layered material, denoted as M-2.
实施例3Example 3
按氨基改性MXene二维层状材料、乙酸丁酯和蒽醌-2-磺酰氯重量比1:12:0.2以及碳酸钠和蒽醌-2-磺酰氯摩尔比1:0.7配料，将氨基改性MXene二维层状材料分散在乙酸丁酯中，加入碳酸钠搅拌溶解，加入蒽醌-2-磺酰氯，在60℃以下搅拌2小时，过滤，清洗，干燥，获得改性MXene二维层状材料，记为M-3。According to the formula of amino-modified MXene two-dimensional layered material, butyl acetate and anthraquinone-2-sulfonyl chloride in a weight ratio of 1:12:0.2 and a molar ratio of sodium carbonate and anthraquinone-2-sulfonyl chloride at 1:0.7, the amino-modified The two-dimensional MXene layered material was dispersed in butyl acetate, sodium carbonate was added and stirred to dissolve, anthraquinone-2-sulfonyl chloride was added, stirred for 2 hours below 60 °C, filtered, washed, and dried to obtain a modified MXene two-dimensional layer. material, denoted as M-3.
实施例4Example 4
按氨基改性MXene二维层状材料、四氢呋喃和蒽醌-2-磺酰氯重量比1:15:0.25以及三乙胺和蒽醌-2-磺酰氯摩尔比1:0.8配料，将氨基改性MXene二维层状材料分散在四氢呋喃中，加入三乙胺搅拌溶解，加入蒽醌-2-磺酰氯，在50℃以下搅拌6小时，过滤，清洗，干燥，获得改性MXene二维层状材料，记为M-4。Amino-modified MXene two-dimensional layered material, tetrahydrofuran and anthraquinone-2-sulfonyl chloride in a weight ratio of 1:15:0.25, and triethylamine and anthraquinone-2-sulfonyl chloride in a molar ratio of 1:0.8 were prepared. The MXene two-dimensional layered material was dispersed in tetrahydrofuran, added with triethylamine and stirred to dissolve, added with anthraquinone-2-sulfonyl chloride, stirred at below 50 °C for 6 hours, filtered, washed and dried to obtain the modified MXene two-dimensional layered material , denoted as M-4.
实施例5Example 5
将M-1超声分散在四氢呋喃中形成浓度为25mg/ml的分散液，倒入放置有微滤膜的抽滤瓶中，真空抽滤，干燥，获得改性微滤膜，记为F-1。取下F-1表面的MXene膜，记为MX-1。M-1 was ultrasonically dispersed in tetrahydrofuran to form a dispersion with a concentration of 25 mg/ml, poured into a suction filtration bottle with a microfiltration membrane, vacuum filtered, and dried to obtain a modified microfiltration membrane, denoted as F-1 . The MXene film on the surface of F-1 was removed and recorded as MX-1.
实施例6Example 6
将M-2超声分散在无水乙醇中形成浓度为5mg/ml的分散液，倒入放置有微滤膜的抽滤瓶中，真空抽滤，干燥，获得改性微滤膜，记为F-2。取下F-2表面的MXene膜，记为MX-2。M-2 was ultrasonically dispersed in absolute ethanol to form a dispersion with a concentration of 5 mg/ml, poured into a suction filtration bottle with a microfiltration membrane, vacuum filtered, and dried to obtain a modified microfiltration membrane, denoted as F -2. The MXene film on the surface of F-2 was removed and recorded as MX-2.
实施例7Example 7
将M-3超声分散在乙酸丁酯中形成浓度为50mg/ml的分散液，倒入放置有微滤膜的抽滤瓶中，真空抽滤，干燥，获得改性微滤膜，记为F-3。取下F-3表面的MXene膜，记为MX-3。M-3 was ultrasonically dispersed in butyl acetate to form a dispersion with a concentration of 50 mg/ml, poured into a suction filtration bottle with a microfiltration membrane, vacuum filtered, and dried to obtain a modified microfiltration membrane, denoted as F -3. The MXene film on the surface of F-3 was removed and recorded as MX-3.
实施例8Example 8
将M-4超声分散在四氢呋喃中形成浓度为35mg/ml的分散液，倒入放置有微滤膜的抽滤瓶中，真空抽滤，干燥，获得改性微滤膜，记为F-4。取下F-4表面的MXene膜，记为MX-4。M-4 was ultrasonically dispersed in tetrahydrofuran to form a dispersion with a concentration of 35 mg/ml, poured into a suction filtration bottle with a microfiltration membrane, vacuum filtered, and dried to obtain a modified microfiltration membrane, denoted as F-4 . The MXene film on the surface of F-4 was removed and recorded as MX-4.
实施例9Example 9
将M-2超声分散在异丙醇中形成浓度为20mg/ml的分散液，倒入放置有微滤膜的抽滤瓶中，真空抽滤，干燥，获得改性微滤膜，记为F-5。取下F-5表面的MXene膜，记为MX-5。M-2 was ultrasonically dispersed in isopropanol to form a dispersion with a concentration of 20 mg/ml, poured into a suction filtration bottle with a microfiltration membrane, vacuum filtered, and dried to obtain a modified microfiltration membrane, denoted as F -5. The MXene film on the surface of F-5 was removed and recorded as MX-5.
实施例10Example 10
将M-3超声分散在四氢呋喃中形成浓度为30mg/ml的分散液，倒入放置有微滤膜的抽滤瓶中，真空抽滤，干燥，获得改性微滤膜，记为F-6。取下F-6表面的MXene膜，记为MX-6。M-3 was ultrasonically dispersed in tetrahydrofuran to form a dispersion with a concentration of 30 mg/ml, poured into a suction filtration bottle with a microfiltration membrane, vacuum filtered, and dried to obtain a modified microfiltration membrane, denoted as F-6 . The MXene film on the surface of F-6 was removed and denoted as MX-6.
对比例1Comparative Example 1
蒽醌化合物固定在尼龙膜上，记为P-1。The anthraquinone compound was immobilized on the nylon membrane, denoted as P-1.
对比例2Comparative Example 2
市售微滤膜，记为F-7。Commercially available microfiltration membrane, denoted as F-7.
对偶氮染料的降解加速效果测试：分别取0.5g待测样品用生理盐水冲洗3次，加入到200ml含对数生长期的偶氮染料降解菌株GYZ(staphylococcus sp.)的150mg/L的酸性红B水溶液中，测定酸性红B浓度随时间的变化。结果如附图1所示。Degradation acceleration effect test on azo dyes: respectively take 0.5g of the sample to be tested and rinse it with normal saline for 3 times, add it to 200ml of acid red containing 150mg/L of the azo dye-degrading strain GYZ (staphylococcus sp.) in the logarithmic growth phase In the B aqueous solution, the change of acid red B concentration with time was measured. The results are shown in Figure 1.
对硝酸盐降解加速效果测试：分别取0.5g待测样品用生理盐水冲洗3次，加入到200ml含对数生长期反硝化微生物的150mg/L的硝酸盐水溶液中，测定硝酸盐浓度随时间的变化。结果如附图2所示。Test for the acceleration effect of nitrate degradation: take 0.5g of the sample to be tested and rinse it with physiological saline three times, add it to 200ml of 150mg/L nitrate aqueous solution containing denitrifying microorganisms in the logarithmic growth phase, and measure the nitrate concentration over time. Variety. The results are shown in Figure 2.
对酸性红B和硝酸盐的降解速率的循环测试结果分别如附图3和附图4所示。The cycle test results for the degradation rates of Acid Red B and nitrate are shown in Figure 3 and Figure 4, respectively.
用待测微滤膜过滤酸性红B浓度为150mg/L的水溶液，测试不同过滤时间的滤出液中酸性红B浓度，结果如附图5所示。The aqueous solution with the acid red B concentration of 150 mg/L was filtered with the microfiltration membrane to be tested, and the acid red B concentration in the filtrate with different filtration times was tested. The results are shown in Figure 5.
用待测微滤膜过滤硝酸盐浓度为150mg/L的水溶液，测试不同过滤时间的滤出液中硝酸盐浓度，结果如附图6所示。Use the microfiltration membrane to be tested to filter an aqueous solution with a nitrate concentration of 150 mg/L, and test the nitrate concentration in the filtrate with different filtration times. The results are shown in Figure 6.
因此，本发明的改性微滤膜可用于含偶氮染料、硝酸盐等的污水处理，处理效果较好。Therefore, the modified microfiltration membrane of the present invention can be used for the treatment of sewage containing azo dyes, nitrates, etc., and the treatment effect is good.
以上所述，显示和描述了本发明的基本原理、主要特征和优点。本领域技术人员应该了解本发明不受上述实施例的限制，上述实施例仅为本发明的较佳实施例而已，不能依此限定本发明实施的范围，即依本发明专利范围及说明书内容所作的等效变化与修饰，皆应仍属本发明涵盖的范围内。本发明要求保护范围由所附的权利要求书及其等同物界定。The foregoing has shown and described the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above-mentioned embodiments, and the above-mentioned embodiments are only preferred embodiments of the present invention, and the scope of the implementation of the present invention cannot be limited accordingly, that is, the scope of the present invention and the contents of the description are made Equivalent changes and modifications should still fall within the scope of the present invention. The claimed scope of the present invention is defined by the appended claims and their equivalents.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010327667.8A CN111495220A (en) | 2020-04-23 | 2020-04-23 | Preparation method of modified MXene two-dimensional layered material, modified microfiltration membrane and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010327667.8A CN111495220A (en) | 2020-04-23 | 2020-04-23 | Preparation method of modified MXene two-dimensional layered material, modified microfiltration membrane and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111495220A true CN111495220A (en) | 2020-08-07 |
Family
ID=71877895
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010327667.8A Pending CN111495220A (en) | 2020-04-23 | 2020-04-23 | Preparation method of modified MXene two-dimensional layered material, modified microfiltration membrane and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111495220A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111825215A (en) * | 2020-06-17 | 2020-10-27 | 龙岩市厦龙工程技术研究院 | Membrane bioreactor treatment method for nitrogen-containing wastewater |
| CN111925560A (en) * | 2020-08-18 | 2020-11-13 | 中国科学院兰州化学物理研究所 | Ti3C2Application of (E) -MXene and modified Ti3C2-MXene/NBR composite material and preparation thereof |
| CN112473372A (en) * | 2020-12-07 | 2021-03-12 | 江南大学 | Conductive forward osmosis membrane and preparation method thereof |
| CN112973476A (en) * | 2021-02-20 | 2021-06-18 | 华南理工大学 | Hydrophobic porous MXene membrane and preparation method and application thereof |
| CN113003675A (en) * | 2021-02-05 | 2021-06-22 | 南方科技大学 | Mxene material with organic chelating functional group grafted on surface and preparation method thereof |
| CN113060734A (en) * | 2021-04-06 | 2021-07-02 | 郑州大学 | A kind of infrared low emissivity MXene film and preparation method thereof |
| CN113582352A (en) * | 2021-07-29 | 2021-11-02 | 郑州大学 | Modified magnetic transition metal carbonitride and preparation method and application thereof |
| CN114162820A (en) * | 2021-12-07 | 2022-03-11 | 徐州纳烯新材料研究院有限公司 | Preparation method of MXene organic solvent dispersion liquid |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731285A (en) * | 2012-06-28 | 2012-10-17 | 大连理工大学 | A class of anthraquinone compounds and their applications |
| CN103801395A (en) * | 2014-02-26 | 2014-05-21 | 大连理工大学 | Graphene material modified by water-soluble anthraquinone compound and preparation method of graphene material |
| CN106178979A (en) * | 2016-08-31 | 2016-12-07 | 华南理工大学 | High-performance two-dimensional layered Ti3C2-MXene film and its preparation method and application in water treatment |
| EP3444020A1 (en) * | 2016-04-15 | 2019-02-20 | Nissan Chemical Corporation | Method for manufacturing gas separation membrane |
| CN110040842A (en) * | 2019-04-29 | 2019-07-23 | 厦门理工学院 | A kind of redox mediators are grafted on the method and application of inorganic filler surface |
-
2020
- 2020-04-23 CN CN202010327667.8A patent/CN111495220A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731285A (en) * | 2012-06-28 | 2012-10-17 | 大连理工大学 | A class of anthraquinone compounds and their applications |
| CN103801395A (en) * | 2014-02-26 | 2014-05-21 | 大连理工大学 | Graphene material modified by water-soluble anthraquinone compound and preparation method of graphene material |
| EP3444020A1 (en) * | 2016-04-15 | 2019-02-20 | Nissan Chemical Corporation | Method for manufacturing gas separation membrane |
| CN106178979A (en) * | 2016-08-31 | 2016-12-07 | 华南理工大学 | High-performance two-dimensional layered Ti3C2-MXene film and its preparation method and application in water treatment |
| CN110040842A (en) * | 2019-04-29 | 2019-07-23 | 厦门理工学院 | A kind of redox mediators are grafted on the method and application of inorganic filler surface |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111825215A (en) * | 2020-06-17 | 2020-10-27 | 龙岩市厦龙工程技术研究院 | Membrane bioreactor treatment method for nitrogen-containing wastewater |
| CN111925560A (en) * | 2020-08-18 | 2020-11-13 | 中国科学院兰州化学物理研究所 | Ti3C2Application of (E) -MXene and modified Ti3C2-MXene/NBR composite material and preparation thereof |
| CN112473372A (en) * | 2020-12-07 | 2021-03-12 | 江南大学 | Conductive forward osmosis membrane and preparation method thereof |
| CN112473372B (en) * | 2020-12-07 | 2022-04-29 | 江南大学 | A kind of conductive forward osmosis membrane and preparation method thereof |
| CN113003675A (en) * | 2021-02-05 | 2021-06-22 | 南方科技大学 | Mxene material with organic chelating functional group grafted on surface and preparation method thereof |
| WO2022165989A1 (en) * | 2021-02-05 | 2022-08-11 | 南方科技大学 | Mxene material having organic chelating functional groups grafted on surface and preparation method therefor |
| CN112973476A (en) * | 2021-02-20 | 2021-06-18 | 华南理工大学 | Hydrophobic porous MXene membrane and preparation method and application thereof |
| CN113060734A (en) * | 2021-04-06 | 2021-07-02 | 郑州大学 | A kind of infrared low emissivity MXene film and preparation method thereof |
| CN113582352A (en) * | 2021-07-29 | 2021-11-02 | 郑州大学 | Modified magnetic transition metal carbonitride and preparation method and application thereof |
| CN114162820A (en) * | 2021-12-07 | 2022-03-11 | 徐州纳烯新材料研究院有限公司 | Preparation method of MXene organic solvent dispersion liquid |
| WO2023103645A1 (en) * | 2021-12-07 | 2023-06-15 | 徐州纳烯新材料研究院有限公司 | Preparation method for mxene organic solvent dispersion |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111495220A (en) | Preparation method of modified MXene two-dimensional layered material, modified microfiltration membrane and application | |
| CN114163817B (en) | A kind of slow-release antibacterial film and preparation method thereof | |
| CN108554389B (en) | EDTA (ethylene diamine tetraacetic acid) -modified bacterial cellulose membrane adsorbent as well as preparation method and application thereof | |
| CN111545230A (en) | A kind of preparation method, product and application of nanometer titanium dioxide/MXene composite film | |
| CN110272895A (en) | A kind of medium immobilised enzymes and its preparation method and application | |
| CN110615817B (en) | Preparation of a ferrocene-based metal organic framework material and its application in water treatment | |
| CN107376851A (en) | A kind of preparation method and applications of partial vulcanization metal organic frame composite | |
| CN111569665A (en) | A kind of preparation method of flexible graphene oxide/metal organic framework composite filter membrane | |
| CN112358745B (en) | A kind of preparation method and application of modified pyrite | |
| CN105413496A (en) | Silver-loaded halloysite nanotube-polyvinyl alcohol separation membrane and preparation and application thereof | |
| CN117801203A (en) | High-temperature-resistant antistatic polyurethane foam material and preparation method thereof | |
| CN103193956B (en) | A kind of preparation and application of grafting-type optical azo polyurethane thermal-optic material | |
| CN114887494B (en) | Preparation method and application of metal ion leaching-free release-type MIL-53 modified membrane | |
| CN111495204B (en) | Modified microfiltration membrane and preparation method thereof | |
| CN110787774A (en) | Chitosan-manganese dioxide composite adsorption material and preparation method thereof | |
| WO2022100228A1 (en) | Method for applying pyrite in sewage treatment | |
| CN111944195A (en) | A kind of polyionic liquid modified cellulose aerogel and its preparation method and application | |
| CN115569638B (en) | Zr-MOF composite film protective material and preparation method thereof | |
| CN111533130A (en) | Preparation method of anthraquinone modified MXene two-dimensional layered material, modified microfiltration membrane and application | |
| CN109926030A (en) | A kind of poly ion liquid adsorbent material and preparation method thereof based on biomass residue | |
| WO2023173670A1 (en) | Preparation method for graphene oxide nano roll | |
| CN113667994B (en) | Preparation method of electrolytic hydrogen production electrode directly loaded with COF protective film | |
| CN111170422B (en) | A kind of preparation method of organic solvent resistant anion exchange membrane | |
| CN114618450A (en) | Conjugated microporous polymer composite material, preparation method thereof and adsorbent | |
| CN110330569A (en) | A kind of preparation method of high substituted degree oxycellulose |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |