A porous MXene / epoxy resin material for oil-water separation and its preparation method

Abstract

This invention discloses an MXene / epoxy resin porous material for oil-water separation and its preparation method. The porous material comprises: 3-10 parts by weight of MXene, 50-100 parts by weight of a hydrophobic modifier, 100-800 parts by weight of epoxy resin, 100-800 parts by weight of an epoxy curing agent, 100-500 parts by weight of polydimethylsiloxane (PDMS), and 10-50 parts by weight of PDMS curing agent. The porous material of this invention exhibits high oil absorption capacity and fast oil absorption rate, and can adsorb high-viscosity oils through photothermal conversion under light irradiation.

Description

Technical Field

[0001] This invention relates to the field of oil-absorbing materials technology. Specifically, it relates to an MXene / epoxy resin porous material for oil-water separation and its preparation method. Background Technology

[0002] The direct discharge of oily wastewater from chemical plants and crude oil leaks from oil and gas extraction have caused serious environmental pollution and resource waste. When oil leaks into the aquatic environment, it severely harms aquatic plants and animals, leading to ecological imbalance. Currently, oil-absorbing materials are one of the main solutions to these problems. There are many types of oil-absorbing materials, including clay, plant straw, foam, oil-absorbing gels, and oil-absorbing resins. Clay and plant straw have low oil absorption rates and are difficult to recycle, limiting their practical application. While oil-absorbing gels and resins have fast absorption rates and high absorption ratios, they are not effective at adsorbing high-viscosity oils (such as silicone oil, crude oil, and vegetable oil). Foam materials have a well-developed porous structure, allowing oil to easily diffuse into the pores and be adsorbed under capillary action. Therefore, porous materials are the primary choice for adsorbing high-viscosity oils.

[0003] Conventional porous materials exhibit poor oil-water selectivity, absorbing both oil and water simultaneously, and showing low adsorption rates when adsorbing high-viscosity oils. Therefore, this invention introduces MXene material with photothermal effects and performs a simple hydrophobic modification process to prepare an MXene / epoxy resin porous material for oil-water separation, which is of great significance for environmental protection and the recycling of non-renewable energy. Summary of the Invention

[0004] Therefore, the technical problem to be solved by the present invention is to provide an MXene / epoxy resin porous material for oil-water separation and its preparation method. The porous material has superhydrophobicity and a simple preparation process. The MXene material therein can enhance the photothermal conversion performance of the porous material and help improve the material's adsorption performance for high-viscosity oils.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution:

[0006] A porous MXene / epoxy resin material for oil-water separation comprises the following components: 3-10 parts by weight of MXene, 50-100 parts by weight of hydrophobic modifier, 100-800 parts by weight of epoxy resin, 100-800 parts by weight of epoxy resin curing agent, 100-500 parts by weight of polydimethylsiloxane, and 10-50 parts by weight of polydimethylsiloxane curing agent.

[0007] The aforementioned MXene / epoxy resin porous material for oil-water separation, wherein the MXene is one or more of Ti3C2, V2C, V4C3, Mo2TiC2, Mo2C, and Ta4C3.

[0008] The aforementioned MXene / epoxy resin porous material for oil-water separation uses a polar organic solvent selected from tetrahydrofuran, ethyl acetate, dichloromethane, chloroform, and cyclohexane.

[0009] The hydrophobic modifier in the above-mentioned MXene / epoxy resin porous material for oil-water separation is one of trimethoxy(1H,1H,2H,2H-heptadecylfluorodecyl)silane, octadecyltrichlorosilanemethyl, and trimethoxysilane.

[0010] The aforementioned MXene / epoxy resin porous material for oil-water separation, wherein the epoxy resin is one of epoxy resin E44 and epoxy resin E51.

[0011] The aforementioned MXene / epoxy resin porous material for oil-water separation uses an epoxy resin curing agent that is one of aliphatic polyamines, aromatic polyamines, and low molecular weight polyamide resins.

[0012] In the aforementioned MXene / epoxy resin porous material for oil-water separation, the polydimethylsiloxane is cured with diphenylcarbamate or silanol having a vinyl structure.

[0013] The aforementioned MXene / epoxy resin porous material for oil-water separation uses dimethylvinylsilane as a curing agent.

[0014] The preparation method of the above-mentioned MXene / epoxy resin porous material for oil-water separation includes the following steps:

[0015] Step 1) Add monolayer MXene powder to 50 mL of polar organic solvent and stir magnetically at room temperature for 0.5–1.5 h to obtain the first mixed solution;

[0016] Step 2) Disperse the first mixed solution obtained in Step 1) ultrasonically for 2-5 minutes, add a hydrophobic modifier while stirring, and react at 25℃-35℃ for 24 hours to obtain the second mixed solution;

[0017] Step 3) Add epoxy resin and epoxy resin curing agent, polydimethylsiloxane and polydimethylsiloxane curing agent to the second mixed solution obtained in step 2) to obtain the third mixed solution;

[0018] Step 4) The third mixed solution obtained in Step 3) is mechanically stirred at a rate of 350 rpm to 450 rpm for 15 to 30 minutes while simultaneously heating to 66 to 85°C until the porous material is formed; In this step, as the solvent evaporates, the solvent bubbles formed by the epoxy resin, epoxy resin curing agent, polydimethylsiloxane, and polydimethylsiloxane curing agent break down one by one and form cavities, thereby forming a porous material with residual solvent;

[0019] Step 5) The porous material obtained in step 4) is vacuum dried in a vacuum drying oven at 66℃~85℃ until the quality of the porous material no longer changes, and the MXene / epoxy resin porous material for oil-water separation is obtained.

[0020] The technical solution of the present invention achieves the following beneficial technical effects:

[0021] 1. The preparation process is stable and easy to operate, and can be industrialized.

[0022] 2. The porous material prepared by this invention has superhydrophobicity and can be used as an oil-absorbing material in the field of oil-water separation.

[0023] 3. The porous material prepared by this invention is a lightweight material with a true density of up to 0.1 g / cm³. 3 .

[0024] 4. The porous material prepared by this invention has photothermal conversion properties and can accelerate its adsorption of high-viscosity oils under sunlight. Attached Figure Description

[0025] Figure 1 This is a scanning electron microscope image of the porous material in this invention;

[0026] Figure 2 This is a diagram showing the adsorption ratio of the porous material for different oils in this invention.

[0027] Figure 3 This is a graph showing the adsorption ratio of the porous material to high-viscosity silicone oil before and after xenon lamp irradiation in this invention. Detailed Implementation

[0028] Example 1

[0029] In this embodiment, the MXene / epoxy resin porous material for oil-water separation is prepared through the following steps:

[0030] Step 1) Add 5 portions of monolayer Ti3C2 powder to 50 mL of tetrahydrofuran and stir magnetically for 1 h at room temperature to obtain the first mixed solution;

[0031] Step 2) The first mixed solution obtained in Step 1) is ultrasonically dispersed for 2 min, and 0.5 mL of trimethoxy(1H,1H,2H,2H-heptadecyl)silane is added under stirring. The mixture is reacted at 35 °C for 24 h to obtain the second mixed solution.

[0032] Step 3) Add 240 parts of EP and 240 parts of EP curing agent, 200 parts of PDMS and 20 parts of PDMS curing agent to the second mixed solution obtained in step 2) to obtain the third mixed solution;

[0033] Step 4) The third mixed solution obtained in step 3) is mechanically stirred at a rate of 400 rpm for 20 min while simultaneously heating to 80°C until the porous material is formed.

[0034] Step 5) The porous material obtained in step 4) is vacuum dried in a vacuum drying oven at 80°C until the quality of the porous material no longer changes, thus obtaining the MXene / epoxy resin porous material for oil-water separation.

[0035] In this embodiment, the epoxy resin and epoxy resin curing agent are E44 epoxy resin from Shenzhen Mingde Chemical Co., Ltd., and the PDMS and PDMS curing agent are Dow Corning 184PDMS from Shenzhen Songsen New Material Technology Co., Ltd.

[0036] Example 2

[0037] In this embodiment, the MXene / epoxy resin porous material for oil-water separation is prepared through the following steps:

[0038] Step 1) Add 5 portions of monolayer V2C powder to 50 mL of tetrahydrofuran and stir magnetically for 1 h at room temperature to obtain the first mixed solution;

[0039] Step 2): The first mixed solution obtained in Step 1) is ultrasonically dispersed for 2 min, and 0.5 mL of trimethoxy(1H,1H,2H,2H-heptadecyl)silane is added under stirring. The mixture is reacted at 35 °C for 24 h to obtain the second mixed solution.

[0040] Step 3): Add 240 parts of EP and 240 parts of EP curing agent, 200 parts of PDMS and 20 parts of PDMS curing agent to the second mixed solution obtained in step 2) to obtain the third mixed solution;

[0041] Step 4): The third mixed solution obtained in step 3) is mechanically stirred at a rate of 400 rpm for 20 min while simultaneously heating to 80°C until the porous material is formed.

[0042] Step 5): The porous material obtained in step 4) is vacuum dried in a vacuum drying oven at 80°C until the quality of the porous material no longer changes, thus obtaining the MXene / epoxy resin porous material for oil-water separation.

[0043] Example 3

[0044] In this embodiment, the MXene / epoxy resin porous material for oil-water separation is prepared through the following steps:

[0045] Step 1), five monolayer Ti3C2T samples were mixed. x The powder was added to 50 mL of tetrahydrofuran and magnetically stirred at room temperature for 1 h to obtain the first mixed solution;

[0046] Step 2): The first mixed solution obtained in step 1) is ultrasonically dispersed for 2 min, and 1 mL of octadecyltrichlorosilanemethyl is added under stirring. The mixture is reacted at 35 °C for 24 h to obtain the second mixed solution.

[0047] Step 3): Add 240 parts of EP and 240 parts of EP curing agent, 200 parts of PDMS and 20 parts of PDMS curing agent to the second mixed solution obtained in step 2) to obtain the third mixed solution;

[0048] Step 4): The third mixed solution obtained in step 3) is mechanically stirred at a rate of 400 rpm for 20 min while simultaneously heating to 80°C until the porous material is formed.

[0049] Step 5): The porous material obtained in step 4) is vacuum dried in a vacuum drying oven at 80°C until the quality of the porous material no longer changes, thus obtaining the MXene / epoxy resin porous material for oil-water separation.

[0050] Example 4

[0051] In this embodiment, the MXene / epoxy resin porous material for oil-water separation is prepared through the following steps:

[0052] Step 1) Add 5 portions of monolayer V2C powder to 50 mL of tetrahydrofuran and stir magnetically for 1 h at room temperature to obtain the first mixed solution;

[0053] Step 2) The first mixed solution obtained in Step 1) is ultrasonically dispersed for 2 min, and 0.5 mL of trimethoxy(1H,1H,2H,2H-heptadecyl)silane is added under stirring. The mixture is reacted at 35 °C for 24 h to obtain the second mixed solution.

[0054] Step 3) Add 240 parts of EP and 240 parts of EP curing agent, 300 parts of PDMS and 30 parts of PDMS curing agent to the second mixed solution obtained in step 2) to obtain the third mixed solution;

[0055] Step 4) The third mixed solution obtained in step 3) is mechanically stirred at a rate of 400 rpm for 20 min while simultaneously heating to 80°C until the porous material is formed.

[0056] Step 5): The porous material obtained in step 4) is vacuum dried in a vacuum drying oven at 80°C until the quality of the porous material no longer changes, thus obtaining the MXene / epoxy resin porous material for oil-water separation.

[0057] like Figure 1 As shown in the scanning electron microscope images of the MXene / epoxy resin porous material for oil-water separation prepared in Example 1, the MXene / epoxy resin porous material for oil-water separation contains various open cavities. Different cavities can provide different functions. For example, cavities with smaller openings provide retention capacity, meaning that the MXene / epoxy resin porous material for oil-water separation has a better retention capacity for the adsorbed organic solvents or fuels when it is removed from organic solvents or fuels. On the other hand, cavities with larger openings provide greater adsorption force for the MXene / epoxy resin porous material for oil-water separation to adsorb organic solvents or fuels, thereby enabling the MXene / epoxy resin porous material for oil-water separation to adsorb organic solvents or fuels more quickly.

[0058] The true density of the MXene / epoxy resin porous materials for oil-water separation prepared in Examples 1 to 4 is 0.1 g / cm³. 3 The prepared MXene / epoxy resin porous material for oil-water separation was tested for its oil absorption performance. The results showed that the MXene / epoxy resin porous material for oil-water separation has a high oil absorption ratio for organic solvents and fuel oil. Figure 2 As shown, the adsorption of silicone oil by the MXene / epoxy resin porous material for oil-water separation prepared in Example 1 was tested. Xenon lamp irradiation effectively accelerated the adsorption of silicone oil by the MXene / epoxy resin porous material for oil-water separation. Figure 3 As shown.

[0059] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of the claims of this patent application.

Claims

1. A porous MXene / epoxy resin material for oil-water separation, characterized in that, It is composed of the following components: 3-10 parts by weight of MXene, 50-100 parts by weight of hydrophobic modifier, 100-800 parts by weight of epoxy resin, 100-800 parts by weight of epoxy resin curing agent, 100-500 parts by weight of polydimethylsiloxane, and 10-50 parts by weight of polydimethylsiloxane curing agent; the MXene / epoxy resin porous material for oil-water separation contains various open cavities and has a true density of 0.1 g / cm³. 3 Various types of open cavities include cavities with small openings and cavities with large openings; the MXene / epoxy resin porous material for oil-water separation is prepared by the following steps: Step 1) Add monolayer MXene powder to 50 mL of polar organic solvent and stir magnetically at room temperature for 0.5–1.5 h to obtain the first mixed solution; Step 2) Disperse the first mixed solution obtained in Step 1) ultrasonically for 2-5 minutes, add a hydrophobic modifier while stirring, and react at 25℃-35℃ for 24 hours to obtain the second mixed solution; Step 3) Add epoxy resin and epoxy resin curing agent, polydimethylsiloxane and polydimethylsiloxane curing agent to the second mixed solution obtained in step 2) to obtain the third mixed solution; Step 4) The third mixed solution obtained in step 3) is mechanically stirred at a rate of 350 rpm to 450 rpm for 15 to 30 minutes while simultaneously heating to 66 to 85°C until the porous material is formed; wherein, as the solvent evaporates, the solvent bubbles formed by the epoxy resin, epoxy resin curing agent, polydimethylsiloxane and polydimethylsiloxane curing agent rupture one by one and form cavities, thereby forming a porous material with residual solvent; Step 5) The porous material obtained in step 4) is vacuum dried in a vacuum drying oven at 66℃~85℃ until the quality of the porous material no longer changes, and the MXene / epoxy resin porous material for oil-water separation is obtained.

2. The MXene / epoxy resin porous material for oil-water separation according to claim 1, characterized in that, The MXene is one or more of Ti3C2, V2C, V4C3, Mo2TiC2, Mo2C, and Ta4C3.

3. The MXene / epoxy resin porous material for oil-water separation according to claim 1, characterized in that, The polar organic solvent is one of tetrahydrofuran, ethyl acetate, dichloromethane, chloroform, and cyclohexane.

4. The MXene / epoxy resin porous material for oil-water separation according to claim 1, characterized in that, The hydrophobic modifier is one of trimethoxy(1H,1H,2H,2H-heptadecylfluorodecyl)silane, octadecyltrichlorosilanemethyl, and trimethoxysilane.

5. The MXene / epoxy resin porous material for oil-water separation according to claim 1, characterized in that, The epoxy resin is one of epoxy resin E44 and epoxy resin E51.

6. The MXene / epoxy resin porous material for oil-water separation according to claim 1, characterized in that, The curing agent for the epoxy resin is one of aliphatic polyamines, aromatic polyamines, and low molecular weight polyamide resins.

7. The MXene / epoxy resin porous material for oil-water separation according to claim 1, characterized in that, The curing agent for the polydimethylsiloxane is butyl diphenylcarbamate or a silanol having a vinyl structure.

8. The MXene / epoxy resin porous material for oil-water separation according to claim 1, characterized in that, The curing agent for the polydimethylsiloxane is dimethylvinylsilanol.

9. The method for preparing the MXene / epoxy resin porous material for oil-water separation according to claim 1, characterized in that, Includes the following steps: Step 1) Add monolayer MXene powder to 50 mL of polar organic solvent and stir magnetically at room temperature for 0.5–1.5 h to obtain the first mixed solution; Step 2) Disperse the first mixed solution obtained in Step 1) ultrasonically for 2-5 minutes, add a hydrophobic modifier while stirring, and react at 25℃-35℃ for 24 hours to obtain the second mixed solution; Step 3) Add epoxy resin and epoxy resin curing agent, polydimethylsiloxane and polydimethylsiloxane curing agent to the second mixed solution obtained in step 2) to obtain the third mixed solution; Step 4) The third mixed solution obtained in step 3) is mechanically stirred at a rate of 350 rpm to 450 rpm for 15 to 30 minutes while simultaneously heating to 66 to 85°C until the porous material is formed; wherein, as the solvent evaporates, the solvent bubbles formed by the epoxy resin, epoxy resin curing agent, polydimethylsiloxane and polydimethylsiloxane curing agent rupture one by one and form cavities, thereby forming a porous material with residual solvent; Step 5) The porous material obtained in step 4) is vacuum dried in a vacuum drying oven at 66℃~85℃ until the quality of the porous material no longer changes, and the MXene / epoxy resin porous material for oil-water separation is obtained.

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