Preparation method of modified funnel

By constructing low surface free energy microparticles on the surface of the sand core, the problems of complex preparation steps, high cost and poor durability of existing hydrophobic materials are solved, and efficient oil-water separation and a modification funnel that broadens the application range are achieved.

CN119075423APending Publication Date: 2024-12-06SHANGHAI ERSHIYE CONSTR CO LTD +2
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Patent Information

Application Number
CN202411167418.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-08-23
Publication Date
2024-12-06

AI Technical Summary

Technical Problem

The existing hydrophobic materials have complex preparation steps, high cost and poor durability. The reduction in the pore size of the sand core after modification leads to a reduced separation efficiency, making it difficult to meet the needs of large-scale applications.

Method used

Using eco-inorganic nano-superhydrophobic materials prepared based on polysilicon materials, low surface free energy microparticles are constructed on the surface of the sand core through simple processing operations, forming a microscopic plush structure similar to the surface of 'loose leaves', combined with orthosiliic acid Compounds such as ethyl ester, dopamine hydrochloride and fluorosilane are ultrasonic and stirred to form a modified funnel, avoiding hole blockage and improving mechanical strength and chemical stability.

Benefits of technology

It achieves efficient oil-water separation, with high mechanical strength, acid corrosion resistance, good hydrophobicity and economic benefits. It is suitable for environmental water treatment, oil-water separation and emulsion separation, and broadens the application range of sand core funnel.

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Abstract

The invention relates to a preparation method of a modified funnel, which basically does not cause blockage when a sand core is modified, and meanwhile, the subsequent organic reagent washing step can effectively prevent excessive crosslinking of organosilanized nanoparticles and effectively prevent the reduction of the radius of a sand core hole. According to different types of modified sand core funnels, the oil-water separation sand core funnel with the adjustable aperture can be obtained to meet different separation requirements, the application range of the sand core funnel is greatly widened, and the oil-water separation sand core funnel can be applied to the fields of environmental water treatment, oil-water separation, emulsion separation and the like and has good economic benefit prospects.
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Description

Technical Field

[0001] The invention belongs to the field of filtering materials, and particularly relates to a preparation method of a modified funnel. Background Art

[0002] The hydrophobicity of the surface of an object can be achieved mainly in two ways: one is to construct a rough surface, and the other is to modify the surface with a chemical substance (such as a silicon compound) with low surface free energy. In recent years, a large number of works have reported methods for synthesizing hydrophobic materials based on this. For example, Jiang Lei et al. prepared a porous microsphere / nanofiber composite membrane by electrohydrodynamics to imitate the biological functions of lotus leaves such as self-cleaning and aquatic high load (Angew.Chem., Int.Ed.2004,43,4338-4341). Wang Fajun et al. prepared a super-hydrophobic silver-coated copper mesh with a water contact angle of 164.1° by immersion method (ChemPhysChem2015,16,2237-2243). However, due to complex steps, high cost, poor mechanical durability and chemical stability, the application of such hydrophobic materials is greatly limited. It is necessary to find a hydrophobic material with excellent durability performance to meet the urgent requirements in applications.

[0003] The sand core funnel is a filtering device that can achieve solid-liquid separation. It is widely used in instrumental analysis, chemical synthesis, and environmental testing. The filter element is a sand core sintered from high-quality boron glass powder. It has strong physical and chemical properties and can withstand acidic treatment. The high-boron silicon oxide material based on the sand core contains a large number of hydroxyl structures on its surface, which is highly hydrophilic and not selective when separating liquids. The sand core filter plate has a wide range of pore size distribution, ranging from hundreds to thousands of microns to less than 1 micron. The surface itself has a certain degree of roughness, which is very suitable for hydrophobic modification.

[0004] The following technical difficulties are currently present in the preparation of hydrophobic surface on silicon dioxide surface: the existing preparation of hydrophobic silica-based material method steps are complicated, the early material construction is complicated, the post-processing process is relatively cumbersome, the production cost is high, and the possibility of large-scale application is very small. Importantly, the original situ hydrophobic modified sand core funnel can cause the reduction of sand core pore size, cause the blocking of sand core, reduce separation efficiency, and affect the application of sand core funnel. In order to expand the application of sand core funnel in separating liquid, the sand core material is hydrophobically modified with ecological inorganic nano super hydrophobic material, and the modified sand core surface water contact angle reaches more than 120 ° and the oil contact angle is less than 15 °, which can achieve a good oil-water separation effect, and can achieve efficient water-oil separation under the operating conditions of vacuum filtration.

[0005] There is a method for preparing a hydrophobic sand core material, 201810878474.4. This method uses an organic silane reagent atmosphere to modify the sand core material, so that the organic silane reagent is deposited on the surface of the sand core material to form a hydrophobic silane coating. It specifically includes the following steps: adding an organic silane reagent to a container, and then placing the sand core material in a container, heating the sealed container, gasifying the organic silane reagent and fully contacting and reacting with the sand core material to obtain a hydrophobic sand core material. This method can effectively increase the contact angle of the sand core funnel, but the sand core material is rich in micron pores. Due to the capillary effect, the organic silane vapor has a lower vapor pressure at the pores and is easily condensed into liquid droplets, resulting in blockage of the pores. It is less suitable for sand core holes with small pores. Summary of the invention

[0006] In view of the defects of the prior art, the technical problem to be solved by the present invention is to provide a method for preparing a modified funnel, and in particular to a method for preparing an oil-water separation sand core funnel based on ecological inorganic nano super hydrophobic material.

[0007] The ecological inorganic nano super hydrophobic material used in the present invention is an ecological inorganic nano material prepared from active substances mainly composed of polysilicon materials. It can be easily processed with the target device to efficiently construct low surface free energy micron particles on the surface of various substances, forming a microscopic plush structure similar to the surface of a "lotus leaf", which has extremely high hydrophobic properties, chemical stability and durability.

[0008] The present invention provides a method for preparing a modified funnel, comprising:

[0009] (1) mixing water and an organic solvent, adjusting the pH, ultrasonically dispersing and / or stirring, adding tetraethyl orthosilicate, and ultrasonically dispersing and / or stirring to obtain a first solution;

[0010] (2) mixing dopamine hydrochloride and a buffer solution, ultrasonicating, and stirring to obtain a second solution;

[0011] (3) mixing the first solution, the second solution and fluorosilane or perfluorocarboxylic acid, stirring and / or ultrasonicating to obtain a mixed solution;

[0012] (4) Pour the mixed solution of step (3) into a funnel for suction filtration, then wash with an organic solvent, dry, and anneal to obtain a modified funnel.

[0013] Preferably, the organic solvent in steps (1) and (4) is one or more of aromatic hydrocarbons, aliphatic hydrocarbons, alicyclic hydrocarbons, halogenated hydrocarbons, alcohols, ethers, esters, and ketones;

[0014] Preferably, the aromatic hydrocarbon organic solvent includes one or more of benzene, toluene, and xylene; the aliphatic hydrocarbon organic solvent includes one or more of pentane, hexane, and octane; the alicyclic hydrocarbon organic solvent includes one or more of cyclohexane, cyclohexanone, toluene, and cyclohexanone; the halogenated hydrocarbon organic solvent includes one or more of chlorobenzene, dichlorobenzene, and dichloromethane; the alcohol organic solvent includes one or more of methanol, ethanol, and isopropanol; the ether organic solvent includes one or more of ether and propylene oxide; the ester organic solvent includes one or more of methyl acetate, ethyl acetate, and propyl acetate; the ketone organic solvent includes one or more of acetone, methyl butyl ketone, and methyl isobutyl ketone.

[0015] Preferably, in step (1), the volume ratio of water, organic solvent and tetraethyl orthosilicate is (10-20):(50-90):(3-5); the water is ultrapure water or deionized water;

[0016] Preferably, in step (1), adjusting the pH is to 7.8-9 using a base; wherein the base is at least one of sodium hydroxide and ammonia water, wherein the concentration of sodium hydroxide is 0.3%-0.4% (mass fraction), and the concentration of ammonia water is 25-28% (volume fraction);

[0017] Preferably, after adjusting the pH in step (1), ultrasonic dispersion is performed for 10-30 min and / or stirring is performed at room temperature for 20-40 min, and then ethyl orthosilicate is added and ultrasonic dispersion is performed for 0.5-1 h and / or stirring is performed at 15-50° C. for 6-12 h.

[0018] Preferably, in the step (2), the ratio of dopamine hydrochloride to buffer is (100-250 mg):50 mL; the buffer is Tris-HCl buffer, and the pH of the buffer is 7.8-9; the ultrasonic time is 5-30 min; and the stirring is stirring at room temperature for 12-24 h.

[0019] The Tris-HCl buffer solution is prepared by fully stirring and mixing tris(hydroxymethyl)aminomethane and water, and adding concentrated hydrochloric acid to adjust the pH to 7.8-9, wherein the mass ratio of tris(hydroxymethyl)aminomethane to water is 1:500-900; the water is ultrapure water or deionized water; the concentration of the concentrated hydrochloric acid is 1 mol / L; the stirring temperature is room temperature, and the stirring time is 30-60 min.

[0020] Preferably, in the step (3), the volume ratio of the first solution to the second solution is (1-1.5):1; the volume ratio of the fluorosilane or perfluorocarboxylic acid to ethyl orthosilicate is 1:(1-3); the fluorosilane is one or more of perfluorooctyltrimethylsilane, 1H, 1H, 2H, 2H perfluorododecyltriethoxysilane, tridecafluorooctylsilane, and heptadecafluorodecylsilane; the perfluorocarboxylic acid includes one or more of perfluorobutyric acid, perfluoropentanoic acid, perfluorohexanoic acid, perfluoroheptanoic acid, and perfluorooctanoic acid.

[0021] Preferably, in step (3), the first solution and the second solution are mixed and stirred, and then fluorosilane is added for stirring and / or ultrasonication to obtain a mixed solution; wherein the first solution and the second solution are mixed and stirred at a temperature of 35-50°C and a stirring time of 12-24 hours. Further, fluorosilane is added for stirring and / or ultrasonication, wherein the stirring is at 10-50°C for 2-10 hours and the ultrasonication time is 20-40 minutes.

[0022] Preferably, the funnel in step (4) is a sand core funnel; the filtration is reduced pressure filtration, and the negative pressure range is 5-30Pa; the washing is filtration washing, wherein the filtration is normal pressure filtration; the volume ratio of the sand core of the funnel to the mixed solution is 1:(3-5); the volume ratio of the sand core to the organic solvent is 1:(5-30).

[0023] Furthermore, in step (4), the sand core funnel has a specification of at least one of G1, G2, G3, and G4.

[0024] The funnel in step (4) comprises two components: a sand core filter plate and a glass funnel body, wherein the sand core filter plate is a sheet-like cylinder fixed on the glass funnel by sintering, the upper part of the glass funnel body is cylindrical, the sand core filter plate is located above the closing part, and the smaller tubular part of the funnel mouth can have an air pipe interface for decompression filtration.

[0025] The funnel is an oil-water separation sand core funnel.

[0026] Preferably, in the step (4), the drying temperature is 40-120° C. and the time is 2-12 h; the annealing is annealing under a protective atmosphere, wherein the annealing temperature is 200-350° C. and the time is 3-6 h; wherein the protective atmosphere is one or more of nitrogen, helium, argon, neon, and krypton.

[0027] The invention provides a modified funnel prepared by the method.

[0028] The invention provides an application of the modified funnel in the fields of environmental water treatment, oil-water separation and emulsion separation.

[0029] The present invention uses a nano super hydrophobic agent to modify a sand core material to prepare an oil-water separation sand core funnel. The particle size of the organic silanized nanoparticles in the dispersion used is 70-100nm, which is much smaller than the pore size of the G5 sand core funnel of 2-5μm, and basically does not cause blockage. At the same time, the subsequent organic reagent flushing step can effectively prevent excessive cross-linking of the organic silanized nanoparticles and effectively prevent the reduction of the radius of the sand core hole. The method is simple and fast, has a relatively low cost, can withstand a high water content in the emulsion, and has high mechanical strength, acid corrosion resistance, high durability, and has both solid-liquid separation and oil-water separation capabilities, and can be used as a hydrophobic oil-water separation material.

[0030] Beneficial Effects

[0031] In the prior art, the preparation of hydrophobic surface on the surface of silica has the following technical difficulties: the existing modification method has complicated steps, the material precursor preparation is complicated, the production cost is expensive, and it is difficult to put into large-scale actual production. At the same time, since the glass sand core needs to be prepared at high temperature, it will destroy the hydrophobic precursor, so it needs post-processing modification. Compared with the prior art, the method of the present invention is simple in process, low in cost, and does not require any expensive equipment. The hydrophobic modified sand core funnel obtained according to the method of the present invention has good hydrophobicity, and the water contact angle can reach 120°-150°. At the same time, it has high mechanical strength, acid corrosion resistance, high durability, and both solid-liquid separation and oil-water separation capabilities, and can be used as a hydrophobic oil-water separation material. While the method basically does not cause blockage when modifying the sand core, the subsequent organic reagent rinsing step can effectively prevent excessive cross-linking of organic silanized nanoparticles and effectively prevent the reduction of the radius of the sand core holes. By modifying different types of sand core funnels, an oil-water separation sand core funnel with adjustable pore size can be obtained to meet different separation needs, which greatly broadens the application scope of the sand core funnel. It can be used in environmental water treatment, oil-water separation, emulsion separation and other fields, and has good economic benefit prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 The invention discloses an oil-water separation sand core funnel structure based on ecological inorganic nano super hydrophobic material, wherein 1 is a glass funnel body, 2 is a sand core filter plate, and 3 is an air pipe interface for decompression filtration. DETAILED DESCRIPTION

[0033] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall within the scope limited by the appended claims of the application equally.

[0034] Example 1

[0035] Mix 10mL of deionized water and 50mL of ethanol, add 25% ammonia water to adjust the pH to 7.8, ultrasonically disperse for 20min, and stir at 600r / min for 20min at room temperature. Then add 3mL of tetraethyl orthosilicate, ultrasonically disperse for 1h, and stir at 600r / min for 6h at 35℃ to obtain the first solution. Mix 100mg of trishydroxymethylaminomethane with 65mL of deionized water, add 1mol / L concentrated hydrochloric acid to adjust the pH to 7.8, ultrasonically disperse for 30min, and stir at 600r / min for 30min at room temperature to obtain TrisHCl buffer. Mix 150mg of dopamine hydrochloride with 50mL of Tris-HCl solution, ultrasonically disperse for 5min, and then stir at 600r / min for 12h at room temperature to obtain the second solution. Mix 15mL of the first solution with 10mL of the second solution, and stir at 1500r / min for 12h at 35℃ to obtain the third solution. 0.7 mL of perfluorooctyltrimethylsilane was added to the third solution, stirred at 1500 r / min for 6 h at 35 ° C, and then ultrasonicated for 30 min to obtain the fourth solution. 30 mL of the fourth solution was poured into the G1 sand core funnel and filtered under a low pressure of 15 Pa to obtain the first sand core funnel. The first sand core funnel was rinsed with ethyl acetate in small amounts for multiple times, and 200 mL of ethyl acetate was used to obtain the second sand core funnel. The second sand core funnel was placed in a blast oven and dried at 120 ° C for 3 h to obtain the third sand core funnel. The third sand core funnel was placed in a muffle furnace and annealed at 220 ° C for 3 h under the protection of 80 mL / min nitrogen atmosphere to obtain a hydrophobic G1 sand core funnel that can be used for oil-water separation.

[0036] Example 2

[0037] Mix 10mL ultrapure water and 60mL acetone, add 28% ammonia water to adjust the pH to 8, ultrasonically disperse for 20min, and stir at 500r / min for 20min at room temperature. Then add 3mL of tetraethyl orthosilicate, ultrasonically disperse for 1h, and stir at 500r / min for 6h at 15℃ to obtain the first solution. Mix 100mg of trishydroxymethylaminomethane with 80mL of deionized water, add 1mol / L concentrated hydrochloric acid to adjust the pH to 7.8, ultrasonically disperse for 30min, and stir at 600r / min for 30min at room temperature to obtain Tris HCl buffer. Mix 150mg of dopamine hydrochloride with 50mL of Tris-HCl solution, ultrasonically disperse for 5min, and then stir at 600r / min for 12h at room temperature to obtain the second solution. Mix the first solution and the second solution in a volume ratio of 15mL:10mL, and stir at 1500r / min for 15h at 15℃ to obtain the third solution. Add 0.6 mL of perfluorobutyric acid to the third solution, stir in a sealed state at 15 ° C for 8 hours, and then ultrasonicate for 40 minutes to obtain the fourth solution. Add 15 mL of the fourth solution dropwise into the G4 sand core funnel, and filter under reduced pressure at a low pressure of 20 Pa to obtain the first sand core funnel. Ultrasonicate the first sand core funnel with ethanol for 5 minutes, then add a small amount of ethanol to rinse multiple times, and use 45 mL of ethanol to obtain the second sand core funnel. Place the second sand core funnel in a blast oven and dry it at 120 ° C for 2 hours to obtain the third sand core funnel. Place the third sand core funnel in a muffle furnace and anneal it at 250 ° C for 5 hours under the protection of 100 mL / min argon atmosphere to obtain a hydrophobic G4 sand core funnel that can be used for oil-water separation.

[0038] Example 3

[0039] Mix 15mL ultrapure water and 50mL isopropanol, add 28% ammonia water to adjust the pH to 7.8, ultrasonically disperse for 10min, and stir at 100r / min for 10min at room temperature. Then add 3.5mL of tetraethyl orthosilicate, ultrasonically disperse for 1h, and stir at 100r / min for 6h at room temperature to obtain the first solution. Mix 100mg of trishydroxymethylaminomethane with 75mL of deionized water, add 1mol / L concentrated hydrochloric acid to adjust the pH to 7.8, ultrasonically disperse for 1h, and stir at 500r / min for 30min at room temperature to obtain Tris HCl buffer. Mix 150mg of dopamine hydrochloride with 50mL of Tris-HCl solution, ultrasonically disperse for 5min, and then stir at 500r / min for 12h at room temperature to obtain the second solution. Mix the first solution and the second solution in a volume ratio of 10mL:10mL, reflux and stir at 1500r / min at 70℃ for 5h to obtain the third solution. Add 0.5 mL of perfluorobutyric acid to the third solution cooled to room temperature, stir at room temperature for 6 hours, and then ultrasonicate for 30 minutes to obtain the fourth solution. Add 30 mL of the fourth solution dropwise into the G2 sand core funnel, and filter under reduced pressure at a low pressure of 15 Pa to obtain the first sand core funnel. After the first sand core funnel is allowed to stand at room temperature for 15 minutes, add a small amount of ethanol to rinse it several times, and use 15 mL of ethanol to obtain the second sand core funnel. Place the second sand core funnel in a blast oven and dry it at 100 ° C for 3 hours to obtain the third sand core funnel. Place the third sand core funnel in a muffle furnace and anneal it at 200 ° C for 6 hours under the protection of a 50 mL / min helium atmosphere to obtain a hydrophobic G2 sand core funnel that can be used for oil-water separation.

[0040] Comparative Example 1

[0041] Mix 200mL of deionized water and 400mL of ethanol, add 28% ammonia water to adjust the pH to 7.8, and stir at room temperature for 20min. Then add 30mL of tetraethyl orthosilicate and stir at 35℃ for 6h to obtain the first solution. Add 30mL of perfluorooctyltrimethylsilane to the first solution, ultrasonicate for 30min, and stir at room temperature for 6h to obtain the second solution. Pour 30mL of the second solution into the G1 sand core funnel, and filter under reduced pressure at a low pressure of 15Pa to obtain the first sand core funnel. After the first sand core funnel is left at room temperature for 15min, add a small amount of ethanol to rinse it several times, and use 15mL of ethanol to obtain the second sand core funnel. Place the second sand core funnel in a blast oven and dry it at 150℃ for 3h to obtain the third sand core funnel. Place the third sand core funnel in a muffle furnace and anneal it at 250℃ for 6h under the protection of a 100mL / min nitrogen atmosphere to obtain a hydrophobic G1 sand core funnel for comparison.

[0042] Comparative Example 2

[0043] Mix 200mL of deionized water and 400mL of ethanol, add 28% ammonia water to adjust the pH to 8.5, and stir at room temperature for 30min. Then add 40mL of tetraethyl orthosilicate and stir at 45℃ for 10h to obtain the first solution. Add 40mL of perfluorooctyltrimethylsilane to the first solution, ultrasonicate for 50min, and stir at 45℃ for 20h to obtain the second solution. Pour 30mL of the second solution into the G2 sand core funnel, and filter under reduced pressure at a low pressure of 15Pa to obtain the first sand core funnel. After the first sand core funnel is left at room temperature for 15min, add a small amount of ethanol to rinse it several times, and use 15mL of ethanol to obtain the second sand core funnel. Place the second sand core funnel in a blast oven and dry it at 150℃ for 3h to obtain the third sand core funnel. Place the third sand core funnel in a muffle furnace and anneal it at 250℃ for 6h under the protection of a 100mL / min nitrogen atmosphere to obtain a hydrophobic G2 sand core funnel for comparison.

[0044] The hydrophobic sand core funnels prepared in Examples 1-3 and Comparative Examples 1-2 were respectively:

[0045] Hydrophobic performance test: Use a contact angle meter to measure the contact angle using the height method, angle method and curve fitting method. The contact angle is used to characterize the hydrophobic and oleophilic properties. The pump-free flow rate of dichloromethane per unit area of ​​the hydrophobic sand core is used to characterize the oil permeability.

[0046] The test results are shown in the following table:

[0047]

[0048] It can be seen from the table that the hydrophobic sand core funnel for oil-water separation prepared in this embodiment has good hydrophobicity and lipophilicity, and can achieve oil-water separation operation with high efficiency.

Claims

1. A method for preparing a modified funnel, comprising: (1) mixing water and an organic solvent, adjusting the pH, ultrasonically dispersing and / or stirring, adding tetraethyl orthosilicate, and ultrasonically dispersing and / or stirring to obtain a first solution; (2) mixing dopamine hydrochloride and a buffer solution, ultrasonicating, and stirring to obtain a second solution; (3) mixing the first solution, the second solution and fluorosilane or perfluorocarboxylic acid, stirring and / or ultrasonicating to obtain a mixed solution; (4) Pour the mixed solution of step (3) into a funnel for suction filtration, then wash with an organic solvent, dry, and anneal to obtain a modified funnel.

2. The preparation method according to claim 1, characterized in that: In the steps (1) and (4), the organic solvent is one or more of aromatic hydrocarbons, aliphatic hydrocarbons, alicyclic hydrocarbons, halogenated hydrocarbons, alcohols, ethers, esters, and ketones; The aromatic hydrocarbon organic solvents include one or more of benzene, toluene, and xylene; the aliphatic hydrocarbon organic solvents include one or more of pentane, hexane, and octane; the alicyclic hydrocarbon organic solvents include one or more of cyclohexane, cyclohexanone, toluene, and cyclohexanone; the halogenated hydrocarbon organic solvents include one or more of chlorobenzene, dichlorobenzene, and dichloromethane; the alcohol organic solvents include one or more of methanol, ethanol, and isopropanol; the ether organic solvents include one or more of ether and propylene oxide; the ester organic solvents include one or more of methyl acetate, ethyl acetate, and propyl acetate; the ketone organic solvents include one or more of acetone, methyl butyl ketone, and methyl isobutyl ketone.

3. The preparation method according to claim 1, characterized in that: In the step (1), the volume ratio of water, organic solvent and tetraethyl orthosilicate is (10-20):(50-90):(3-5); the water is ultrapure water or deionized water; The pH is adjusted to 7.8-9 by using a base; wherein the base is at least one of sodium hydroxide and ammonia water, wherein the mass percentage concentration of the sodium hydroxide is 0.3%-0.4%, and the volume percentage concentration of the ammonia water is 25-28%; After adjusting the pH, ultrasonic dispersion and / or stirring at room temperature for 20-40 min are performed, and ethyl orthosilicate is added, and ultrasonic dispersion and / or stirring at 15-50° C. is performed for 6-12 h.

4. The preparation method according to claim 1, characterized in that: In the step (2), the ratio of dopamine hydrochloride to buffer is 100-250 mg:50 mL; the buffer is Tris-HCl buffer, and the pH of the buffer is 7.8-9; the ultrasonic time is 5-30 min; and the stirring is stirring at room temperature for 12-24 h.

5. The preparation method according to claim 1, characterized in that: In the step (3), the volume ratio of the first solution to the second solution is 1-(1.5:1); the volume ratio of the fluorosilane or perfluorocarboxylic acid to tetraethyl orthosilicate is 1:(1-3); the fluorosilane is one or more of perfluorooctyltrimethylsilane, 1H, 1H, 2H, 2H perfluorododecyltriethoxysilane, tridecafluorooctylsilane, and heptadecafluorodecylsilane; the perfluorocarboxylic acid includes one or more of perfluorobutyric acid, perfluoropentanoic acid, perfluorohexanoic acid, perfluoroheptanoic acid, and perfluorooctanoic acid.

6. The preparation method according to claim 1, characterized in that: In the step (3), the first solution and the second solution are mixed and stirred, and then fluorosilane or perfluorocarboxylic acid is added and stirred and / or ultrasonicated to obtain a mixed solution; wherein the mixing and stirring temperature of the first solution and the second solution is 35-50° C., and the stirring time is 12-24 hours; Add fluorosilane and stir and / or ultrasonicate, wherein the stirring is at 10-50° C. for 2-10 hours and the ultrasonicate time is 20-40 minutes.

7. The preparation method according to claim 1, characterized in that: In the step (4), the funnel is a sand core funnel; the suction filtration is reduced pressure suction filtration; the washing is filtration washing, wherein the filtration is normal pressure filtration; the volume ratio of the sand core of the funnel to the mixed solution is 1:(3-5); the volume ratio of the sand core to the organic solvent is 1:(5-30).

8. The preparation method according to claim 1, characterized in that: In the step (4), the drying temperature is 40-120° C. and the time is 2-12 hours; the annealing is annealing under a protective atmosphere, wherein the annealing temperature is 200-350° C. and the time is 3-6 hours; wherein the protective atmosphere is one or more of nitrogen, helium, argon, neon, and krypton.

9. A modified funnel prepared by the method of claim 1.

10. Use of the modified funnel according to claim 9 in the fields of environmental water treatment, oil-water separation, and emulsion separation.

Citation Information

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