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CN-115672053-B - Super-hydrophobic fiber membrane with fold structure and preparation method thereof

CN115672053BCN 115672053 BCN115672053 BCN 115672053BCN-115672053-B

Abstract

The invention discloses a super-hydrophobic fiber membrane with a fold structure and a preparation method thereof, wherein the preparation method comprises the steps of immersing a polypropylene fiber membrane in a methanol solution of a photoinitiator; taking out, irradiating under ultraviolet lamp, immersing in methanol solution of amino monomer, irradiating under ultraviolet lamp, immersing in n-hexane solution of acyl chloride, taking out, immersing in methanol solution of hydroxy monomer for interfacial polymerization, taking out, drying, immersing in n-hexane solution of long-chain alkyl chlorosilane, taking out, and drying to obtain the superhydrophobic fibrous membrane with surface having fold structure. The method is simple and feasible, has mild conditions, does not need precise instruments, and has high separation speed, high efficiency and good reusability. The fiber membrane surface fold structure is used for separating the water-in-oil emulsion containing the surfactant, so that the contact area between the super-hydrophobic surface and the emulsion can be increased, the coalescence and demulsification of the micro-emulsion are promoted, and the water retention rate can reach more than 99%.

Inventors

  • ZHANG JINLI
  • WANG YIFEI
  • YANG LIN
  • LI WEI

Assignees

  • 天津大学
  • 物质绿色创造与制造海河实验室

Dates

Publication Date
20260505
Application Date
20221118

Claims (7)

  1. 1. The preparation method of the super-hydrophobic fiber membrane with the fold structure is characterized by comprising the following steps of: (1) Soaking the polypropylene fiber membrane in methanol solution of photoinitiator in concentration of 0.1-10wt% for 1-12 hr, taking out, and irradiating under ultraviolet lamp for 1-3 min; (2) Immersing the fiber membrane obtained in the step (1) into a methanol solution of an amino monomer containing double bonds, the concentration of which is 0.5-5 wt%, irradiating for 3-15 min under an ultraviolet lamp, taking out, immersing into an n-hexane solution of acyl chloride, the concentration of which is 0.01-0.5 wt%, for 3-10 min, taking out, immersing into a methanol solution of a hydroxyl monomer, the concentration of which is 0.1-1 wt%, for 3-10 min, performing interfacial polymerization, taking out, and drying; (3) Soaking the fiber membrane obtained in the step (2) in n-hexane solution of long-chain alkyl chlorosilane with the concentration of 0.1-5 wt% for 6-12h, taking out, and drying to obtain the super-hydrophobic fiber membrane with the surface having a fold structure; the acyl chloride is trimesoyl chloride, terephthaloyl chloride or isophthaloyl chloride; the long-chain alkyl chlorosilane is octyl trichlorosilane, decyl trichlorosilane, dodecyl trichlorosilane and octadecyl trichlorosilane.
  2. 2. The method according to claim 1, wherein the polypropylene fiber membrane has a pore size of 0.1 μm to 10. Mu.m.
  3. 3. The method of claim 1, wherein the photoinitiator is benzophenone, 4-methylbenzophenone, 2, 4-dihydroxybenzophenone, 4' -bis (N, N-dimethylamino) benzophenone, or 2-isopropylthioxanthone.
  4. 4. The method according to claim 1, wherein the double bond-containing amine-based monomer is N-methylallylamine, diallylamine, 5-hexene-1-amine or 4-pentene-1-amine.
  5. 5. The method of claim 1, wherein the hydroxy monomer is 3, 4-dihydroxybenzoic acid, 4-amino-3-hydroxybenzoic acid, 4-hydroxybenzoic acid, salicylic acid, or aminosalicylic acid.
  6. 6. A superhydrophobic fibrous membrane having a pleated structure prepared by the method of any of claims 1-5.
  7. 7. The application of the super-hydrophobic fiber membrane with the fold structure in oil-water separation.

Description

Super-hydrophobic fiber membrane with fold structure and preparation method thereof Technical Field The invention belongs to the field of preparation of super-hydrophobic fiber membranes, and particularly relates to a super-hydrophobic fiber membrane with a fold structure, a preparation method and application thereof in oil-water separation. Background With the continuous expansion of the scale of industrial production, the oil-water emulsion produced in the industries of petroleum exploitation, chemical industry, pharmacy and the like can cause resource waste and adverse effect on the environment and human health without oil-water separation treatment. Therefore, how to efficiently separate and recover the emulsified product has attracted a great deal of attention. The traditional oil-water separation technology comprises a gravity separator, an oil skimming device, flotation and the like, has the defects of low efficiency, high energy consumption, large occupied area and the like, and has an unsatisfactory separation effect on water-in-oil emulsion with the diameter smaller than 20 mu m. In recent years, special wettability of the surface of the superhydrophobic material has attracted a great deal of attention. The contact angle of the super-hydrophobic surface to water drops is larger than 150 degrees, and the rolling angle is smaller than 10 degrees, so that the super-hydrophobic surface has great application value in the field of oil-water separation due to the special selectivity of the super-hydrophobic surface to oil and water. The super-hydrophobic material can be prepared by regulating and controlling the micro-nano structure and the surface energy of the solid surface. Chinese patent CN108939952a discloses a preparation method of super-hydrophobic fiber membrane, which comprises preparing nanofiber membrane by electrostatic spinning, then spraying, depositing, ultraviolet irradiating, polymerizing to obtain polyaniline micro-nano particles, loading on the surface of the fiber membrane, and further performing surface etching to obtain the super-hydrophobic nanofiber membrane for oil-water separation. The technology has the defects of complicated preparation process and expensive use equipment. Chinese patent CN104988737a discloses a method for preparing super-hydrophobic textile, which comprises immersing polyester fiber fabric in different buffer solutions, depositing nanoparticles generated by dopamine polymerization on the surface of fiber adhered with polydopamine, and treating the fiber with fluorine-containing low surface energy modifier to obtain super-hydrophobic textile. The technology has the defects of fluorine-containing raw materials and poor product stability. Disclosure of Invention The invention aims to overcome the defects of the prior art and provides a super-hydrophobic fiber membrane with a fold structure. The second object of the present invention is to provide a method for preparing a superhydrophobic fibrous membrane having a pleated structure. The third object of the invention is to provide an application of the super-hydrophobic fiber membrane with the fold structure in oil-water separation. The technical scheme of the invention is summarized as follows: a preparation method of a super-hydrophobic fiber membrane with a fold structure comprises the following steps: (1) Soaking the polypropylene fiber membrane in methanol solution of photoinitiator in concentration of 0.1-10wt% for 1-12 hr, taking out, and irradiating under ultraviolet lamp for 1-3 min; (2) Immersing the fiber membrane obtained in the step (1) into a methanol solution of an amino monomer with the concentration of 0.5-5 wt%, irradiating for 3-15 min under an ultraviolet lamp, taking out, immersing into an n-hexane solution of acyl chloride with the concentration of 0.01-0.5 wt% for 3-10 min, taking out, immersing into a methanol solution of a hydroxyl monomer with the concentration of 0.1-1 wt% for 3-10 min, performing interfacial polymerization, taking out, and drying; (3) Soaking the fiber membrane obtained in the step (2) in n-hexane solution of long-chain alkyl chlorosilane with the concentration of 0.1-5 wt% for 6-12h, taking out, and drying to obtain the super-hydrophobic fiber membrane with the surface having the fold structure. Preferably, the polypropylene fiber membrane is a polypropylene fiber membrane having a pore size of 0.1 μm to 10. Mu.m. Preferably, the photoinitiator is benzophenone, 4-methylbenzophenone, 2, 4-dihydroxybenzophenone, 4' -bis (N, N-dimethylamino) benzophenone or 2-isopropylthioxanthone. Preferably, the amine-based monomer is N-methylallylamine, diallylamine, 5-hexen-1-amine or 4-penten-1-amine. Preferably, the acid chloride is trimesoyl chloride, terephthaloyl chloride or isophthaloyl chloride. Preferably, the hydroxy monomer is 3, 4-dihydroxybenzoic acid, 4-amino-3-hydroxybenzoic acid, 4-hydroxybenzoic acid, salicylic acid or aminosalicylic acid. Preferably, the long chain al