CN109666253B - Preparation method of underwater super-oleophobic microgel/fiber composite material - Google Patents
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Abstract
The invention relates to a preparation method of a microgel/fiber composite material with underwater super-oleophobic property, which comprises the following steps: preparing a first monomer solution from a first monomer, a cross-linking agent and an initiator; thermally initiating polymerization to form a first monomer hydrogel; then, drying the first monomer hydrogel and grinding the dried first monomer hydrogel into microgel particles; preparing a second monomer solution from a second monomer, a cross-linking agent and an initiator; preparing a mixed solution from the microgel particles and a second monomer solution; and finally pouring the mixed solution on two sides of the fiber woven mesh substrate, and carrying out thermal initiation polymerization to obtain the microgel/fiber composite material. The surface of the microgel/fiber composite material obtained by the method has a micro-nano composite coarse structure, so that the microgel/fiber composite material has excellent underwater super-oleophobic property and oil adhesion resistance. Meanwhile, the composite structure of the double-network micro-gel layer and the fiber substrate enables the material to have high mechanical strength, and can be applied to the fields of ship antifouling shells, bridge underwater antifouling and the like.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a preparation method of an underwater super-oleophobic microgel/fiber composite material.
Background
With the increasing severity of marine oil pollution, devices and equipment such as ships, bridges and offshore drilling platforms which are soaked in seawater for a long time are corroded by the oil pollution, and phenomena such as corrosion and aging occur, so that the service life of the devices and equipment is seriously influenced. The preparation of materials with superoleophobic properties is an effective means to address this problem. Two articles, namely "facility differentiation of a super-amphiphatic coating surface with a bionic microstructure" (2004, 16, 302-. However, the fluorine-containing long-chain alkane has high toxicity and is not suitable for the practical application of marine antifouling.
Chinese patent CN101220165B takes fish scales with micro-nano structures as templates, and adopts a single network hydrogel material to prepare the underwater super oleophobic material. The material is nontoxic, but the single network structure causes the material to have poor mechanical property, which is not beneficial to practical application. On the basis, Chinese patent CN102140218B adopts fish scales and a silicon wafer with an array structure as templates to prepare a composite film of polymer and inorganic nano particles, and the composite film has better mechanical strength on the basis of keeping the underwater super oleophobic property. However, the preparation of the fish scale template and the silicon wafer template with the array structure is complex, high in cost and not beneficial to industrial production. Thus, designing a template-independent material with high mechanical strength and underwater superoleophobic properties remains a challenge.
A composite material is prepared by adopting a double-network microgel and a fiber substrate, and a surface with a micro-nano structure is formed by utilizing the structural characteristics of the microgel, so that the underwater super-oleophobic property is obtained. The double-network gel structure of the material is combined with a fiber substrate, so that the material has very high mechanical strength. The preparation method has the advantages of simple process, low cost, environmental protection by using water as a solvent and wide application prospect in the field of marine oil pollution prevention.
Disclosure of Invention
The invention aims to provide a preparation method of a microgel/fiber composite material with high strength, low cost, green and environment-friendly underwater super-oleophobic property, aiming at the defects that the current underwater super-oleophobic material has poor mechanical strength and depends on a high-cost template to obtain a micro-nano structure.
The technical scheme for solving the technical problems is as follows:
a preparation method of a microgel/fiber composite material with underwater super oleophobic property comprises the following steps:
1) dissolving a first monomer, a cross-linking agent and an initiator in water to obtain a first monomer solution, wherein the concentration of the first monomer is 0.5-3 mol/L, the concentration of the cross-linking agent is 0.005-0.03 mol/L, and the concentration of the initiator is 0.005-0.03 mol/L;
2) heating the first monomer solution obtained in the step 1) at 80-90 ℃ for 1-2 hours to obtain a first network hydrogel, mashing, drying, and grinding into microgel powder;
3) dissolving a second monomer, a cross-linking agent and an initiator in water to obtain a second monomer solution, wherein the concentration of the second monomer is 1.0-6 mol/L, the concentration of the cross-linking agent is 0.0005-0.003 mol/L, and the concentration of the initiator is 0.01-0.06 mol/L;
4) mixing the microgel powder obtained in the step 2) with the second monomer solution obtained in the step 3) to prepare a mixed solution, wherein the mass ratio of the microgel powder to the second monomer solution is controlled to be 1: (1-10);
5) and (3) uniformly coating the mixed solution obtained in the step 4) on two surfaces of the fiber woven mesh, and heating at 80-90 ℃ for 1-2 hours to obtain the microgel/fiber composite material.
Further, the first monomer in step 1) is any one or a mixture of two or more of 2-acrylamido-2-methylpropanesulfonic acid, sodium p-styrenesulfonate, acrylamide, acrylic acid and N-vinylpyrrolidone, and preferably, the first monomer is any one or a mixture of two or more of 2-acrylamido-2-methylpropanesulfonic acid, acrylamide and acrylic acid.
Further, the crosslinking agent in the step 1) is N, N-methylene bisacrylamide.
Further, the initiator in the step 1) is any one of ammonium persulfate, potassium persulfate and sodium persulfate.
Further, the particle size of the microgel powder in the step 2) is 10-800 μm.
Further, the second monomer in step 3) is any one or a mixture of two or more of 2-acrylamido-2-methylpropanesulfonic acid, sodium p-styrenesulfonate, acrylamide, acrylic acid and N-vinylpyrrolidone, and preferably, the second monomer is acrylamide.
Further, the cross-linking agent in the step 3) is N, N-methylene bisacrylamide.
Further, the initiator in the step 3) is any one of ammonium persulfate, potassium persulfate and sodium persulfate.
Further, the fiber woven mesh in the step 5) is one of a glass fiber woven mesh, a carbon fiber woven mesh, a polyester fiber woven mesh, a nylon fiber woven mesh, an acrylic fiber woven mesh, a vinylon fiber woven mesh and an aramid fiber woven mesh, and preferably, the fiber woven mesh is a glass fiber woven mesh.
Further, the mesh number of the fiber woven mesh in the step 5) is 100-500 meshes.
The preparation method of the invention has the following action principle:
the first network microgel powder has a micrometer-scale coarse structure, and swells after being mixed with the second monomer solution to generate a nanometer-scale coarse structure on the micrometer-scale structure. After the microgel/fiber composite material is coated on the surface of the fiber woven mesh substrate, the microgel/fiber composite material with a micro-nano composite structure is formed through a thermal initiation polymerization process. The micro-nano composite structure enables a stable water layer to be formed on the surface of the material after the material absorbs water underwater in a balanced manner, and the material shows stable super-oleophobic and oil adhesion resistant properties underwater. Meanwhile, a mixed solution formed by the first network microgel powder and the second network monomer solution is polymerized to form a double-network gel layer with high mechanical strength, and the obtained microgel/fiber composite material has excellent mechanical property by combining the mechanical enhancement effect of the fiber woven mesh.
The microgel/fiber composite material prepared by the method has the following structural characteristics:
1) the surface of the microgel/fiber composite material is provided with a micron-sized package block structure with the size of 10-800 mu m, and the surface of the micron-sized package block is provided with a nano-scale convex structure with the size of 30-500 nm.
2) The microgel/fiber composite material is prepared by wrapping a fiber woven mesh by a gel layer, wherein the fiber woven mesh is positioned at the position of the middle interlayer, and the thickness of the material is 100-2000 mu m.
The invention has the beneficial effects that:
1) the microgel/fiber composite material obtained by the method has a contact angle of 156-165 degrees to oil in water, and the microgel particles with the micro-nano composite structure increase the roughness of the surface of the material, so that the material has more excellent underwater super-oleophobic property and is not easy to adhere by oil.
2) The mechanical strength of the microgel/fiber composite material obtained by the method is far greater than that of the traditional gel polymer of the same type, and the microgel/fiber composite material has high tensile strength.
3) The solvent used in the preparation process of the microgel/fiber composite material obtained by the method is water, and the microgel/fiber composite material is economical and environment-friendly.
4) The microgel/fiber composite material obtained by the method does not depend on a template, the raw materials are cheap and easy to obtain, the equipment and the manufacturing process are simple, and the cost is low.
5) The microgel/fiber composite material obtained by the method has wide application prospect in the field of marine oil contamination prevention.
Drawings
FIG. 1 is an SEM photograph of the surface morphology of a microgel/fiber composite prepared in example 1;
fig. 2 is a photograph showing the shape of the surface of the microgel/fiber composite prepared in example 1, measured underwater for gasoline droplets (2 microliters).
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1:
a preparation method of a microgel/fiber composite material with underwater super oleophobic property comprises the following steps:
1) dissolving 2-acrylamide-2-methylpropanesulfonic acid, N, N-methylene bisacrylamide and ammonium persulfate in water to obtain a first monomer solution, wherein the concentration of the 2-acrylamide-2-methylpropanesulfonic acid is 0.5 mol/L, the concentration of the N, N-methylene bisacrylamide is 0.005 mol/L, and the concentration of the ammonium persulfate is 0.005 mol/L;
2) heating the first monomer solution obtained in the step 1) at 80 ℃ for 1 hour to obtain poly (2-acrylamide-2-methylpropanesulfonic acid) hydrogel, mashing, drying, and grinding into microgel powder with the size of 300-500 mu m;
3) dissolving acrylamide, N, N-methylene-bisacrylamide and ammonium persulfate in water to obtain a second monomer solution, wherein the concentration of the acrylamide is 1.0 mol/L, the concentration of the N, N-methylene-bisacrylamide is 0.0005 mol/L, and the concentration of the ammonium persulfate is 0.01 mol/L;
4) mixing the microgel powder obtained in the step 2) with the second monomer solution obtained in the step 3) to prepare a mixed solution, and controlling the mass ratio of the microgel powder to the second monomer solution to be 1:1;
5) and (3) uniformly coating the mixed solution obtained in the step 4) on two surfaces of a glass fiber woven mesh with 100 meshes, and heating at 80 ℃ for 1 hour to obtain the microgel/glass fiber composite material with the thickness of 1000 microns.
The microgel/glass fiber composite material obtained in the embodiment 1 has a micron-sized inclusion block structure with the size of 300-500 μm, and a nano-sized protrusion structure with the size of 200-300 nm on the surface of the micron-sized inclusion block (see fig. 1). The resulting microgel/glass fiber composite had a contact angle of 156 ° to gasoline underwater (see fig. 2). The mechanical strength of the microgel/glass fiber composite material is far greater than that of the traditional similar polymer, and the tensile strength is about 350 MPa.
Example 2:
a preparation method of a microgel/fiber composite material with underwater super oleophobic property comprises the following steps:
1) dissolving acrylamide, N, N-methylene-bisacrylamide and sodium persulfate in water to obtain a first monomer solution, wherein the concentration of the acrylamide is 3 mol/L, the concentration of the N, N-methylene-bisacrylamide is 0.03 mol/L, and the concentration of the sodium persulfate is 0.03 mol/L;
2) heating the first monomer solution obtained in the step 1) at 90 ℃ for 2 hours to obtain polyacrylamide hydrogel, mashing, drying, and then grinding into microgel powder with the size of 10-30 microns;
3) dissolving sodium p-styrenesulfonate, N, N-methylene bisacrylamide and sodium persulfate in water to obtain a second monomer solution, wherein the concentration of the sodium p-styrenesulfonate is 6.0 mol/L, the concentration of the N, N-methylene bisacrylamide is 0.003 mol/L, and the concentration of the sodium persulfate is 0.06 mol/L;
4) mixing the microgel powder obtained in the step 2) with the second monomer solution obtained in the step 3) to prepare a mixed solution, and controlling the mass ratio of the microgel powder to the second monomer solution to be 1:10;
5) and (3) uniformly coating the mixed solution obtained in the step 4) on two surfaces of a 500-mesh carbon fiber woven mesh, and heating at 90 ℃ for 2 hours to obtain the microgel/carbon fiber composite material with the thickness of 100 mu m.
The microgel/carbon fiber composite material obtained in the embodiment 2 has a micron-sized inclusion block structure with the size of 10-30 μm, and a nano-sized protrusion structure with the size of 30-50 nm on the surface of the micron-sized inclusion block. The contact angle of the microgel/carbon fiber composite underwater to diesel oil is 160 degrees. The mechanical strength of the microgel/carbon fiber composite material is far greater than that of the traditional similar polymer, and the tensile strength is about 200 MPa.
Example 3:
a preparation method of a microgel/fiber composite material with underwater super oleophobic property comprises the following steps:
1) dissolving acrylic acid, N, N-methylene bisacrylamide and potassium persulfate in water to obtain a first monomer solution, wherein the concentration of the acrylic acid is 1.75 mol/L, the concentration of the N, N-methylene bisacrylamide is 0.0175 mol/L, and the concentration of the potassium persulfate is 0.0175 mol/L;
2) heating the first monomer solution obtained in the step 1) at 85 ℃ for 1.5 hours to obtain polyacrylic acid hydrogel, mashing, drying, and then grinding into microgel powder with the size of 700-800 mu m;
3) dissolving N-vinyl pyrrolidone, N, N-methylene bisacrylamide and potassium persulfate in water to obtain a second monomer solution, wherein the concentration of the N-vinyl pyrrolidone is 3.5 mol/L, the concentration of the N, N-methylene bisacrylamide is 0.00175 mol/L, and the concentration of the potassium persulfate is 0.035 mol/L;
4) mixing the microgel powder obtained in the step 2) with the second monomer solution obtained in the step 3) to prepare a mixed solution, and controlling the mass ratio of the microgel powder to the second monomer solution to be 1:5;
5) and (3) uniformly coating the mixed solution obtained in the step 4) on two surfaces of a 300-mesh nylon fiber woven mesh, and heating at 85 ℃ for 1.5 hours to obtain the microgel/nylon fiber composite material with the thickness of 2000 mu m.
The microgel/nylon fiber composite material obtained in the embodiment 3 has a micron-sized inclusion block structure with the size of 700-800 μm, and a nano-sized protrusion structure with the size of 400-500 nm on the surface of the micron-sized inclusion block. The contact angle of the microgel/nylon fiber composite underwater to the vegetable oil is 165 degrees. The mechanical strength of the microgel/nylon fiber composite material is far greater than that of the traditional similar polymer, and the tensile strength is about 200 MPa.
Example 4:
a preparation method of a microgel/fiber composite material with underwater super oleophobic property comprises the following steps:
1) dissolving N-vinyl pyrrolidone, N, N-methylene bisacrylamide and ammonium persulfate in water to obtain a first monomer solution, wherein the concentration of the N-vinyl pyrrolidone is 2 mol/L, the concentration of the N, N-methylene bisacrylamide is 0.02 mol/L, and the concentration of the ammonium persulfate is 0.02 mol/L;
2) heating the first monomer solution obtained in the step 1) at 80 ℃ for 2 hours to obtain N-vinyl pyrrolidone hydrogel, mashing, drying, and then grinding into microgel powder with the size of 100-200 mu m;
3) dissolving acrylic acid, N, N-methylene-bisacrylamide and ammonium persulfate in water to obtain a second monomer solution, wherein the concentration of the acrylic acid is 2 mol/L, the concentration of the N, N-methylene-bisacrylamide is 0.001 mol/L, and the concentration of the ammonium persulfate is 0.02 mol/L;
4) mixing the microgel powder obtained in the step 2) with the second monomer solution obtained in the step 3) to prepare a mixed solution, and controlling the mass ratio of the microgel powder to the second monomer solution to be 1:7;
5) and (3) uniformly coating the mixed solution obtained in the step (4) on two surfaces of a 200-mesh aramid fiber woven mesh, and heating at 80 ℃ for 2 hours to obtain the microgel/aramid fiber composite material, wherein the thickness of the material is 500 microns.
The microgel/aramid fiber composite material obtained in the embodiment 4 has a micron-sized inclusion block structure with the size of 100-200 μm, and a nano-sized protrusion structure with the size of 80-100 nm on the surface of the micron-sized inclusion block. The contact angle of the microgel/aramid fiber composite material underwater to crude oil is 162 degrees. The mechanical strength of the microgel/aramid fiber composite material is far greater than that of the traditional similar polymer, and the tensile strength is about 180 MPa.
Example 5:
a preparation method of a microgel/fiber composite material with underwater super oleophobic property comprises the following steps:
1) dissolving sodium p-styrene sulfonate, N, N-methylene bisacrylamide and sodium persulfate in water to obtain a first monomer solution, wherein the concentration of the sodium p-styrene sulfonate is 1 mol/L, the concentration of the N, N-methylene bisacrylamide is 0.008 mol/L, and the concentration of the ammonium persulfate is 0.01 mol/L;
2) heating the first monomer solution obtained in the step 1) at 90 ℃ for 1 hour to obtain sodium p-styrenesulfonate hydrogel, mashing, drying, and then grinding into microgel powder with the size of 550-650 microns;
3) dissolving 2-acrylamide-2-methylpropanesulfonic acid, N, N-methylene bisacrylamide and sodium persulfate in water to obtain a second monomer solution, wherein the concentration of the 2-acrylamide-2-methylpropanesulfonic acid is 5 mol/L, the concentration of the N, N-methylene bisacrylamide is 0.002 mol/L, and the concentration of the sodium persulfate is 0.05 mol/L;
4) mixing the microgel powder obtained in the step 2) with the second monomer solution obtained in the step 3) to prepare a mixed solution, and controlling the mass ratio of the microgel powder to the second monomer solution to be 1:3;
5) and (3) uniformly coating the mixed solution obtained in the step 4) on two surfaces of a 400-mesh acrylic fiber woven net, and heating at 90 ℃ for 1 hour to obtain the microgel/acrylic fiber composite material with the thickness of 1500 mu m.
The microgel/acrylic fiber composite material obtained in the embodiment 5 has a micron-sized inclusion block structure with the size of 550-650 mu m, and a nano-sized protrusion structure with the size of 350-450 nm on the surface of the micron-sized inclusion block. The underwater contact angle of the microgel/acrylic fiber composite material to normal hexane is 158 degrees. The mechanical strength of the microgel/acrylic fiber composite material is far greater than that of the traditional similar polymer, and the tensile strength is about 320 MPa.
Claims (3)
1. A preparation method of a microgel/fiber composite material with underwater super oleophobic property is characterized by comprising the following steps:
1) dissolving a first monomer, a cross-linking agent and an initiator in water to obtain a first monomer solution, wherein the concentration of the first monomer is 0.5-3 mol/L, the concentration of the cross-linking agent is 0.005-0.03 mol/L, the concentration of the initiator is 0.005-0.03 mol/L, and the first monomer is any one or a mixture of two or more of 2-acrylamido-2-methylpropanesulfonic acid, sodium p-styrenesulfonate, acrylamide, acrylic acid and N-vinyl pyrrolidone;
2) heating the first monomer solution obtained in the step 1) at 80-90 ℃ for 1-2 hours to obtain a first network hydrogel, mashing, drying, and grinding into microgel powder;
3) dissolving a second monomer, a cross-linking agent and an initiator in water to obtain a second monomer solution, wherein the concentration of the second monomer is 1.0-6 mol/L, the concentration of the cross-linking agent is 0.0005-0.003 mol/L, the concentration of the initiator is 0.01-0.06 mol/L, and the second monomer is any one or a mixture of two or more of 2-acrylamido-2-methylpropanesulfonic acid, sodium p-styrenesulfonate, acrylamide, acrylic acid and N-vinyl pyrrolidone;
4) mixing the microgel powder obtained in the step 2) with the second monomer solution obtained in the step 3) to prepare a mixed solution, wherein the mass ratio of the microgel powder to the second monomer solution is controlled to be 1: (1-10);
5) and (3) uniformly coating the mixed solution obtained in the step (4) on two surfaces of a fiber woven mesh, and heating at 80-90 ℃ for 1-2 hours to obtain the microgel/fiber composite material, wherein the fiber woven mesh is one of glass fiber, carbon fiber, nylon, acrylic fiber and aramid fiber woven mesh.
2. The method according to claim 1, wherein the crosslinking agent in step 1) and step 3) is N, N-methylenebisacrylamide.
3. The preparation method according to claim 1, wherein the initiator in step 1) and step 3) is any one of ammonium persulfate, potassium persulfate and sodium persulfate.
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