Material used for rapid separation of oil and water and preparation method and application thereof

Abstract

The present invention discloses a material used for rapid separation of oil and water and preparation method and application thereof, the mesh material is placed into monomer solution, reacting with the presence of initiator to prepare material used for rapid separation of oil and water. The monomer is divinylbenzene or 2-(dimethylamino) ethyl methacrylate, and the mesh material is stainless steel mesh. The present invention modifies the functional small molecules and polymers to the surface of the materials, thereby preparing multifunctional composite materials, effectively separating oil-water emulsion, so as to achieve the purpose of oil-water separation.

Claims

1. A preparation method of a material used for separation of oil and water, the method consisting of the following steps in a sequential order without any additional steps: providing a mesh material, the mesh material being a stainless steel mesh; cleaning the mesh material with an organic solvent; treating the mesh material with an acid; treating the mesh material with a silanating agent; placing the mesh material into a monomer solution; and reacting the monomer with the presence of an initiator at between 60 to 80 C. and for between 15 to 30 hours to prepare the material used for separation of oil and water, wherein the monomer is 2-(dimethylamino) ethyl methacrylate; wherein the initiator is azobisisobutyronitrile; and wherein the mass ratio of the monomer and the initiator is 40:0.5 to 40:2.

2. The preparation method of the material used for separation of oil and water according to claim 1, wherein the organic solvent is ethanol or acetone.

3. The preparation method of the material used for separation of oil and water according to claim 1, wherein the acid is hydrochloric acid.

4. The preparation method of the material used for separation of oil and water according to claim 1, wherein the silanating agent is vinyltrichlorosilane.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 is a scanning electron micrograph (SEM) of a prior stainless steel mesh;

(2) FIG. 2 shows the polydivinylbenzene-modified stainless steel mesh SEM;

(3) FIG. 3 is a SEM image of a stainless steel mesh modified with poly (2-(dimethylamino) ethyl methacrylate);

(4) FIG. 4 is a graph showing the wettability of a stainless steel mesh after polydivinylbenzene modification;

(5) FIG. 5 shows emulsion separation effect of the modified stainless steel mesh;

(6) FIG. 6 shows separation efficiency and flux diagrams of the modified stainless steel mesh;

(7) FIG. 7 shows the recycling separation efficiency and flux diagrams of the modified stainless steel mesh.

DETAILED DESCRIPTIONS

Embodiment 1

(8) Preparation of polydivinylbenzene-modified stainless steel mesh (PDVB@SSM), the procedure is as follows:

(9) The stainless steel mesh was washed by ethanol and acetone respectively, to remove the surface impurities of the stainless steel mesh. The treated stainless steel mesh was acidified in hydrochloric acid and placed in a toluene solution containing 0.8 g of vinyltrichlorosilane and allowed to stand at room temperature for 12 hours silanized and washed by toluene for three times and drying in a vacuum oven stand-by. A solution of 30 mL of N,N-dimethylformamide was poured into a three-neck flask, 0.8 g of divinylbenzene was added, and the mixture was stirred at room temperature for two hours. The mixed solution was deoxygenated by bubbling and finally 0.006 g of azobisisobutyronitrile (dissolved in N,N-dimethylformamide) was added, and the mixed solution was stirred in an oil bath at 60 C. for 12 hours. The stainless steel mesh was taken out and rinsed with a large amount of toluene and dried in a vacuum oven for 30 minutes to obtain a PDVB-modified stainless steel mesh.

(10) FIG. 1 is a SEM of a prior stainless steel mesh, FIG. 2 shows the PDVB-modified stainless steel mesh SEM image, through the figure, it can be seen that the mesh surface is covered with a layer of PDVB polymer.

Embodiment 2

(11) Preparation of polydivinylbenzene-modified stainless steel mesh (PDVB@SSM), the procedure is as follows:

(12) The stainless steel mesh was washed by ethanol and acetone respectively, to remove the surface impurities of the stainless steel mesh. The treated stainless steel mesh was acidified in hydrochloric acid and placed in a toluene solution containing 0.5 g of vinyltrichlorosilane and allowed to stand at room temperature for 15 hours silanized and washed by toluene for three times and drying in a vacuum oven stand-by. A solution of 50 mL of N,N-dimethylformamide was poured into a three-neck flask, 1.0 g of divinylbenzene was added, and the mixture was stirred at room temperature for two hours. The mixed solution was deoxygenated by bubbling and finally 0.002 g of azobisisobutyronitrile (dissolved in N,N-dimethylformamide) was added, and the mixed solution was stirred in an oil bath at 50 C. for 15 hours. The stainless steel mesh was taken out and rinsed with a large amount of toluene and dried in a vacuum oven for 60 minutes to obtain a PDVB-modified stainless steel mesh.

Embodiment 3

(13) Preparation of poly (2-(dimethylamino) ethyl methacrylate-modified stainless steel mesh (PDMAEMA@SSM), as follows:

(14) A vinyl trichlorosilane-modified stainless steel mesh was placed in a three-necked flask, 30 mL of tetrahydrofuran was added, and then 4 g of 2-(dimethylamino) ethyl methacrylate was added and the solution was deoxygenated by bubbling at 30 minute, finally 0.1 g of azobisisobutyronitrile (dissolved in 5 mL of tetrahydrofuran) was added to the three-necked flask by injection, the mixture was stirred in an oil bath at 68 C. for 24 hours. The stainless steel mesh was taken out and washed with a large amount of tetrahydrofuran. The mesh was dried in a vacuum oven at 120 C. for 1 hour to obtain a PDMAEMA-modified stainless steel mesh.

(15) FIG. 3 shows the PDMAEMA modified stainless steel mesh SEM images, the polymer PDMAEMA successfully modified on the stainless steel mesh as shown in the picture.

Embodiment 4

(16) Preparation of poly (2-(dimethylamino) ethyl methacrylate-modified stainless steel mesh (PDMAEMA@SSM), as follows:

(17) A vinyl trichlorosilane-modified stainless steel mesh was placed in a three-necked flask, 30 mL of tetrahydrofuran was added, and then 5 g of 2-(dimethylamino) ethyl methacrylate was added and the solution was deoxygenated by bubbling at 60 minute, finally 0.05 g of azobisisobutyronitrile (dissolved in 5 mL of tetrahydrofuran) was added to the three-necked flask by injection, the mixture was stirred in an oil bath at 80 C. for 15 hours. The stainless steel mesh was taken out and washed with a large amount of tetrahydrofuran. The mesh was dried in a vacuum oven at 150 C. for 1 hour to obtain a PDMAEMA-modified stainless steel mesh.

Embodiment 5

(18) Wetting behavior of modified stainless steel net.

(19) FIG. 4 shows the water wettability of the stainless steel net before and after the PDVB modification. It can be seen that the water before the modification is easy to wet the stainless steel mesh and the water droplets adhere to the mesh. While the water droplets quickly rolled down from the modified stainless steel mesh and could not wet the mesh, illustration is the contact Angle of water. Water droplets on the surface of modified stainless steel mesh to form a spherical shape with the contact angle 151, indicating its good hydrophobicity, the unmodified stainless steel mesh, water droplets on its surface is not spherical, further shows PDVB modified stainless steel mesh with super hydrophobicity.

Embodiment 6

(20) Emulsion separation test, the specific steps are as follows:

(21) 5 mL of water was added to 45 mL of toluene, and then 2.5 mg of sodium dodecyl sulfonate was further added for 12 hours with ultrasound followed by an emulsion separation test.

(22) Take the modified double-layer stainless steel mesh into the glass, as shown in FIG. 5 for the oil-water emulsion separation diagram, and then pour 50 mL oil-water emulsion, seen from the figure, the when the milky white oil-water emulsion into the glass with modified double-layer stainless steel mesh and clarified toluene into the beaker, indicating that it has a good emulsion separation effect.

Embodiment 7

(23) Test of separation efficiency and flow rate of stainless steel net modified by PDVB and PDMAEMA. With steps as follows:

(24) A variety of oil-water emulsion was separated from the prepared double layer stainless steel mesh. Then the water content in the filtrate was measured by the micro moisture detector. The separation efficiency of different oil-water emulsion was all over 99.8%.

(25) For the determination of the separation flow rate of various emulsion, the following equation is used to calculate the flux of the modified double layer stainless steel mesh:
Flux=V/At

(26) In which V is the volume of penetration, A is the effective filter surface (cm.sup.2) of SSM, and t is the effective time. For each test, A certain amount of water/oil mixture and emulsion are poured into the filter to obtain the average value.

(27) FIG. 6 is the different oil-water emulsion separation efficiency and flow, can be seen from the figure for the different emulsion has a high separation efficiency and flow.

(28) FIG. 7 is the recyclability of the test, we can see from the figure after 10 cycles also maintain a good separation efficiency and flow, which indicating a better reusability.

Embodiment 8

(29) Separation efficiency and flow rate test of PDVB and PDMAEMA modified double layer stainless steel mesh.

(30) With the steps of embodiment 5, the separation efficiency of different oil-water emulsion is all over 99.8%, and the flow rate is over 1000. After 10 cycles, the separation efficiency and flow rate remain very good, indicating that it has good reusability.

(31) Through the above analysis, the surface modification method is successfully used to functionalize the stainless steel mesh, so that it has the function of separating the emulsion, and the modified stainless steel mesh has the advantages of high separation speed, high efficiency and good recyclability. The preparation method is simple and the raw material is cheap. Therefore, the wastewater treatment and emulsion separation has a very good application prospects.