CN108786759B - Oil-water separation material with antifouling, sterilizing and dye adsorbing functions and preparation method thereof - Google Patents
Oil-water separation material with antifouling, sterilizing and dye adsorbing functions and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- Water Treatment By Sorption (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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Abstract
The invention discloses an oil-water separation material with antifouling, sterilization and dye adsorption functions and a preparation method thereof. Dipping a base material into a copolymer aqueous solution by adopting a dip coating method, taking out after ultrasonic dispersion for a certain time, naturally airing, washing and secondarily drying to obtain the oil-water separation material with the functions of antifouling, sterilization and dye adsorption. The oil-water separation material disclosed by the invention is simple in preparation method, green and environment-friendly, has multiple functions of antifouling and sterilization, dye adsorption, oil-water separation and the like, and can be used in the fields of oil-water mixture separation, dye-containing oil sewage treatment and the like.
Description
Technical Field
The invention relates to a preparation method of an oil-water separation material with antifouling, sterilization and dye adsorption functions, and belongs to the technical field of organic-inorganic composite functional materials.
Background
The discharge of a large amount of oily sewage and the occurrence of crude oil leakage accidents put higher requirements on oil-water separation technology and materials. The oil-water separation is realized by utilizing the special wettability of the material to act on different interfaces of oil and water, and the oil-water separation material becomes an important breakthrough for promoting the development of an oil-water separation technology.
On the premise of keeping high oil-water separation efficiency, the universal material is utilized, the technological process is simplified, the stability is improved, the manufacturing cost is reduced, and the large-scale preparation and application of the oil-water separation material are the development direction in the field. Compared with a metal net film or other hard materials, the filter paper, cloth, sponge and other general materials have the advantages of softness, easy forming and the like, and have unique advantages when being used for preparing oil-water separation materials. At present, the problems of complex process, complex steps and the like generally exist in the preparation of the oil-water separation material, and certain environmental pollution is caused in the aspects of material recycling and disposal, so that a simple, quick, economic and environment-friendly method needs to be found for preparing the oil-water separation material.
In the oil-water separation process, proteins and bacteria in a system are easily attached to the surface of a material, so that the material is polluted, and the permeability and the separation effect of the material are influenced. Particularly in the process of treating the oil-containing sewage, the dye components in the water are often removed in addition to the oil-water separation.
The oil-water separation, antifouling self-purification, dye adsorption and other functions are combined, so that the material is simultaneously used for the functions, and the method has important significance for expanding the application of the oil-water separation material. Therefore, the development of a preparation method of the oil-water separation material with antifouling, sterilization and dye adsorption functions is imperative.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an oil-water separation material with antifouling, sterilization and dye adsorption functions and a preparation method thereof.
The preparation method of the oil-water separation material with antifouling, sterilization and dye adsorption functions comprises the steps of preparing a specific polymer into an aqueous solution by a dip-coating method, adjusting the pH value of the aqueous solution to be alkaline, immersing a base material into the prepared solution, taking out the base material after ultrasonic dispersion, naturally airing, washing and secondarily drying to obtain the oil-water separation material with antifouling, sterilization and dye adsorption functions;
the method is characterized in that:
the specific polymer is a polymer with a structure shown in a formula (I):
wherein R is1Is H or CH3，R2Is H or CH3Z is CH2Or CH2CH2A, b, c and d are natural numbers larger than 0, and n is 10-50; the molar ratio of the polyoxyethylene ether chain segment, the carboxyl chain segment, the siloxane chain segment and the quaternary ammonium salt segment in the polymer is (a), (b), (c) and (d) is 1: 3-7: 0.2-1.0;
the concentration of the polymer aqueous solution is 5-10 wt%, and the pH value is 8-9;
the base material is filter paper, cotton cloth or sponge;
the ultrasonic dispersion time is 10-30 min, the natural drying time is 12-24 h, the washing mode is deionized water washing, soaking and washing for 2-3 times, and the secondary drying is drying for 4-6 h at 60-70 ℃.
The preferable embodiment of the preparation method of the oil-water separation material with the functions of antifouling, sterilization and dye adsorption is as follows: r in the polymer1Is H, R2Is H, Z is CH2A, b, c and d are natural numbers larger than 0, and n is 20-40. The molar ratio of the polyoxyethylene ether chain segment to the carboxyl chain segment to the siloxane chain segment to the quaternary ammonium salt segment in the polymer is (a: b) - (c: d) 1: 3.5: 5: 0.2-0.5. The concentration of the polymer aqueous solution is 7-8 wt%.
In the preparation method of the oil-water separation material with antifouling, sterilization and dye adsorption functions, the polymer is prepared by the following method: the material is polyoxyethylene ether macromonomer, (methyl) acrylic acid, 3-methacryloxypropyltrimethoxysilane and methacryloxyethyltrimethyl ammonium chloride, and the material is prepared by free radical polymerization by using an oxidation-reduction system; wherein the polyoxyethylene ether macromonomer is Allyl Polyoxyethylene Ether (APEG), isobutenol polyoxyethylene ether (HPEG) or isobutenol polyoxyethylene ether (TPEG); the redox system is hydrogen peroxide/vitamin C, and the chain transfer agent in the free radical polymerization reaction is mercaptopropionic acid.
The oil-water separation material with the functions of antifouling, sterilization and dye adsorption is prepared by the preparation method.
The material treated by the method can realize the quick and effective separation of oil-water mixture, and has the functions of antifouling, sterilization and dye adsorption.
The oil-water separation material with the functions of antifouling, sterilization and dye adsorption has the following characteristics:
(1) provides a preparation method of the oil-water separation material with simple process and environmental protection;
(2) the common material is utilized, and the oil-water separation material is obtained in one step by a dip coating method, so that the method is quick and convenient;
(3) hydrophilic components (polyoxyethylene ether and carboxyl) on the surface of the material can react with water molecules to form a hydration layer, so that protein adsorption and the attachment of other organic matters are inhibited, and the material has a self-cleaning function;
(4) the surface of the material contains quaternary ammonium salt cations, so that the material has a bactericidal effect;
(5) the surface of the material contains carboxyl, so that cationic dyes such as methylene blue, methyl orange and the like can be effectively adsorbed;
(6) the material can be repeatedly used and is easy to dispose.
Detailed Description
In order that the invention may be readily understood, the following examples are set forth in order to provide a further understanding of the invention. These examples are representative and do not include all examples, but are provided to more clearly illustrate the invention and not to limit the scope of the invention.
Example 1
(1) Preparation of polymers
A250 mL four-necked flask was charged with 60g of polyether macromonomer TPEG2400, 1.86g of methacryloxypropyltrimethoxysilane (KH570), 2.1g of methacryloxyethyltrimethyl ammonium chloride, and 52g of deionized water, stirred at room temperature to dissolve the macromonomer, and charged with 0.69g of hydrogen peroxide (30 wt%). After stirring for 15min, A, B liquid (the liquid A is an aqueous solution prepared from 7.56g of acrylic acid and 5g of deionized water, and the liquid B is an aqueous solution prepared from 0.36g of 3-mercaptopropionic acid, 0.429g of vitamin C and 12g of deionized water) is added dropwise at a constant speed. Dropwise adding the solution A for 2.5h, dropwise adding the solution B for 3.0h, and preserving heat for 1.5h after dropwise adding. And after the reaction is finished, adding 30 wt% of NaOH solution to neutralize until the pH value is 6-7, and supplementing water until the solid content is 40% to obtain light yellow viscous liquid, namely the product polymer.
(2) Preparation of oil-water separation material
Taking the polymer viscous liquid prepared in the step (1), preparing a 5 wt% polymer aqueous solution, and adjusting the pH value to 8-9 by using a 30 wt% NaOH solution. Soaking filter paper in the solution for 30min by ultrasonic dispersion, naturally airing for 24h, washing, soaking and washing for 3 times by deionized water, and drying for 6h at 70 ℃ by secondary drying to obtain the oil-water separation material with the functions of antifouling, sterilization and dye adsorption.
(3) Oil-water separation
Preparing petroleum ether/deionized water mixed liquor (the volume ratio is 1:1) and petroleum ether/deionized water emulsion (the volume ratio is 1:1) with Sodium Dodecyl Sulfate (SDS) as an emulsifier. And (3) separating the mixed solution from the emulsion by using the oil-water separation material prepared in the step (2).
(4) Dye adsorption
And (3) respectively adding a certain amount of methylene blue solution into the petroleum ether/deionized water mixed solution and the petroleum ether/deionized water emulsion prepared in the step (3), and uniformly mixing by ultrasonic waves. And (3) carrying out oil-water separation and dye adsorption on the mixed liquid and the emulsion by using the oil-water separation material prepared in the step (2).
Example 2
(1) Preparation of polymers
The same as in example 1.
(2) Preparation of oil-water separation material
Taking the polymer viscous liquid prepared in the step (1), preparing a polymer aqueous solution with the concentration of 7.5 wt%, and adjusting the pH to 8-9 by using a 30 wt% NaOH solution. Soaking cotton cloth in the solution for 20min by ultrasonic dispersion, naturally drying for 18h, washing with deionized water, soaking and washing for 2 times, and drying at 70 deg.C for 4h to obtain the oil-water separation material with antifouling, bactericidal and dye adsorption functions.
(3) Oil-water separation
The same as in example 1.
(4) Dye adsorption
The same as in example 1.
Example 3
(1) Preparation of polymers
The same as in example 1.
(2) Preparation of oil-water separation material
Taking the polymer viscous liquid prepared in the step (1), preparing a polymer aqueous solution with the concentration of 10 wt%, and adjusting the pH to 8-9 by using a 30 wt% NaOH solution. Soaking sponge in the solution for 15min by ultrasonic dispersion, naturally drying for 12h, washing with deionized water, soaking and washing for 3 times, and drying at 70 deg.C for 6h to obtain the oil-water separation material with antifouling, bactericidal and dye adsorption functions.
(3) Oil-water separation
The same as in example 1.
(4) Dye adsorption
The same as in example 1.
Example 4
(1) Preparation of polymers
A250 mL four-necked flask was charged with 60g of a polyether macromonomer HPEG2400, 3.1g of methacryloxypropyltrimethoxysilane (KH570), 2.1g of methacryloxyethyltrimethyl ammonium chloride, and 52g of deionized water, stirred at room temperature to dissolve the macromonomer, and charged with 0.69g of hydrogen peroxide (30 wt%). After stirring for 15min, A, B liquid (the liquid A is an aqueous solution prepared from 7.56g of acrylic acid and 5g of deionized water, and the liquid B is an aqueous solution prepared from 0.36g of 3-mercaptopropionic acid, 0.43g of vitamin C and 12g of deionized water) is added dropwise at a constant speed. Dropwise adding the solution A for 2.5h, dropwise adding the solution B for 3.0h, and preserving heat for 1.5h after dropwise adding. After the reaction is finished, adding 30 wt% NaOH solution to neutralize to the pH value of 6-7, and replenishing water until the solid content is 40% to obtain light yellow viscous liquid.
(2) Preparation of oil-water separation material
Taking the polymer viscous liquid prepared in the step (1), preparing a polymer aqueous solution with the concentration of 5 wt%, and adjusting the pH to 8-9 by using a 30 wt% NaOH solution. Soaking filter paper in the solution for 15min by ultrasonic dispersion, naturally airing for 24h, washing, soaking and washing for 3 times by deionized water, and drying for 4h at 70 ℃ by secondary drying to obtain the oil-water separation material with antifouling, sterilization and dye adsorption functions.
(3) Oil-water separation
The same as in example 1.
(4) Dye adsorption
The same as in example 1.
Example 5
(1) Preparation of polymers
The same as in example 4.
(2) Preparation of oil-water separation material
Taking the polymer viscous liquid prepared in the step (1), preparing a polymer aqueous solution with the concentration of 7.5 wt%, and adjusting the pH value to 8-9 by using a 30 wt% NaOH solution. Soaking cotton cloth in the solution for 15min by ultrasonic dispersion, naturally drying for 24h, washing with deionized water, soaking and washing for 3 times, and drying at 70 deg.C for 4h to obtain the oil-water separation material with antifouling, bactericidal and dye adsorption functions.
(3) Oil-water separation
The same as in example 1.
(4) Dye adsorption
The same as in example 1.
Example 6
(1) Preparation of polymers
The same as in example 4.
(2) Preparation of oil-water separation material
Taking the polymer viscous liquid prepared in the step (1), preparing a polymer aqueous solution with the concentration of 10 wt%, and adjusting the pH to 8-9 by using a 30 wt% NaOH solution. Soaking sponge in the solution for 20min by ultrasonic dispersion, naturally drying for 18h, washing with deionized water, soaking and washing for 3 times, and drying at 60 deg.C for 6h to obtain the oil-water separation material with antifouling, bactericidal and dye adsorption functions.
(3) Oil-water separation
The same as in example 1.
(4) Dye adsorption
The same as in example 1.
Example 7
(1) Preparation of polymers
A250 mL four-necked flask was charged with 60g of polyether macromonomer APEG2400, 2.48g of methacryloxypropyltrimethoxysilane (KH570), 2.8g of methacryloxyethyltrimethyl ammonium chloride, and 52g of deionized water, stirred at room temperature to dissolve the macromonomer, and charged with 0.69g of hydrogen peroxide (30 wt%). After stirring for 15min, A, B liquid (the liquid A is an aqueous solution prepared from 7.56g of acrylic acid and 5g of deionized water, and the liquid B is an aqueous solution prepared from 0.36g of 3-mercaptopropionic acid, 0.429g of vitamin C and 12g of deionized water) is added dropwise at a constant speed. Dropwise adding the solution A for 2.5h, dropwise adding the solution B for 3.0h, and preserving heat for 1.5h after dropwise adding. After the reaction is finished, adding 30 wt% NaOH solution to neutralize to the pH value of 6-7, and replenishing water until the solid content is 40% to obtain light yellow viscous liquid.
(2) Preparation of oil-water separation material
Taking the polymer viscous liquid prepared in the step (1), preparing a polymer aqueous solution with the concentration of 5 wt%, and adjusting the pH to 8-9 by using a 30 wt% NaOH solution. Soaking filter paper in the solution for 30min by ultrasonic dispersion, naturally airing for 24h, washing, soaking and washing for 3 times by deionized water, and drying for 4h at 70 ℃ by secondary drying to obtain the oil-water separation material with antifouling, sterilization and dye adsorption functions.
(3) Oil-water separation
The same as in example 1.
(4) Dye adsorption
The same as in example 1.
Example 8
(1) Preparation of polymers
The same as in example 7.
(2) Preparation of oil-water separation material
Taking the polymer viscous liquid prepared in the step (1), preparing a polymer aqueous solution with the concentration of 7.5 wt%, and adjusting the pH to 8-9 by using a 30 wt% NaOH solution. Soaking filter paper in the solution for 30min by ultrasonic dispersion, naturally airing for 24h, washing, soaking and washing for 3 times by deionized water, and drying for 4h at 70 ℃ by secondary drying to obtain the oil-water separation material with antifouling, sterilization and dye adsorption functions.
(3) Oil-water separation
The same as in example 1.
(4) Dye adsorption
The same as in example 1.
Example 9
(1) Preparation of polymers
The same as in example 7.
(2) Preparation of oil-water separation material
Taking the polymer viscous liquid prepared in the step (1), preparing a polymer aqueous solution with the concentration of 10 wt%, and adjusting the pH to 8-9 by using a 30 wt% NaOH solution. Soaking filter paper in the solution for 30min by ultrasonic dispersion, naturally airing for 24h, washing, soaking and washing for 3 times by deionized water, and drying for 4h at 70 ℃ by secondary drying to obtain the oil-water separation material with antifouling, sterilization and dye adsorption functions.
(3) Oil-water separation
The same as in example 1.
(4) Dye adsorption
The same as in example 1.
Claims (6)
1. A preparation method of an oil-water separation material with antifouling, sterilization and dye adsorption functions comprises the steps of preparing a specific polymer into an aqueous solution by a dip-coating method, adjusting the pH value of the aqueous solution to be alkaline, immersing a base material into the prepared solution, taking out the base material after ultrasonic dispersion, naturally airing, washing and secondarily drying to obtain the oil-water separation material with antifouling, sterilization and dye adsorption functions;
the method is characterized in that:
the specific polymer is a polymer with a structure shown in a formula (I):
wherein R is1Is H or CH3，R2Is H or CH3Z is CH2Or CH2CH2A, b, c and d are natural numbers larger than 0, and n is 10-50; the molar ratio of the polyoxyethylene ether chain segment to the carboxyl chain segment to the siloxane chain segment to the quaternary ammonium salt segment in the polymer is (a), (b), (c) and (d) is 1: 3-7: 0.2-1.0;
the concentration of the polymer aqueous solution is 5-10 wt%, and the pH value is 8-9;
the base material is filter paper, cotton cloth or sponge;
the ultrasonic dispersion time is 10-30 min, the natural drying time is 12-24 h, the washing mode is deionized water washing, soaking and washing for 2-3 times, and the secondary drying is drying for 4-6 h at 60-70 ℃.
2. The method for preparing the oil-water separation material with antifouling, sterilization and dye adsorption functions according to claim 1, wherein the method comprises the following steps: r in the polymer1Is H, R2Is H, Z is CH2A, b, c and d are natural numbers larger than 0, and n is 20-40.
3. The method for preparing the oil-water separation material with antifouling, sterilization and dye adsorption functions according to claim 1, wherein the method comprises the following steps: the molar ratio of the polyoxyethylene ether chain segment to the carboxyl chain segment to the siloxane chain segment to the quaternary ammonium salt segment in the polymer is (a: b) - (c: d) 1: 3.5: 5: 0.2-0.5.
4. The method for preparing the oil-water separation material with antifouling, sterilization and dye adsorption functions according to claim 1, wherein the method comprises the following steps: the concentration of the polymer aqueous solution is 7-8 wt%.
5. The method for preparing the oil-water separation material with the functions of antifouling, sterilization and dye adsorption according to claim 1, wherein the polymer is prepared by the following method: the material is polyoxyethylene ether macromonomer, (methyl) acrylic acid, 3-methacryloxypropyltrimethoxysilane and methacryloxyethyltrimethyl ammonium chloride, and the material is prepared by free radical polymerization by using an oxidation-reduction system; wherein the polyoxyethylene ether macromonomer is Allyl Polyoxyethylene Ether (APEG), isobutenol polyoxyethylene ether (HPEG) or prenol polyoxyethylene ether (TPEG); the redox system is hydrogen peroxide/vitamin C, and the chain transfer agent in the free radical polymerization reaction is mercaptopropionic acid.
6. An oil-water separating material having antifouling, bactericidal and dye adsorbing functions, prepared by the method according to any one of claims 1 to 4.
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| JP2002316838A (en) * | 2001-04-12 | 2002-10-31 | Hiroki Koma | Functional inorganic material |
| CN103347496A (en) * | 2010-12-27 | 2013-10-09 | 道康宁公司 | Drug delivery dispersion and film formed therefrom |
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| WO2016143651A1 (en) * | 2015-03-06 | 2016-09-15 | 日本化学工業株式会社 | Oil-water separating material and oil-water separation method |
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