CN114108325B - Preparation method of composite coating for resisting oil stain and degrading dye - Google Patents
Preparation method of composite coating for resisting oil stain and degrading dye Download PDFInfo
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Abstract
The invention relates to a preparation method of a composite coating of an oil stain resistant and degradation dye. The invention aims to solve the problems of complex preparation process, low pollutant removal efficiency and secondary environmental pollution caused by dye desorption of the traditional composite material for resisting oil stains and degrading dyes. The invention takes chemical fiber cotton as a base material and utilizes the poly-dopamine coating phenolic hydroxyl group to carry out Ag reaction + Silver nano particles are grown under the metal coordination and reduction action, and finally polyaniline doped with hydrochloric acid is grown in situ. The material has excellent oil stain resistance, the removal efficiency of various greasy dirt is more than 99%, the visible light catalytic degradation efficiency of organic dye can reach 99.7%, and the material is applied to the field of functional composite coating material synthesis.
Description
Technical field:
the invention belongs to the field of synthesis of functional composite coating materials, and particularly relates to a composite coating for resisting oil stains and degrading dyes and a preparation method thereof.
The background technology is as follows:
with population growth and rapid development of modern industry, household garbage, crude oil leakage and improper discharge of organic pollutants in industrial production cause serious pollution to water resources in nature. Domestic wastewater and factory wastewater often contain oil substances insoluble in water and organic dyes soluble in water, and simultaneously degreasing and organic dyes become a great challenge for current wastewater treatment. Therefore, development of a separation material having oil stain resistance and dye removal properties is urgently required for application to the field of wastewater treatment.
The material with the special wettability surface has excellent oil stain resistance, can quickly and efficiently remove floating oil in water, but is difficult to effectively remove water-soluble organic dye. A series of composite separation materials capable of simultaneously removing greasy dirt and organic dye are prepared by adopting a composite technology at present, but the problems of complex preparation process, low pollutant removal efficiency or secondary environmental pollution caused by dye desorption exist.
The invention comprises the following steps:
the invention aims to solve the problems of complex preparation process, low pollutant removal efficiency and secondary environmental pollution caused by dye desorption of the traditional composite material for resisting oil stains and degrading dyes, and provides a preparation method of a composite coating for resisting the oil stains and degrading the dyes.
The invention relates to a preparation method of a composite coating for resisting oil stain and degrading dye, which is characterized by comprising the following steps:
1. dissolving dopamine in tris hydrochloride solution, and adding CuSO 4 ·5H 2 O and H 2 O 2 Immersing chemical fiber cotton, and stirring to obtain PDA@CFC; dopamine, cuSO 4 ·5H 2 O, tris hydrochloride solution and H 2 O 2 The mass volume ratio is 30-50mg:20-30mg:15-25mL:0.03-0.07mL;
2. immersing PDA@CFC into silver ammonia solution, and obtaining Ag/PDA@CFC after the reaction is completed;
3. mixing aniline and HCl solution to obtain mixed solution, immersing Ag/PDA@CFC into the mixed solution, stirring, dripping APS solution, and fully reacting to obtain the composite coating with oil stain resistance and degradation dye; the volume ratio of the aniline to the HCl solution is 1-1.2:620-760; the volume ratio of the APS solution to the HCl solution is 1:1-1.5.
The invention takes chemical fiber cotton (polyester screen mesh, porous sponge and cotton fabric) as a base material, and utilizes Polydopamine (PDA) to coat phenolic hydroxyl groups on Ag + Silver nanoparticles (AgNPs) were grown by metal complexation and reduction, and finally hydrochloric acid doped Polyaniline (PANI) was grown in situ.
The invention has the advantages that: the preparation method adopts polydopamine reduction and aniline in-situ chemical oxidation polymerization, has simple synthesis process, uses non-fluorine raw materials, and is environment-friendly; the invention has universality and can be applied to the surfaces of various base materials; the coating material has excellent super-hydrophilic/underwater super-oleophobic property, and can effectively separate various oil-water mixtures. The coupling effect of PANI and AgNPs widens the light absorption range of AgNPs, enhances the light absorption capacity under visible light, and has the degradation efficiency of 99.7% on organic dye under the irradiation of visible light.
Drawings
FIG. 1 is an SEM image of PANI/Ag/PDA@CFC at various magnifications;
FIG. 2 is a contact angle of a composite coating of an anti-oil and degradation dye to a water drop;
FIG. 3 is a graph showing the underwater contact angle of a composite coating of oil stain resistant and dye degrading to various organic solvents;
FIG. 4 is a graph showing the separation flux and efficiency of a composite coating of greasy dirt resistant and degradation dye for different organic solvents; wherein a is the separation flux and b is the separation efficiency;
FIG. 5 is a graph showing the repeated separation capacity of the composite coating of anti-oil and degradation dye from toluene/water;
FIG. 6 shows the effect of visible light catalytic degradation of methyl orange; wherein 1 is before photocatalytic degradation, and 2 is after photocatalytic degradation;
FIG. 7 is a graph showing the color change of a filter flask containing methyl orange solution before and after photocatalytic degradation;
FIG. 8 is the effect of Congo red on visible light catalytic degradation; wherein 3 is before photocatalytic degradation, and 4 is after photocatalytic degradation;
fig. 9 shows the color change of the filter flask containing congo red solution before and after photocatalytic degradation.
Detailed Description
The first embodiment is as follows: the preparation method of the composite coating for resisting oil stain and degrading dye in the embodiment comprises the following steps:
1. dissolving dopamine in tris hydrochloride solution, and adding CuSO 4 ·5H 2 O and H 2 O 2 Immersing chemical fiber cotton, and stirring to obtain PDA@CFC; dopamine, cuSO 4 ·5H 2 O, tris hydrochloride solution and H 2 O 2 The mass volume ratio is 30-50mg:20-30mg:15-25mL:0.03-0.07mL;
2. immersing PDA@CFC into silver ammonia solution, and obtaining Ag/PDA@CFC after the reaction is completed;
3. mixing aniline and HCl solution to obtain mixed solution, immersing Ag/PDA@CFC into the mixed solution, stirring, dripping APS solution, and fully reacting to obtain the composite coating with oil stain resistance and degradation dye; the volume ratio of the aniline to the HCl solution is 1-1.2:620-760; the volume ratio of the APS solution to the HCl solution is 1:1-1.5.
The chemical fiber cotton in the present embodiment may be a polyester screen, a porous sponge or a cotton fabric.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: in the first step, the concentration of the tris hydrochloride solution was 50mM, and the pH was adjusted to 8.5 using NaOH solution. The other is the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: in step one, dopamine and CuSO 4 ·5H 2 The mass ratio of O is 0.04:0.0265. the other is the same as the first or second embodiment.
The specific embodiment IV is as follows: this embodiment differs from one of the first to third embodiments in that: step one, tris hydrochloride solution and H 2 O 2 Is 20:0.053. the other is the same as in one of the first to third embodiments.
Fifth embodiment: this embodiment differs from one to four embodiments in that: in the first step, stirring is carried out for 1h. The others are the same as in one to one fourth embodiments.
Specific embodiment six: this embodiment differs from one of the first to fifth embodiments in that: the preparation method of the silver ammonia solution comprises the following steps: will be 0.1g AgNO 3 Dissolved in 50mL of water, then aqueous ammonia was added dropwise until the brown precipitate disappeared. The others are the same as in one of the first to fifth embodiments.
Seventh embodiment: this embodiment differs from one of the first to sixth embodiments in that: in the second step, the reaction time is 12h. The others are the same as in one of the first to sixth embodiments.
Eighth embodiment: this embodiment differs from one of the first to seventh embodiments in that: in the step III, the volume ratio of aniline to HCl solution is 0.04:25, wherein the concentration of HCl solution is 1M. The other is the same as in one of the first to seventh embodiments.
Detailed description nine: this embodiment differs from one to eight of the embodiments in that: and step three, immersing the Ag/PDA@CFC into the mixed solution and stirring for 15min. The others are the same as in one to eight embodiments.
Detailed description ten: this embodiment differs from one of the embodiments one to nine in that: the preparation method of the APS solution in the third step comprises the following steps: 0.08g APS was dissolved in 25mL1M HCl aqueous solution. The others are the same as in one of the embodiments one to nine.
Example 1, preparation method of composite coating of greasy dirt resistance and degradation dye: 1. 40mg of Dopamine (DA) was dissolved in 20mL of 50mM Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) solution (pH adjusted to 8.5 with 1M NaOH solution), and 0.0265g of CuSO was then added 4· 5H 2 O and 53.2. Mu. LH 2 O 2 Immersing Chemical Fiber Cotton (CFC) and stirring for 1h to obtain PDA@CFC.
2. Immersing the PDA@CFC in silver ammonia solution, and reacting for 12 hours to obtain Ag/PDA@CFC; the preparation method of the silver ammonia solution comprises the following steps: 0.1g of AgNO3 was dissolved in 50mL of water, and then ammonia was slowly added dropwise until the brown precipitate disappeared;
3. adding 40 mu L of aniline into 25mL of 1MHCl aqueous solution to obtain a mixed solution, immersing Ag/PDA@CFC in the mixed solution, stirring for 15 minutes, dropwise adding APS solution, and fully reacting for 24 hours to obtain the multifunctional coating material PANI/Ag/PDA@CFC, namely the composite coating for resisting greasy dirt and degrading dye. The preparation method of the APS solution comprises the following steps: 0.08g APS was dissolved in 25mL1M HCl aqueous solution,
the microscopic morphological characterization of the composite coating against oil and degraded dye is shown in fig. 1: FIG. 1a shows the macroscopic fiber interlacing of PANI/Ag/PDA@CFC exhibiting a porous structure, and FIG. 1b shows the microscopic structure of PANI/Ag/PDA@CFC, with polyaniline exhibiting nanofibers covering the surface of the Ag nanoparticles.
Wetting properties of composite coatings (multifunctional coating materials PANI/Ag/pda@cfc) for grease resistance and degradation of dyes: the excellent hydrophilicity and underwater superoleophobicity of PANI/Ag/pda@cfc are shown in fig. 2, and the water drops rapidly dip into the surface for 1s, exhibiting excellent superhydrophilic properties.
The underwater oil contact angles of PANI/Ag/PDA@CFC for various organic solvents are shown in figure 3, and the PANI/Ag/PDA@CFC has general underwater super-oleophobic performance for the contact angles of high-density and low-density organic solvents (methylene dichloride, dichloroethane, chloroform, carbon tetrachloride, petroleum ether and n-hexane).
Degreasing properties of multifunctional coating material PANI/Ag/PDA@CFC: as shown in FIG. 4, for various oil stains floating on the water surface, the PANI/Ag/PDA@CFC accomplishes efficient oil stain removal by virtue of its large pore size and excellent super-hydrophilic/underwater super-oleophobic wetting characteristics. Oil-water separation is carried out by taking normal hexane, toluene, xylene, N-methylaniline, soybean oil, pump oil and petroleum ether as models and the same volume of deionized water. The PANI/Ag/PDA@CFC shows ultra-high flux and separation efficiency of more than 99%, and proves that the PANI/Ag/PDA@CFC can realize thorough greasy dirt removal.
Taking volatile toluene as an example, fig. 5 examines the cyclic cleaning capability of PANI/Ag/pda@cfc, and it can be found that the separation efficiency is basically unchanged after 10 cycles, thus proving that the catalyst has good recycling property.
Dye degradation capability of multifunctional coating material PANI/Ag/pda@cfc: the unique schottky heterojunction structure formed by PANI and AgNPs can be used for visible light catalytic degradation of organic dyes. The effect of visible light catalytic degradation is shown in fig. 6. The characteristic absorption peak of Methyl Orange (MO) at 464nm is clear and visible, after visible light catalytic degradation of MO is carried out by a PANI-AgNPs heterojunction structure, an almost smooth curve is obtained, and as can be seen in an illustration, the original MO presents orange yellow, a solution after visible light catalytic degradation presents colorless transparency, and the visible light catalytic degradation efficiency of PANI/Ag/PDA@CFC to MO is 99.7% after the absorbance at 464nm is calculated. Similarly, the visible light catalytic degradation efficiency of PANI/Ag/PDA@CFC on Congo Red (CR) is 99.3%.
Claims (8)
1. The preparation method of the composite coating for resisting oil stain and degrading dye is characterized by comprising the following steps:
dissolving dopamine in tris hydrochloride solution, and adding CuSO 4 ·5H 2 O and H 2 O 2 Immersing chemical fiber cotton, and stirring to obtain PDA@CFC; dopamine, cuSO 4 ·5H 2 O, tris hydrochloride solution and H 2 O 2 The mass volume ratio is 30-50mg:20-30mg:15-25mL:0.03-0.07mL; wherein the concentration of the tris hydrochloride solution is 50mM, and the pH is adjusted to 8.5 by using NaOH solution;
immersing PDA@CFC into silver ammonia solution, and obtaining Ag/PDA@CFC after the reaction is completed; the preparation method of the silver ammonia solution comprises the following steps: 0.1g AgNO 3 Dissolving in 50mL water, and then dripping ammonia until brown precipitate disappears;
mixing aniline and HCl solution to obtain mixed solution, immersing Ag/PDA@CFC into the mixed solution, stirring, dripping APS solution, and fully reacting to obtain the composite coating with oil stain resistance and degradation dye; the volume ratio of the aniline to the HCl solution is 1-1.2:620-760; the volume ratio of the APS solution to the HCl solution is 1:1-1.5.
2. The method for preparing the composite coating with oil stain resistance and degradation dye according to claim 1, wherein the method is characterized by comprising the following step oneMedium dopamine and CuSO 4 ·5H 2 The mass ratio of O is 0.04:0.0265.
3. the method for preparing a composite coating for oil stain resistance and degradation of dye according to claim 1, wherein in the step one, the solution of tris hydrochloride and H 2 O 2 Is 20:0.053.
4. the method for preparing the composite coating for resisting oil stains and degrading the dye according to claim 1, wherein the stirring is carried out for 1h in the first step.
5. The method for preparing the composite coating for resisting oil stains and degrading the dye according to claim 1, wherein the reaction time in the second step is 12 hours.
6. The method for preparing the composite coating for resisting oil stains and degrading dyes according to claim 1, wherein in the step three, the volume ratio of aniline to HCl solution is 0.04:25, wherein the concentration of HCl solution is 1M.
7. The method for preparing the composite coating with oil stain resistance and degradation dye according to claim 1, wherein in the third step, ag/PDA@CFC is immersed in the mixed solution and stirred for 15min.
8. The method for preparing the composite coating for resisting oil stains and degrading dyes according to claim 1, wherein the preparation method of the APS solution in the step three is as follows: 0.08g APS was dissolved in 25mL1M aqueous HCl.
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| CN105837841A (en) * | 2016-03-31 | 2016-08-10 | 常州大学 | Polydopamine-modified chitosan-based material and preparation method thereof |
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| CN109876188A (en) * | 2019-03-21 | 2019-06-14 | 浙江大学 | A kind of process for manufacturing intraocular lenses based on photothermal conversion prevention inverse position method |
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| WO2020006718A1 (en) * | 2018-07-04 | 2020-01-09 | 苏州大学张家港工业技术研究院 | Aramid fiber electrochemical capacitor and preparation method therefor |
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| CN105837841A (en) * | 2016-03-31 | 2016-08-10 | 常州大学 | Polydopamine-modified chitosan-based material and preparation method thereof |
| CN107812453A (en) * | 2017-10-31 | 2018-03-20 | 石狮市川大先进高分子材料研究中心 | A kind of preparation method of the biodegradable water-oil separationg film of multifunctional application |
| CN109364528A (en) * | 2018-12-11 | 2019-02-22 | 哈尔滨工程大学 | Multilevel structure water-oil separating material and preparation method thereof with pH responsiveness |
| CN109876188A (en) * | 2019-03-21 | 2019-06-14 | 浙江大学 | A kind of process for manufacturing intraocular lenses based on photothermal conversion prevention inverse position method |
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| 用于骨科植入体的纳米银/氧化钛纳米管复合抗菌涂层;方思懿;方明;李翔;;材料科学与工程学报(03);全文 * |
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