CN103740211B - A kind of preparation method of microporous nano coating - Google Patents
A kind of preparation method of microporous nano coating Download PDFInfo
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- CN103740211B CN103740211B CN201410039048.3A CN201410039048A CN103740211B CN 103740211 B CN103740211 B CN 103740211B CN 201410039048 A CN201410039048 A CN 201410039048A CN 103740211 B CN103740211 B CN 103740211B
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Abstract
The present invention relates to a kind of preparation method of microporous nano coating, it is characterized in that microporous nano coating comprises following component: (1) porous material, the content of described porous material is 1-40%.(2) nanoparticle, content is 1-40%, described nanoparticle be selected from nano-titanium oxide, nanometer silver, nano aluminum or its composition.(3) filmogen, content is 5-80%, and described filmogen is acrylic resin.(4) additive, described additive comprises the thickening material of 1-2% dispersion agent, 1-2% defoamer and 1-3%, and described thickening material is selected from, and molecular weight is the Natvosol of 3-10 ten thousand.(5) deionized water, the content of described deionized water is 5-15%.Make the nanoparticle of film inside also can play the effect of absorption and catalysis, be also conducive to the orderly release of antimicrobial substance simultaneously, thus make coating have effect of long-acting absorption degradation objectionable impurities and long acting antibiotic.
Description
Technical field
The invention belongs to nano material technology, be specifically related to a kind of preparation method of microporous nano coating.
Background technology
Composite nano materials is integrated together by the nano material of difference in functionality, thus the synergistic effect obtained outside single-material physico-chemical property, the absorption band gap of functionalization as easier in surface, more binding site, higher specific surface area, more high-k, change and catalytic activity etc.Wherein, the nano composite structure of metal and inorganics, because combine the high conductivity of metal and the intrinsic physical and chemical performance of inorganic materials, has wide investigation and application prospect (Shanghai Communications University's Ph D dissertation in 2009 in fields such as energy storage, Industrial Catalysis, function ceramics, bio-pharmaceuticals; Desalination, 2013,308:15 ~ 33).And in various nanostructure, porous material owing to having higher surface-area and being beneficial to the advantage such as duct of gas solution infiltration, and is widely studied application.Therefore, the porous nanometer structure of development of metallic/inorganic materials has important Research Significance and application prospect.
At present, nano material has started to have had in coating to apply widely.Because nanoparticle has quantum size effect, small-size effect, surface effects and macro quanta tunnel effect, thus show much special character.When these materials are added among traditional coating, just can good effect be produced, as long acting antibiotic performance, uv-shielding capacity, photocatalysis performance etc., and some inherent naturies simultaneously increasing coating, as film snappiness, coating hardness, sticking power, petrol-resistance, performances such as alkali-resistivity etc.Porous material of the present invention is the three-dimensional open-framework that carbon coated copper/metal oxide has nano-scale, product morphology is homogeneous, controlled, and preparation method is simple, with low cost, environmental friendliness, and it can be used as a component to add in coating, nanoparticle can easily be adsorbed and not easily absorption is agglomerating mutually by porous mass.The existence of porous mass, effective micro channel can be formed in coating, make the nanoparticle of film inside also can play the effect of absorption and catalysis, be also conducive to the orderly release of antimicrobial substance simultaneously, thus make coating have effect of long-acting absorption degradation objectionable impurities and long acting antibiotic.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of microporous nano coating, it is characterized in that described microporous nano coating comprises following component:
(1) porous material, the content of described porous material is 1-40%.
(2) nanoparticle, content is 1-40%, described nanoparticle be selected from nano-titanium oxide, nanometer silver, nano aluminum or its composition.
(3) filmogen, content is 5-80%, and described filmogen is acrylic resin.
(4) additive, described additive comprises the thickening material of 1-2% dispersion agent, 1-2% defoamer and 1-3%, and described thickening material is selected from, and molecular weight is the Natvosol of 3-10 ten thousand.
(5) deionized water, the content of described deionized water is 5-15%.
First the preparation of porous material:
Step one, chooses nanometal mixture
Described nanometal mixture is made up of nanometer zinc acetate and nanometer venus crystals powder, and the mol ratio of described zinc acetate and venus crystals is 2:1.
Step 2, the preparation of the first solution
The nanometal mixture of step one is mixed with tensio-active agent and ethylene glycol solution, mass ratio is: nanometal mixture: tensio-active agent: ethylene glycol solution=(4-6): (3-5): 300, mixed solution is stirred 10-30 minute with the speed of 600-1000r/min in 60-90 DEG C of oil bath, and naturally cooling obtains the first solution.
Step 3: the preparation of the second solution
Ethylene glycol and oxalic acid are mixed under normal temperature, obtained second solution, the mass ratio of described ethylene glycol and oxalic acid is 100:3.
Step 4: the preparation of composite precursor
By the dripping in fast the first solution instilled obtained by step 2 with 3-10mL/min of the second solution obtained by step 3, stir 4h with the speed 60-100 of 600-1000r/min DEG C of constant temperature; After reaction terminates, resultant of reaction is respectively washed 3 times, collected by centrifugation with deionized water and dehydrated alcohol respectively, and in baking oven, 80 DEG C of dry 6h, namely obtain composite precursor.The mass ratio of described second solution and the first solution is: 1:3-4.
Step 5: the preparation of the coated Cu/ZnO composite porous material of carbon
By composite precursor obtained by step 4 as in tube furnace, pass to the X/H2 atmosphere that hydrogen volume content is 1-10%, with the ramp to 200 DEG C of 5 DEG C/min, constant temperature keeps 2h, then rise to 500 DEG C with 5 DEG C/min, constant temperature keeps 2h, obtains the coated Cu/ZnO composite porous material of carbon, described X is nitrogen, argon gas, the one in helium that purity is not less than 99.9%, and the volume content of hydrogen is at 1%-10%.
Then, choose porous material, nanoparticle, filmogen, additive and deionized water by aforementioned component, and porous material is crossed 800 object sieves, be mixed in container, adopt mechanical stirring to mix, form stable coating.
2. the preparation method of microporous nano coating as claimed in claim 1, is characterized in that the particle diameter of described nanometer zinc acetate and nanometer venus crystals powder is 1-50nm, and the porosity of obtained porous material is more than 86%, and the size of hole is 1-25nm.
3. the preparation method of microporous nano coating as claimed in claim 1, it is characterized in that described tensio-active agent be selected from a kind of in polyvinylpyrrolidone (PVP), cetyl trimethylammonium bromide (CTAB), chlorination trimethylcetylammonium (CTAC), polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer (P123), polyoxyethylene-poly-oxypropylene polyoxyethylene triblock polymer (F127) or with arbitrarily than mixture.
4. the preparation method of microporous nano coating as claimed in claim 1, is characterized in that the particle diameter of described nanoparticle is 1-10nm.
Beneficial effect of the present invention is mainly:
Porous material of the present invention is the three-dimensional open-framework that carbon coated copper/metal oxide has nano-scale, product morphology is homogeneous, controlled, and preparation method is simple, with low cost, environmental friendliness, and it can be used as a component to add in coating, nanoparticle can easily be adsorbed and not easily absorption is agglomerating mutually by porous mass.The existence of porous mass, effective micro channel can be formed in coating, make the nanoparticle of film inside also can play the effect of absorption and catalysis, be also conducive to the orderly release of antimicrobial substance simultaneously, thus make coating have effect of long-acting absorption degradation objectionable impurities and long acting antibiotic.
Embodiment
A preparation method for microporous nano coating, is characterized in that described microporous nano coating comprises following component:
(1) porous material, the content of described porous material is 1-40%.
(2) nanoparticle, content is 1-40%, described nanoparticle be selected from nano-titanium oxide, nanometer silver, nano aluminum or its composition.
(3) filmogen, content is 5-80%, and described filmogen is acrylic resin.
(4) additive, described additive comprises the thickening material of 1-2% dispersion agent, 1-2% defoamer and 1-3%, and described thickening material is selected from, and molecular weight is the Natvosol of 3-10 ten thousand.
(5) deionized water, the content of described deionized water is 5-15%.
First the preparation of porous material:
Step one, chooses nanometal mixture
Described nanometal mixture is made up of nanometer zinc acetate and nanometer venus crystals powder, and described zinc acetate and venus crystals are respectively 0.02mol and 0.01mol.
Step 2, the preparation of the first solution
Mixed with 4g tensio-active agent and 300ml ethylene glycol solution by the nanometal mixture of step one, mixed solution is stirred 15 minutes with the speed of 800r/min in 80 DEG C of oil baths, naturally cooling obtains the first solution.
Step 3: the preparation of the second solution
100 ethylene glycol and 0.03mol oxalic acid are mixed under normal temperature, obtained second solution.
Step 4: the preparation of composite precursor
By the second solution obtained by step 3 with in the first solution obtained by a speed instillation step 2 of 5mL/min, stir 4h with speed 80 DEG C of constant temperature of 800r/min; After reaction terminates, resultant of reaction is respectively washed 3 times, collected by centrifugation with deionized water and dehydrated alcohol respectively, and in baking oven, 80 DEG C of dry 6h, namely obtain composite precursor.The mass ratio of described second solution and the first solution is: 1:3-4.
Step 5: the preparation of the coated Cu/ZnO composite porous material of carbon
By composite precursor obtained by step 4 as in tube furnace, pass to the X/H2 atmosphere that hydrogen volume content is 1-10%, with the ramp to 200 DEG C of 5 DEG C/min, constant temperature keeps 2h, then rise to 500 DEG C with 5 DEG C/min, constant temperature keeps 2h, obtains the coated Cu/ZnO composite porous material of carbon, described X is nitrogen, argon gas, the one in helium that purity is not less than 99.9%, and the volume content of hydrogen is at 1%-10%.
Choose the porous material that 800 object 40g are prepared above, 16g nano-titanium oxide, 4 grams of nano-silver powders, 80g acrylic resin, 3g dispersion agent and 3g defoamer, 4g Natvosol and 30g deionized water, as in container, adopt mechanical stirring to mix, form stable coating.Described coating has more micro channel, has long-acting absorption, the organic obnoxious flavour of catalyzed degradation and bactericidal property.Described coating water at normal temperature contact angle is greater than 120 degree
The particle diameter of described nanometer zinc acetate and nanometer venus crystals powder is 1-50nm, and the porosity of obtained porous material is more than 86%, and the size of hole is 1-25nm.
Described tensio-active agent be selected from a kind of in polyvinylpyrrolidone (PVP), cetyl trimethylammonium bromide (CTAB), chlorination trimethylcetylammonium (CTAC), polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer (P123), polyoxyethylene-poly-oxypropylene polyoxyethylene triblock polymer (F127) or with arbitrarily than mixture.
The particle diameter of described nanoparticle is 1-10nm.
The water-fast experimental results of GB/T1733-93 is 360 hours nothing difference;
Alcohol resistance (60% ethanolic soln) test result of GB1727-79 is 100 hours nothing difference.
Below in conjunction with specific embodiment technical scheme of the present invention done and introduce in detail further; but protection scope of the present invention is not limited thereto; those skilled in the art makes some nonessential improvement and adjustment according to the content of the invention described above, all belongs to scope.
Claims (1)
1. a preparation method for microporous nano coating, is characterized in that described microporous nano coating comprises following component:
(1) porous material, the content of described porous material is 1-40%;
(2) nanoparticle, content is 1-40%, and described nanoparticle is selected from nano-titanium oxide, nanometer silver, nano aluminum or its composition;
(3) filmogen, content is 5-80%, and described filmogen is acrylic resin;
(4) additive, described additive comprises the thickening material of 1-2% dispersion agent, 1-2% defoamer and 1-3%, and described thickening material is selected from, and molecular weight is the Natvosol of 3-10 ten thousand;
(5) deionized water, the content of described deionized water is 5-15%;
First the preparation of porous material:
Step one, chooses nanometal mixture
Described nanometal mixture is made up of nanometer zinc acetate and nanometer venus crystals powder, and the mol ratio of described zinc acetate and venus crystals is 2:1;
Step 2, the preparation of the first solution
The nanometal mixture of step one is mixed with tensio-active agent and ethylene glycol solution, mass ratio is: nanometal mixture: tensio-active agent: ethylene glycol solution=(4-6): (3-5): 300, mixed solution is stirred 10-30 minute with the speed of 600-1000r/min in 60-90 DEG C of oil bath, and naturally cooling obtains the first solution;
Step 3: the preparation of the second solution
Ethylene glycol and oxalic acid are mixed under normal temperature, obtained second solution, the mass ratio of described ethylene glycol and oxalic acid is 100:30;
Step 4: the preparation of composite precursor
By the dripping in fast the first solution instilled obtained by step 2 with 3-10mL/min of the second solution obtained by step 3, stir 4h with the speed 60-100 of 600-1000r/min DEG C of constant temperature; After reaction terminates, resultant of reaction is respectively washed 3 times, collected by centrifugation with deionized water and dehydrated alcohol respectively, and in baking oven, 80 DEG C of dry 6h, namely obtain composite precursor; The mass ratio of described second solution and the first solution is: 1:3-4;
Step 5: the preparation of the coated Cu/ZnO composite porous material of carbon
Composite precursor obtained by step 4 is placed in tube furnace, passes to the X/H that hydrogen volume content is 1-10%
2atmosphere, with the ramp to 200 DEG C of 5 DEG C/min, constant temperature keeps 2h, then rise to 500 DEG C with 5 DEG C/min, constant temperature keeps 2h, obtains the coated Cu/ZnO composite porous material of carbon, described X is nitrogen, argon gas, the one in helium that purity is not less than 99.9%, and the volume content of hydrogen is at 1%-10%;
Then, choose porous material, nanoparticle, filmogen, additive and deionized water by aforementioned component, and porous material is crossed 800 object sieves, be mixed in container, adopt mechanical stirring to mix, form stable coating;
The particle diameter of described nanometer zinc acetate and nanometer venus crystals powder is 1-50nm, and the porosity of obtained porous material is more than 86%, and the size of hole is 1-25nm;
Described tensio-active agent be selected from a kind of in polyvinylpyrrolidone, cetyl trimethylammonium bromide, chlorination trimethylcetylammonium, polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer or with arbitrarily than mixture;
The particle diameter of described nanoparticle is 1-10nm.
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| CN104530851B (en) * | 2014-12-17 | 2017-07-21 | 广州市侗富贵化工原材料有限公司 | A kind of multifunction surface inorganic agent and its application method |
| CN108627528A (en) * | 2018-05-02 | 2018-10-09 | 山东非金属材料研究所 | Nano silver reference materials for particle size analysis and preparation method thereof |
| CN111410888A (en) * | 2019-01-08 | 2020-07-14 | 上海先着点光电科技有限公司 | Preparation process of nano-silver coated zinc composite coating resistant to marine organism adhesion |
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| CN1216104C (en) * | 2002-03-12 | 2005-08-24 | 深圳市尊业纳米材料有限公司 | Microporous nano composite paint |
| DE102004014483A1 (en) * | 2004-03-24 | 2005-10-13 | Gesellschaft zur Förderung von Medizin-, Bio- und Umwelttechnologien e.V. | Coating composition, useful for antimicrobially coating and providing antimicrobial properties to substrates (e.g. papers, textiles), comprises porous inorganic coating contained in a homogenous distribution and a cationic polysaccharide |
| CN101322497B (en) * | 2008-07-08 | 2012-07-25 | 西南科技大学 | Active stephanoporate mineral TiO2-doped composite catalytic antimicrobial material preparation and using method |
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