CN103740211A - Method for preparing microporous type nano coating - Google Patents
Method for preparing microporous type nano coating Download PDFInfo
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- CN103740211A CN103740211A CN201410039048.3A CN201410039048A CN103740211A CN 103740211 A CN103740211 A CN 103740211A CN 201410039048 A CN201410039048 A CN 201410039048A CN 103740211 A CN103740211 A CN 103740211A
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Abstract
The invention relates to a method for preparing a microporous type nano coating. The microporous type nano coating is characterized by comprising the following components: (1) a porous material, wherein the content of the porous material is 1-40%, (2) nano particles, wherein the content of the nano particles is 1-40%, and the nano particles are selected from nano titanium oxide, nano silver, nano aluminum or other compositions, (3) a filming substance, wherein the content of the filming substance is 5-80%, and the filming substance is an acrylic resin, (4) an additive, wherein the additive comprises 1-2% of dispersing agent, 1-2% of defoaming agent and 1-3% of thickening agent; the thickening agent is selected from hydroxyethyl cellulose with the molecular weight of 30-100 thousand, and (5) deionized water, wherein the content of the deionized water is 5-15%. The functions of adsorption and catalysis of the nano particles inside the coating film can be brought into play, and meanwhile sequential emission of antibacterial substances is facilitated, so that the coating has the effects of long-lasting harmful substance adsorption and degradation and long-lasting antibiosis.
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
The nano material that composite nano materials is about to difference in functionality is integrated together, thereby obtain the synergistic effect 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, variation and catalytic activity etc.Wherein, the nano composite structure of metal and inorganics, because combine high conductivity and the intrinsic physical and chemical performance of inorganic materials of metal, has wide research 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 nanostructures, porous material is owing to having higher surface-area and being beneficial to the advantages such as duct of gas solution infiltration, and be 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 application widely in coating.Because nanoparticle has quantum size effect, small-size effect, surface effects and macro quanta tunnel effect, thereby show much special character.When these materials being added among traditional coating, just can produce good effect, as long acting antibiotic performance, uv-shielding capacity, photocatalysis performance etc., and increase some inherent naturies of coating simultaneously, as the snappiness of filming, 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 pattern homogeneous, controlled, and preparation method is simple, with low cost, environmental friendliness, and it is added in coating as a component, nanoparticle can easily be adsorbed and to be difficult for absorption mutually agglomerating by porous mass.The existence of porous mass, can in coating, form effective micro channel, the inner nanoparticle that makes to film also can be brought into play the effect of absorption and catalysis, and the while is also conducive to the orderly release of antimicrobial substance, thereby makes coating have the 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%, 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 1, chooses nano metal mixture
Described nano metal mixture is by nanometer zinc acetate and nanometer venus crystals phosphor composing, and the mol ratio of described zinc acetate and venus crystals is 2:1.
Step 2, the preparation of the first solution
The nano metal mixture of step 1 is mixed with tensio-active agent and ethylene glycol solution, mass ratio is: nano metal mixture: tensio-active agent: ethylene glycol solution=(4-6): (3-5): 300, mixed solution speed with 600-1000r/min in 60-90 ℃ of oil bath is stirred to 10-30 minute, and naturally cooling makes the first solution.
Step 3: the preparation of the second solution
Ethylene glycol and oxalic acid are mixed under normal temperature, make the second solution, the mass ratio of described ethylene glycol and oxalic acid is 100:3.
Step 4: the preparation of composite precursor
The speed of dripping by prepared the second solution of step 3 with 3-10mL/min splashes in prepared the first solution of step 2, with the speed 60-100 ℃ of constant temperature stirring 4h of 600-1000r/min; After reaction finishes, resultant of reaction is respectively washed 3 times with deionized water and dehydrated alcohol respectively, centrifugal collection, in baking oven, 80 ℃ of dry 6h, obtain composite precursor.The mass ratio of described the 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 the obtained composite precursor of step 4 as in tube furnace, passing to hydrogen volume content is the X/H2 atmosphere of 1-10%, speed with 5 ℃/min is warming up to 200 ℃, constant temperature keeps 2h, then with 5 ℃/min, rise to 500 ℃, constant temperature keeps 2h, obtains the coated Cu/ZnO composite porous material of carbon, described X is that purity is not less than a kind of in 99.9% nitrogen, argon gas, helium, and the volume content of hydrogen is at 1%-10%.
Then, by aforementioned component, choose porous material, nanoparticle, filmogen, additive and deionized water, and porous material is crossed to 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 prepared 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 trimethylammonium cetyltrimethyl ammonium (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, the particle diameter that it is characterized in that 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 pattern homogeneous, controlled, and preparation method is simple, with low cost, environmental friendliness, and it is added in coating as a component, nanoparticle can easily be adsorbed and to be difficult for absorption mutually agglomerating by porous mass.The existence of porous mass, can in coating, form effective micro channel, the inner nanoparticle that makes to film also can be brought into play the effect of absorption and catalysis, and the while is also conducive to the orderly release of antimicrobial substance, thereby makes coating have the 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%, 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 1, chooses nano metal mixture
Described nano metal mixture is by nanometer zinc acetate and nanometer venus crystals phosphor composing, and described zinc acetate and venus crystals are respectively 0.02mol and 0.01mol.
Step 2, the preparation of the first solution
The nano metal mixture of step 1 is mixed with 4g tensio-active agent and 300ml ethylene glycol solution, mixed solution speed with 800r/min in 80 ℃ of oil baths is stirred 15 minutes, naturally cooling makes the first solution.
Step 3: the preparation of the second solution
100 ethylene glycol and 0.03mol oxalic acid are mixed under normal temperature, make the second solution.
Step 4: the preparation of composite precursor
The speed of dripping by prepared the second solution of step 3 with 5mL/min splashes in prepared the first solution of step 2, with 80 ℃ of constant temperature stirring 4h of speed of 800r/min; After reaction finishes, resultant of reaction is respectively washed 3 times with deionized water and dehydrated alcohol respectively, centrifugal collection, in baking oven, 80 ℃ of dry 6h, obtain composite precursor.The mass ratio of described the 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 the obtained composite precursor of step 4 as in tube furnace, passing to hydrogen volume content is the X/H2 atmosphere of 1-10%, speed with 5 ℃/min is warming up to 200 ℃, constant temperature keeps 2h, then with 5 ℃/min, rise to 500 ℃, constant temperature keeps 2h, obtains the coated Cu/ZnO composite porous material of carbon, described X is that purity is not less than a kind of in 99.9% nitrogen, argon gas, helium, 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, and 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 prepared 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 trimethylammonium cetyltrimethyl ammonium (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;
The alcohol resistance of GB1727-79 (60% ethanolic soln) test result is 100 hours nothing difference.
Below in conjunction with specific embodiment, technical scheme of the present invention is done further and introduced in detail; but protection scope of the present invention is not limited to this; those skilled in the art makes some nonessential improvement and adjustment according to the content of the invention described above, all belongs to protection domain of the present invention.
Claims (4)
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%, described nanoparticle be selected from nano-titanium oxide, nanometer
Silver, nano aluminum or its composition.
(3) filmogen, content is 5-80%, described filmogen is acrylic resin.
(4) additive, described additive comprises the thickening of 1-2% dispersion agent, 1-2% defoamer and 1-3%
Agent, 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 1, chooses nano metal mixture
Described nano metal mixture is by nanometer zinc acetate and nanometer venus crystals phosphor composing, and the mol ratio of described zinc acetate and venus crystals is 2:1.
Step 2, the preparation of the first solution
The nano metal mixture of step 1 is mixed with tensio-active agent and ethylene glycol solution, mass ratio is: nano metal mixture: tensio-active agent: ethylene glycol solution=(4-6): (3-5): 300, mixed solution speed with 600-1000r/min in 60-90 ℃ of oil bath is stirred to 10-30 minute, and naturally cooling makes the first solution.
Step 3: the preparation of the second solution
Ethylene glycol and oxalic acid are mixed under normal temperature, make the second solution, the mass ratio of described ethylene glycol and oxalic acid is 100:3.
Step 4: the preparation of composite precursor
The speed of dripping by prepared the second solution of step 3 with 3-10mL/min splashes in prepared the first solution of step 2, with the speed 60-100 ℃ of constant temperature stirring 4h of 600-1000r/min; After reaction finishes, resultant of reaction is respectively washed 3 times with deionized water and dehydrated alcohol respectively, centrifugal collection, in baking oven, 80 ℃ of dry 6h, obtain composite precursor.The mass ratio of described the 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 the obtained composite precursor of step 4 as in tube furnace, passing to hydrogen volume content is the X/H2 atmosphere of 1-10%, speed with 5 ℃/min is warming up to 200 ℃, constant temperature keeps 2h, then with 5 ℃/min, rise to 500 ℃, constant temperature keeps 2h, obtains the coated Cu/ZnO composite porous material of carbon, described X is that purity is not less than a kind of in 99.9% nitrogen, argon gas, helium, and the volume content of hydrogen is at 1%-10%.
Then, by aforementioned component, choose porous material, nanoparticle, filmogen, additive and deionized water, and porous material is crossed to 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 prepared 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 trimethylammonium cetyltrimethyl ammonium (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, the particle diameter that it is characterized in that described nanoparticle is 1-10nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530851A (en) * | 2014-12-17 | 2015-04-22 | 谭树隆 | Multifunctional surface treating agent and use method thereof |
| 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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| CN1369529A (en) * | 2002-03-12 | 2002-09-18 | 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 |
| CN101322497A (en) * | 2008-07-08 | 2008-12-17 | 西南科技大学 | Active stephanoporate mineral TiO2-doped composite catalytic antimicrobial material preparation and using method |
| CN103268929A (en) * | 2013-06-04 | 2013-08-28 | 山东大学 | Carbon/copper/metal oxide composite porous material and preparation method and application thereof |
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2014
- 2014-01-26 CN CN201410039048.3A patent/CN103740211B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1369529A (en) * | 2002-03-12 | 2002-09-18 | 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 |
| CN101322497A (en) * | 2008-07-08 | 2008-12-17 | 西南科技大学 | Active stephanoporate mineral TiO2-doped composite catalytic antimicrobial material preparation and using method |
| CN103268929A (en) * | 2013-06-04 | 2013-08-28 | 山东大学 | Carbon/copper/metal oxide composite porous material and preparation method and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530851A (en) * | 2014-12-17 | 2015-04-22 | 谭树隆 | Multifunctional surface treating agent and use method thereof |
| 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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