CN107033650B - A kind of preparation method of antifouling antibacterial composite coating - Google Patents
A kind of preparation method of antifouling antibacterial composite coating Download PDFInfo
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- CN107033650B CN107033650B CN201710315980.8A CN201710315980A CN107033650B CN 107033650 B CN107033650 B CN 107033650B CN 201710315980 A CN201710315980 A CN 201710315980A CN 107033650 B CN107033650 B CN 107033650B
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- 238000000576 coating method Methods 0.000 title claims abstract description 44
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 43
- 230000003373 anti-fouling effect Effects 0.000 title claims abstract description 43
- 239000011248 coating agent Substances 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 176
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 123
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 80
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 42
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 42
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 42
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 42
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 42
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 38
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 32
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 19
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims abstract description 11
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 9
- 230000002378 acidificating effect Effects 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 3
- 229910000077 silane Inorganic materials 0.000 claims abstract description 3
- 235000019441 ethanol Nutrition 0.000 claims description 88
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 65
- 238000003756 stirring Methods 0.000 claims description 37
- 239000007788 liquid Substances 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- -1 perfluoroalkyl silanes Chemical class 0.000 claims description 21
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 20
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine group Chemical group NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 20
- 239000012153 distilled water Substances 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 13
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 9
- 239000012265 solid product Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 125000003545 alkoxy group Chemical group 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000011806 microball Substances 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 claims description 3
- 238000005903 acid hydrolysis reaction Methods 0.000 claims description 2
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical group FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 125000000217 alkyl group Chemical group 0.000 claims 1
- 239000002077 nanosphere Substances 0.000 claims 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 claims 1
- 125000005010 perfluoroalkyl group Chemical group 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 22
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 12
- 230000003670 easy-to-clean Effects 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 8
- 241000588724 Escherichia coli Species 0.000 description 7
- 241000191967 Staphylococcus aureus Species 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 238000004821 distillation Methods 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 4
- 239000003981 vehicle Substances 0.000 description 4
- 238000005034 decoration Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 235000015203 fruit juice Nutrition 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000001408 fungistatic effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1606—Antifouling paints; Underwater paints characterised by the anti-fouling agent
- C09D5/1612—Non-macromolecular compounds
- C09D5/1618—Non-macromolecular compounds inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The present invention relates to a kind of preparation methods of antifouling antibacterial composite coating, comprising the following steps: (1) disperses formation solution (A) in alcohol/aqueous solution for ethyl orthosilicate；Ammonium hydroxide is added in alcohol, is formed alcohol ammonia solution (B)；Alcohol ammonia solution (B) is added in solution (A) and is stirred；It is then allowed to stand to obtain the nanometer spherical SiO in solution (C) and solution (C)2Particle；(2) by Nano-meter SiO_2 obtained above2Microballoon is scattered in containing SnCl2·2H2Sensitized treatment is carried out in the acidic aqueous solution of O, obtains being adsorbed with Sn2+SiO2Microballoon (D), will be adsorbed with Sn2+SiO2Microballoon (D) is dispersed in water and AgNO is added3Solution and reducing agent obtain carrying Ag Nano-meter SiO_22Microballoon；(3) by load Ag Nano-meter SiO_2 obtained above2Microballoon is scattered in alcohol solution, and the hydrolyzed silane solution containing perfluoroalkyl is then added into the solution, obtains antifouling antibacterial composite coating.
Description
Technical field
The invention belongs to antifouling antibacterial technical field of paint preparation, more particularly to a kind of Car-use Fabric surface that is used for prevent
The coating of dirty antibacterial processing.
Background technique
Automotive interior is the environment relatively sealed, it is easy to breed a large amount of bacterium, especially trickle down in vehicle
The sweat stain etc. that interior fruit juice, swill and hand contact site leaves creates condition for the breeding of bacterium.Hand frequently contacts
Position and air-conditioner air outlet germ contamination are the most serious, such as steering wheel, shift handle, seat, handle, air outlet, and vehicle age
Longer, interior body surface total plate count is higher.It shows according to investigations, the private car in 1 year and 3 years vehicle ages, steering wheel, shift hand
Total number of bacteria at handle and air-conditioner air outlet three is respectively 95000 cfu/cm2、210900 cfu/cm2、83000 cfu/cm2With
122000 cfu/cm2、237000 cfu/cm2、90100 cfu/cm2, much higher than common objects surface colony sum reference value (<
500 cfu/cm2), it is occupant's health care belt to endanger.
Currently, solved to solve the problems, such as that interior total number of bacteria is severely exceeded frequently with the method for medicinal alcohol wiping, but
It is, although total plate count meeting rapid drawdown after being wiped using medicinal alcohol, for its inside gadget surface colony of the car compared with long vehicle age
Sum still exceeds standard reference value.In addition, having the hydrophobic product for Car-use Fabric on the market, after such product
The processing easy to clean such as the fruit juice on its surface is trickled down, but still cannot fundamentally solve the problems, such as bacterial reproduction；A kind of commercially available light
Catalysis automatically cleaning product can play the role of sterilization and decomposing organic matter after automobile interior decoration coating, but such product needs purple
Outer light irradiation excitation, effect are limited.In view of the deficiencies of the prior art, propose that a kind of antifouling antibacterial composite coating is used to control automobile
The solution of inside gadget surface colony sum.
Summary of the invention
In order to solve above-mentioned technical problem, the present invention devises a kind of preparation side of antifouling antibacterial composite coating
Method can form sterilization nonpolluting coating on automotive upholstery surface.
In order to solve above-mentioned technical problem, present invention employs following scheme:
A kind of preparation method of antifouling antibacterial composite coating, which comprises the following steps:
(1) Nano-meter SiO_2 is prepared2Microballoon: it disperses ethyl orthosilicate in alcohol/aqueous solution and forms solution A；Ammonium hydroxide is added
In alcohol, alcohol ammonia solution B is formed；Alcohol ammonia solution B is added in solution A and is stirred；It is then allowed to stand, obtains being dispersed with nanometer spherical
The solution (C) of SiO2 particle separates the solution (C) for being dispersed with nanometer spherical SiO2 particle, obtains nanometer spherical SiO2
Particle；
(2) preparation carries Ag Nano-meter SiO_22Microballoon: by Nano-meter SiO_2 obtained above2Microballoon is scattered in containing SnCl2·2H2O's
Sensitized treatment is carried out in acidic aqueous solution, is stood, and separation obtains being adsorbed with Sn2+SiO2Microballoon D will be adsorbed with Sn2+SiO2
Microballoon D is dispersed in water and AgNO is added3Solution and reducing agent are stood, separation, obtain carrying Ag Nano-meter SiO_22Microballoon；
(3) by load Ag Nano-meter SiO_2 obtained above2Microballoon is scattered in alcohol solution, is then added and is contained into the solution
There is a hydrolyzed silane solution of perfluoroalkyl, realizes perfluoroalkyl silanes to being loaded with Ag nano particles SiO2The surface modification of microballoon, obtains
To antifouling antibacterial composite coating.
Further, the solution A in step (1), mass ratio shared by water are 0.4%~2.6%, mass ratio shared by ethyl orthosilicate
It is 1.8%~2.0%, surplus is alcohol.
Further, in step (1), NH in alcohol ammonia solution B3Mass percentage is 3.1%~7.2%, and surplus is alcohol.
Further, in step (1), at room temperature, alcohol ammonia solution B is added in solution A and is given simultaneously and is stirred, stirring speed
Degree is 500~1000 turns/min；Alcohol ammonia solution B is added completely into after solution A persistently stirs 30~120min again.
Further, alcohol ammonia solution B is added dropwise in addition solution A in step (1) with the speed of 20~45 μ l/min.
Further, in step (1), alcohol ammonia solution B is added in solution A after persistently stirring, opening stands 24~72h and obtains
Solution C is centrifugated and 1~3 hour dry at 100~180 DEG C to obtained solid product by solution C, and obtaining partial size is 10
The Nano-meter SiO_2 of~75nm2Microballoon.
Further, in step (2), by SnCl2·2H2O is added in acidic aqueous solution and forms SnCl2Mass percentage is
0.08%~0.12% solution, with 800~1200 revs/min of revolving speed, after 15~30 minutes solution of magnetic agitation thereto
Nano-meter SiO_2 is added2Microballoon, then magnetic agitation disperse 30~60 minutes formation mixed solutions, SiO in mixed solution2Microspheres quality hundred
Dividing content is 0.15%~0.25%；Gained mixed solution is stood, is then centrifuged for isolated being adsorbed with Sn2+SiO2Microballoon D.
Further, in step (2), the acidic aqueous solution is hydrochloric acid deionized water solution, pH value 2.5.
Further, in step (2), Sn will be adsorbed with2+SiO2Microballoon D is scattered in deionized water or distilled water, absorption
There is Sn2+SiO2The additional amount and deionized water of microballoon D or the mass ratio of distilled water are 1:5, and AgNO3 solution is then added,
The mass ratio of AgNO3 and the aqueous solution for the SiO2 microballoon D for being adsorbed with Sn2+ in middle AgNO3 solution are 0.005:1~0.032:
After 1, stirring 30~90 minutes, reducing agent is added, is stirred for 1~3 hour after adding reducing agent, then, is centrifugally separating to obtain
Load has the Nano-meter SiO_2 of Ag particle2Microballoon, wherein the mass percentage of silver carrying amount is 5%~8%.
Further, in step (2), AgNO3 solution and reducing agent are added in a manner of dropwise addition.
Further, the reducing agent is hydrazine or formaldehyde, the additional amount and AgNO of reducing agent3Molar ratio be 1:1.4~
1:2.0.
Further, in step (3), above-mentioned load Ag there is into nanoparticle SiO2Microballoon, which is scattered in alcohol solution, forms solid content
10%~20% solution I；Perfluoroalkyl silanes are added in alcohol solution, and appropriate acid-catalyzed hydrolysis is added, obtain solution II；
Solution I is mixed according to a certain percentage with solution II, obtains antifouling antibacterial composite coating；In this step, alcohol in alcohol solution
It is 8:1~14:1 with water mixed volume ratio.
Further, in step (3), perfluoroalkyl silanes and alcohol/aqueous solution are mixed, wherein matter shared by perfluoroalkyl silanes
For amount than being 1.5%~3%, it is 4.5~6 that acid, which is then added, and adjusts the solution ph, small with 200~500 revs/min of stirrings 4~24
When obtain solution II；The perfluoroalkyl silanes structural formula are as follows:
It is 1~3, a is 0~2 that wherein m, which is 2~30, n,；For perfluor carbochain or perfluoroether chain,For hydrolyzable groups halogen
Dai Ji or alkoxy；ForOr alkoxy；The acid is the mixture of one of acetic acid, citric acid or both.
Further, in step (3), the perfluoroalkyl silanes structural formula are as follows:
Wherein the value range of m is 2~30, preferably n=1, preferably a=0 or 1, most preferably a=0；For perfluor carbochain or entirely
Fluorinated ether chain, such asOrOr；For can water
Group halo or alkoxy are solved,ForOr alkoxy, under acid catalysis,In halogeno-groupAnd alcoxyl
BaseIt hydrolyzes, forms the silanol with the Long carbon chain containing F。
Further, solution I is mixed with solution II according to mass ratio 1:1~1:2, with 200~500 revs/min stirring 0.5~
4 hours.
Further, the water is deionized water or distilled water；The alcohol is ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol
One of or wherein several mixtures.
The preparation method of the antifouling antibacterial composite coating has the advantages that
(1) present invention uses Nano-meter SiO_22Microballoon is carrier, deposits nano-Ag particles on its surface, and with perfluoroalkyl silicon
Alkane hydrolysate perfluoroalkyl modifies its surface, obtains having hydrophobic and fungistatic effect nanocomposite.Using
Alcohol/aqueous solution containing the nanocomposite often touches position to automotive upholstery and carries out plated film, and average water contact can be obtained
Angle is remarkably improved automotive upholstery not less than 110 °, the film layer of staphylococcus aureus and 95% or more Escherichia coli bacteriostasis rate
Property easy to clean and reduce inside gadget surface total plate count.
(2) SiO of the present invention2It is microsphere supported while being loaded with hydrophobic grouping and nanometer Ag, in the form of a paint using assigning simultaneously
Give that automobile interior decoration is antifouling and bacteriostasis, the technology raw material sources extensively, using simple, significant effect.
Detailed description of the invention
Fig. 1: the antifouling antibacterial composite coating preparation process flow of the present invention.
Specific embodiment
With reference to the accompanying drawing and embodiment, the present invention will be further described:
Embodiment one: the present embodiment provides a kind of preparation methods of antifouling antibacterial composite coating, comprising the following steps:
(1) it disperses ethyl orthosilicate in ethanol distillation water mixed liquid and obtains solution A, wherein ethyl orthosilicate quality hundred
Dividing content is 1.88%, and distilled water mass percentage is 2.53%, and surplus is ethyl alcohol；By concentrated ammonia liquor (concentration 28%-30%, with
It similarly hereinafter) is added in ethyl alcohol, obtains NH3The alcohol ammonia solution B that mass percentage is 6.60%；By alcohol ammonia solution B with 20 μ l/min's
Speed is added in solution A, while being stirred with 1000 revs/min, persistently stirs 30 after alcohol ammonia solution B is all added in solution A
Minute, then open standing obtains solution C in 24 hours, solution C is centrifugated, then by obtained solid product at 100 DEG C
It is 3 hours dry, obtain the SiO that partial size is about 75nm2Microballoon.
(2) by SnCl2·2H2O is added in aqueous hydrochloric acid solution, forms SnCl2The solution that mass percentage is 0.08%, it is molten
Liquid pH value was 2.5, with mixing speed magnetic agitation 15 minutes of 800 revs/min；Then Nano-meter SiO_2 is added2Microballoon, SiO2Microballoon
Additional amount accounts for the 0.15% of solution gross mass, is persistently dispersed with stirring 30~60 minutes, stands 30 minutes after stirring, centrifugation point
From obtaining being adsorbed with Sn2+SiO2Microballoon D.
(3) it disperses product D in deionized water, the additional amount of product D and the mass ratio of deionized water are 1:5, then
The AgNO of 6mmol/L is added dropwise3Solution, wherein AgNO3AgNO in solution3Be adsorbed with Sn2+SiO2Microballoon D's is water-soluble
The mass ratio of liquid is 0.01:1, after stirring 30~90 minutes, then formaldehyde is added dropwise into solution, formaldehyde additional amount and AgNO3
Molar ratio be 1:2.0, be stirred for 1~3 hour after adding reducing agent, be then centrifuged, obtain product E, that is, load
There is the Nano-meter SiO_2 of Ag particle2Microballoon, carrying Ag amount (mass percentage) is about 5%~8%.
(4) SiO of Ag nano particles will be loaded with2Microballoon E, which is scattered in ethyl alcohol/deionized water solution, to be formed admittedly
The solution I of content 10%~20%, wherein alcohol and deionized water mixed volume ratio are 8:1~14:1；By perfluoroalkyl silanesIt is mixed with ethyl alcohol/deionized water solution, wherein perfluoroalkyl silanes institute
Account for mass ratio be 1.5%~3%, then be added acetic acid adjust solution ph be 4.5~6, with 200~500 revs/min stirring 4~
Obtain solution II within 24 hours, wherein alcohol and water mixed volume ratio are 8~14:1；Solution I and solution II are mixed according to mass ratio 1:1
It closes, is stirred 0.5 hour with 200 revs/min and obtain antifouling antibacterial composite coating.
Position is often touched to automotive upholstery using the antifouling antibacterial composite coating and carries out plated film, average water contact can be obtained
Angle is about the film layer of 111 °, staphylococcus aureus bacteriostasis rate 96%, Escherichia coli bacteriostasis rate 99%, is remarkably improved automobile interior decoration
The property easy to clean of part and the total plate count for reducing inside gadget surface.
Embodiment two: the present embodiment provides a kind of preparation methods of antifouling antibacterial composite coating, comprising the following steps:
(1) it disperses ethyl orthosilicate in ethanol distillation water mixed liquid and obtains solution A, wherein ethyl orthosilicate quality hundred
Dividing content is 1.90%, and distilled water mass percentage is 1.63%, and surplus is ethyl alcohol；Concentrated ammonia liquor is added in ethyl alcohol, NH is obtained3
The alcohol ammonia solution B that mass percentage is 5.55%；Alcohol ammonia solution B is added in solution A with the speed of 25 μ l/min, while with
800 revs/min of stirrings are persistently stirred 60 minutes after alcohol ammonia solution B is all added in solution A, then open to stand 48 hours
Solution C is obtained, solution C is centrifugated, then that obtained solid product is 1.5 hours dry at 120 DEG C, obtaining partial size is about
The SiO of 63nm2Microballoon.
(2) by SnCl2·2H2O is added in aqueous hydrochloric acid solution, forms SnCl2The solution that mass percentage is 0.10%, it is molten
Liquid pH value was 2.5, with mixing speed magnetic agitation 18 minutes of 900 revs/min；Then system is added obtains Nano-meter SiO_22Microballoon,
SiO2Microballoon additional amount accounts for the 0.18% of solution gross mass, is persistently dispersed with stirring 40 minutes, stands 30 minutes after stirring, from
The heart is isolated to be adsorbed with Sn2+SiO2Microballoon D.
(3) it disperses product D in deionized water, the additional amount of product D and the mass ratio of deionized water are 1:5, then
The AgNO3 solution of 6mmol/L is added dropwise, wherein the water of the AgNO3 in AgNO3 solution and the SiO2 microballoon D for being adsorbed with Sn2+
The mass ratio of solution is 0.013:1, after stirring 50 minutes, then formaldehyde is added dropwise into the solution, formaldehyde additional amount and AgNO3
Molar ratio be 1:1.6, be stirred for 1.5 hours after adding reducing agent, be then centrifuged, obtain product E, i.e., load have
The Nano-meter SiO_2 of Ag particle2Microballoon, silver carrying amount (mass percentage) is about 6.2%.
(4) Ag nano particles SiO will be loaded with2Microballoon, which is scattered in ethyl alcohol/deionized water solution, forms the molten of solid content 15%
Liquid I, wherein alcohol and water mixed volume ratio are 9:1；By perfluoroalkyl silanes
With ethyl alcohol/deionized water solution mixing, wherein mass ratio shared by perfluoroalkyl silanes is 1.8%, and second acid-conditioning solution is then added
PH value is 5, is stirred 6 hours with 300 revs/min and obtains solution II, and wherein alcohol and water mixed volume ratio are 9:1；By solution I with it is molten
Liquid II is mixed according to mass ratio 1:1.5, is stirred 1 hour with 400 revs/min and is obtained antifouling antibacterial composite coating.
Position is often touched to automotive upholstery using the antifouling antibacterial composite coating and carries out plated film, it is flat that water contact angle can be obtained
It is the film layer of 114 °, staphylococcus aureus bacteriostasis rate 96.8%, Escherichia coli bacteriostasis rate 99.5%, is remarkably improved in automobile
The property easy to clean of gadget and the total plate count for reducing inside gadget surface.
Embodiment three: the present embodiment provides a kind of antifouling antibacterial composite coating preparation methods, comprising the following steps:
(1) it disperses ethyl orthosilicate in ethanol distillation water mixed liquid and obtains solution A, wherein ethyl orthosilicate quality hundred
Dividing content is 1.91%, and distilled water mass percentage is 1.03%, and surplus is ethyl alcohol；Concentrated ammonia liquor is added in ethyl alcohol, NH is obtained3
The alcohol ammonia solution B that mass percentage is 4.39%；Alcohol ammonia solution B is added in solution A with the speed of 30 μ l/min, while with
500 revs/min of stirrings are persistently stirred 90 minutes after alcohol ammonia solution B is all added in solution A, then open to stand 48 hours
Solution C is obtained, solution C is centrifugated, then that obtained solid product is 3 hours dry at 100 DEG C, obtaining partial size is about
The SiO of 24nm2Microballoon.
(2) by SnCl2·2H2O is added in aqueous hydrochloric acid solution, forms SnCl2The solution that mass percentage is 0.12%, it is molten
Liquid pH value was 2.5, with mixing speed magnetic agitation 15 minutes of 1100 revs/min；Then nanometer obtained in step on being added
SiO2Microballoon, SiO2Microballoon additional amount accounts for the 0.20% of solution gross mass, is persistently dispersed with stirring 60 minutes, 30 are stood after stirring
Minute, it is centrifugally separating to obtain and is adsorbed with Sn2+SiO2Microballoon D.
(3) it disperses product D in deionized water, the additional amount of product D and the mass ratio of deionized water are 1:5, then
The AgNO3 solution of 6mmol/L is added dropwise, wherein the water of the AgNO3 in AgNO3 solution and the SiO2 microballoon D for being adsorbed with Sn2+
The mass ratio of solution is 0.014:1, after stirring 70 minutes, then hydrazine is added dropwise into solution, hydrazine additional amount and AgNO3's
Molar ratio is to be stirred for 3 hours after 1:1.8 adds reducing agent, is then centrifuged, obtains product E, i.e. load has Ag
The Nano-meter SiO_2 of grain2Microballoon, silver carrying amount (mass percentage) is about 7%.
(4) Ag nano particles SiO will be loaded with2Microballoon, which is scattered in isopropanol/distilled water solution, forms the molten of solid content 20%
Liquid I, wherein alcohol and water mixed volume ratio are 14:1；By perfluoroalkyl silanes
With isopropanol/distilled water solution mixing, wherein mass ratio shared by perfluoroalkyl silanes is 3%, and citric acid regulating solution is then added
PH value is 5.5, is stirred 24 hours with 500 revs/min and obtains solution II, and wherein alcohol and water mixed volume ratio are 14:1；By solution I
It is mixed with solution II according to mass ratio 1:2, is stirred 4 hours with 500 revs/min and obtain antifouling antibacterial composite coating.
Position is often touched to automotive upholstery using the antifouling antibacterial composite coating and carries out plated film, average water contact can be obtained
Angle is about the film layer of 116 °, staphylococcus aureus bacteriostasis rate 98%, Escherichia coli bacteriostasis rate 100%, is remarkably improved in automobile
The property easy to clean of gadget and the total plate count for reducing inside gadget surface.
Example IV: the present embodiment provides a kind of antifouling antibacterial composite coating preparation methods, comprising the following steps:
(1) it disperses ethyl orthosilicate in ethanol distillation water mixed liquid and obtains solution A, wherein ethyl orthosilicate quality hundred
Dividing content is 1.92%, and distilled water mass percentage is 0.41%, and surplus is ethyl alcohol；Concentrated ammonia liquor is added in ethyl alcohol, NH is obtained3
The alcohol ammonia solution B that mass percentage is 3.09%；Solution B is added in solution A with the speed of 45 μ l/min, while with 600
Turn/min stirring, persistently stir 120min after solution B is all added in solution A, then open stand obtains solution C for 24 hours, will
Solution C centrifuge separation, it is then that obtained solid product is 1.5 hours dry at 120 DEG C, obtain the SiO that partial size is about 15nm2It is micro-
Ball.
(2) by SnCl2·2H2O is added in aqueous hydrochloric acid solution, forms SnCl2The solution that mass percentage is 0.12%, it is molten
Liquid pH value was 2.5, with mixing speed magnetic agitation 20 minutes of 1200 revs/min;Then Nano-meter SiO_2 obtained is walked on being added2
Microballoon, SiO2Microballoon additional amount accounts for the 0.25% of solution gross mass, is persistently dispersed with stirring 60 minutes, and 30 points are stood after stirring
Clock is centrifugally separating to obtain and is adsorbed with Sn2+SiO2Microballoon D.
(3) it disperses product D in deionized water, the additional amount of product D and the mass ratio of deionized water are 1:5, then
The AgNO3 solution of 6mmol/L is added dropwise, wherein the water of the AgNO3 in AgNO3 solution and the SiO2 microballoon D for being adsorbed with Sn2+
The mass ratio of solution is 0.016:1, after stirring 90 minutes, then hydrazine is added dropwise into solution, hydrazine additional amount and AgNO3's
Molar ratio is to be stirred for 3 hours after 1:2.0 adds reducing agent, is then centrifuged, obtains product E, i.e. load has Ag
The Nano-meter SiO_2 of grain2Microballoon, silver carrying amount (mass content) is about 8%.
(4) Ag nano particles SiO will be loaded with2Microballoon, which is scattered in isopropanol/distilled water solution, forms the molten of solid content 20%
Liquid I, wherein alcohol and water mixed volume ratio are 14:1；By perfluoroalkyl silanes
With isopropanol/distilled water solution mixing, wherein mass ratio shared by perfluoroalkyl silanes is 2.8%, and it is molten that citric acid adjusting is then added
Liquid pH value is 5.4, is stirred 24 hours with 500 revs/min and obtains solution II, and wherein alcohol and water mixed volume ratio are 14:1；It will be molten
Liquid I is mixed with solution II according to mass ratio 1:2, is stirred 4 hours with 500 revs/min and is obtained antifouling antibacterial composite coating.
Position is often touched to automotive upholstery using the antifouling antibacterial composite coating and carries out plated film, average water contact can be obtained
Angle is about the film layer of 113 °, staphylococcus aureus bacteriostasis rate 99%, Escherichia coli bacteriostasis rate 100%, is remarkably improved in automobile
The property easy to clean of gadget and the total plate count for reducing inside gadget surface.
Embodiment five: the present embodiment provides a kind of antifouling antibacterial composite coating preparation methods, comprising the following steps:
(1) it disperses ethyl orthosilicate in ethanol distillation water mixed liquid and obtains solution A, wherein ethyl orthosilicate quality hundred
Dividing content is 1.92%, and distilled water mass percentage is 0.41%, and surplus is ethyl alcohol；Concentrated ammonia liquor is added in ethyl alcohol, NH is obtained3
The alcohol ammonia solution B that mass percentage is 3.09%；Solution B is added in solution A with the speed of 45 μ l/min, while with 600
Turn/min stirring, persistently stir 120min after solution B is all added in solution A, then open stand obtains solution C for 24 hours, will
Solution C centrifuge separation, it is then that obtained solid product is 1.5 hours dry at 120 DEG C, obtain the SiO that partial size is about 15nm2It is micro-
Ball.
(2) by SnCl2·2H2O is added in aqueous hydrochloric acid solution, forms SnCl2The solution that mass percentage is 0.12%, it is molten
Liquid pH value was 2.5, with mixing speed magnetic agitation 20 minutes of 1200 revs/min;Then Nano-meter SiO_2 obtained is walked on being added2
Microballoon, SiO2Microballoon additional amount accounts for the 0.25% of solution gross mass, is persistently dispersed with stirring 60 minutes, and 30 points are stood after stirring
Clock is centrifugally separating to obtain and is adsorbed with Sn2+SiO2Microballoon D.
(3) it disperses product D in deionized water, the additional amount of product D and the mass ratio of deionized water are 1:5, then
The AgNO of 6mmol/L is added dropwise3Solution, wherein AgNO3AgNO in solution3Be adsorbed with Sn2+SiO2Microballoon D's is water-soluble
The mass ratio of liquid is 0.005:1, and stirring after forty minutes, then hydrazine is added dropwise into solution, hydrazine additional amount and AgNO3Rub
You are stirred for 3 hours after adding reducing agent, are then centrifuged, obtain product E, is i.e. load has Ag than being 1:1.4
The Nano-meter SiO_2 of grain2Microballoon, silver carrying amount (mass content) is about 5%.
(4) Ag nano particles SiO will be loaded with2Microballoon, which is scattered in isopropanol/distilled water solution, forms the molten of solid content 18%
Liquid I, wherein alcohol and water mixed volume ratio are 12:1；By perfluoroalkyl silanes
With isopropanol/distilled water solution mixing, wherein mass ratio shared by perfluoroalkyl silanes is 2.0%, and it is molten that citric acid adjusting is then added
Liquid pH value is 5.0, is stirred 24 hours with 500 revs/min and obtains solution II, and wherein alcohol and water mixed volume ratio are 14:1；It will be molten
Liquid I is mixed with solution II according to mass ratio 1:2, is stirred 4 hours with 500 revs/min and is obtained antifouling antibacterial composite coating.
Position is often touched to automotive upholstery using the antifouling antibacterial composite coating and carries out plated film, water mean exposure can be obtained
Angle is about the film layer of 113 °, staphylococcus aureus bacteriostasis rate 95.6%, Escherichia coli bacteriostasis rate 100%, is remarkably improved automobile
The property easy to clean of inside gadget and the total plate count for reducing inside gadget surface.
Embodiment six: the present embodiment provides a kind of antifouling antibacterial composite coating preparation methods, comprising the following steps:
(1) it disperses ethyl orthosilicate in ethanol distillation water mixed liquid and obtains solution A, wherein ethyl orthosilicate quality hundred
Dividing content is 1.91%, and distilled water mass percentage is 1.03%, and surplus is ethyl alcohol；Concentrated ammonia liquor is added in ethyl alcohol, NH is obtained3
The alcohol ammonia solution B that mass percentage is 4.39%；Alcohol ammonia solution B is added in solution A with the speed of 30 μ l/min, while with
500 revs/min of stirrings are persistently stirred 90 minutes after alcohol ammonia solution B is all added in solution A, then open to stand 48 hours
Solution C is obtained, solution C is centrifugated, then that obtained solid product is 3 hours dry at 100 DEG C, obtaining partial size is about
The SiO of 24nm2Microballoon.
(2) by SnCl2·2H2O is added in aqueous hydrochloric acid solution, forms SnCl2The solution that mass percentage is 0.12%, it is molten
Liquid pH value was 2.5, with mixing speed magnetic agitation 15 minutes of 1100 revs/min；Then nanometer obtained in step on being added
SiO2Microballoon, SiO2Microballoon additional amount accounts for the 0.20% of solution gross mass, is persistently dispersed with stirring 30 minutes, 30 are stood after stirring
Minute, it is centrifugally separating to obtain and is adsorbed with Sn2+SiO2Microballoon D.
(3) it disperses product D in deionized water, the additional amount of product D and the mass ratio of deionized water are 1:5, then
The AgNO of 6mmol/L is added dropwise3Solution, wherein AgNO3AgNO in solution3Be adsorbed with Sn2+SiO2Microballoon D's is water-soluble
The mass ratio of liquid is 0.032:1, after stirring 30 minutes, then hydrazine is added dropwise into solution, hydrazine additional amount and AgNO3Rub
You are stirred for 3 hours after adding reducing agent, are then centrifuged, obtain product E, is i.e. load has Ag particle than being 1:1.2
Nano-meter SiO_22Microballoon, silver carrying amount (mass percentage) is about 8%.
(4) Ag nano particles SiO will be loaded with2Microballoon, which is scattered in isopropanol/distilled water solution, forms the molten of solid content 10%
Liquid I, wherein alcohol and water mixed volume ratio are 10:1；By perfluoroalkyl silanes
With isopropanol/distilled water solution mixing, wherein mass ratio shared by perfluoroalkyl silanes is 3%, and citric acid regulating solution is then added
PH value is 5.0, is stirred 24 hours with 500 revs/min and obtains solution II, and wherein alcohol and water mixed volume ratio are 12:1；By solution I
It is mixed with solution II according to mass ratio 1:2, is stirred 4 hours with 500 revs/min and obtain antifouling antibacterial composite coating.
Position is often touched to automotive upholstery using the antifouling antibacterial composite coating and carries out plated film, water mean exposure can be obtained
Angle is about the film layer of 116 °, staphylococcus aureus bacteriostasis rate 98%, Escherichia coli bacteriostasis rate 100%, is remarkably improved in automobile
The property easy to clean of gadget and the total plate count for reducing inside gadget surface.
Above in conjunction with attached drawing, an exemplary description of the invention, it is clear that realization of the invention is not by aforesaid way
Limitation, as long as use the inventive concept and technical scheme of the present invention carry out various improvement, or it is not improved will be of the invention
Conception and technical scheme directly apply to other occasions, be within the scope of the invention.
Claims (10)
1. a kind of preparation method of antifouling antibacterial composite coating, which comprises the following steps:
(1) Nano-meter SiO_2 is prepared2Microballoon: formation solution (A) in alcohol/aqueous solution is dispersed by ethyl orthosilicate；Alcohol is added in ammonium hydroxide
In, it is formed alcohol ammonia solution (B)；Alcohol ammonia solution (B) is added in solution (A) and is stirred；It is then allowed to stand, obtains being dispersed with nanosphere
The solution (C) of shape SiO2 particle separates the solution (C) for being dispersed with nanometer spherical SiO2 particle, obtains nanometer spherical
SiO2 particle；
(2) preparation carries Ag Nano-meter SiO_22Microballoon: by Nano-meter SiO_2 obtained above2Microballoon is scattered in containing SnCl2·2H2The acid water of O
Sensitized treatment is carried out in solution, is stood, and separation obtains being adsorbed with Sn2+SiO2Microballoon (D), will be adsorbed with Sn2+SiO2Microballoon
(D) it is dispersed in water and AgNO is added3Solution and reducing agent are stood, separation, obtain carrying Ag Nano-meter SiO_22Microballoon；
By SnCl2·2H2O is added in acidic aqueous solution and forms SnCl2The solution that mass percentage is 0.08%~0.12%, with
Nano-meter SiO_2 is added after the solution in magnetic agitation 15~30 minutes in 800~1200 revs/min of revolving speed thereto2Microballoon, then magnetic
Power is dispersed with stirring 30~60 minutes formation mixed solutions, SiO in mixed solution2Microspheres quality percentage composition be 0.15%~
0.25%；Gained mixed solution is stood, is then centrifuged for isolated being adsorbed with Sn2+SiO2Microballoon (D)；
Sn will be adsorbed with2+SiO2Microballoon (D) is scattered in deionized water or distilled water, is adsorbed with Sn2+SiO2Microballoon (D)
The mass ratio of additional amount and deionized water or distilled water is 1:5, and AgNO is then added dropwise3Solution, wherein AgNO3In solution
AgNO3Be adsorbed with Sn2+SiO2The mass ratio of the aqueous solution of microballoon (D) is 0.005:1~0.032:1, stirs 30~90 points
Zhong Hou, then reducing agent is added dropwise, it is stirred for 1~3 hour after adding reducing agent, then, being centrifugally separating to obtain load has Ag
The Nano-meter SiO_2 of grain2Microballoon, wherein the content of Ag particle accounts for the Nano-meter SiO_2 that load has Ag particle2The 5%~8% of microballoon gross mass；Institute
Stating reducing agent is hydrazine, the additional amount and AgNO of reducing agent3Molar ratio be 1:1.4~1:2.0；
(3) by load Ag Nano-meter SiO_2 obtained above2Microballoon is scattered in alcohol solution, is then added into the solution and is contained perfluor
The hydrolyzed silane solution of alkyl obtains antifouling antibacterial composite coating.
2. the preparation method of antifouling antibacterial composite coating according to claim 1, which is characterized in that molten in step (1)
Liquid (A), mass ratio shared by water are 0.4%~2.6%, and mass ratio shared by ethyl orthosilicate is 1.8%~2.0%, and surplus is alcohol.
3. the preparation method of antifouling antibacterial composite coating according to claim 1 or 2, which is characterized in that in step (1),
NH in alcohol ammonia solution (B)3Mass percentage is 3.1%~7.2%, and surplus is alcohol.
4. the preparation method of antifouling antibacterial composite coating according to claim 1, which is characterized in that in step (1), in room
Under temperature, alcohol ammonia solution (B) is added in solution (A) and is given simultaneously and is stirred, mixing speed is 500~1000 turns/min；Alcohol ammonia
Solution (B) is added completely into after solution (A) persistently stirs 30~120min again.
5. the preparation method of antifouling antibacterial composite coating according to claim 1 or 4, which is characterized in that in step (1),
Alcohol ammonia solution (B) is added in solution (A) after persistently stirring, opening stands 24~72h and obtains solution (C), and solution (C) is centrifuged
It separates and 1~3 hour dry at 100~180 DEG C to obtained solid product, obtains the Nano-meter SiO_2 that partial size is 10~75nm2It is micro-
Ball.
6. the preparation method of antifouling antibacterial composite coating according to claim 1, which is characterized in that described in step (2)
Acidic aqueous solution is hydrochloric acid deionized water solution, pH value 2.5.
7. the preparation method of antifouling antibacterial composite coating according to claim 1, which is characterized in that, will be upper in step (3)
It states and carries the solution (I) that Ag nanosized SiO_2 microballoon is scattered in formation solid content 10%~20% in alcohol solution；By perfluoroalkyl silanes
It is added in alcohol solution, and appropriate acid-catalyzed hydrolysis is added, obtain solution (II)；By solution (I) with solution (II) according to certain
Ratio mixing, obtain antifouling antibacterial composite coating；In this step, alcohol and water mixed volume ratio are 8:1~14 in alcohol solution:
1。
8. the preparation method of antifouling antibacterial composite coating according to claim 1 or claim 7, which is characterized in that in step (3),
Perfluoroalkyl silanes and alcohol/aqueous solution are mixed, wherein mass ratio shared by perfluoroalkyl silanes is 1.5%~3%, and acid is then added
Adjusting the solution ph is 4.5~6, is stirred 4~24 hours with 200~500 revs/min and obtains solution II；The perfluoroalkyl
Silane structure formula are as follows:
It is 1~3, a is 0~2 that wherein m, which is 2~30, n,；It is hydrolyzable groups halogeno-group or alkane for perfluor carbochain or perfluoroether chain
Oxygroup；For or alkoxy；The acid is the mixture of one of acetic acid, citric acid or both.
9. the preparation method of antifouling antibacterial composite coating according to claim 7, which is characterized in that solution (I) and solution
(II) it mixes according to mass ratio 1:1~1:2, is stirred 0.5~4 hour with 200~500 revs/min.
10. the according to claim 1, preparation method of antifouling antibacterial composite coating described in 2,4,6,7 or 9, which is characterized in that institute
The alcohol stated is one of ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol or wherein several mixtures.
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