CN107974114A - A kind of preparation method of nano paint - Google Patents
A kind of preparation method of nano paint Download PDFInfo
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- CN107974114A CN107974114A CN201711284005.1A CN201711284005A CN107974114A CN 107974114 A CN107974114 A CN 107974114A CN 201711284005 A CN201711284005 A CN 201711284005A CN 107974114 A CN107974114 A CN 107974114A
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- nano
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- 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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- 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
- C09D5/08—Anti-corrosive paints
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
A kind of preparation method of nano paint, prepares nano-TiO first2Powder active material, by the way that the active material is carried out, surface is modified, and with octadecyl acrylate, polystyrene emulsion and acid anhydrides carry out being mixed to get nano paint.The preparation method of the present invention has that technique is simple and convenient, stability is good, has very strong toughness, high mechanical strength.
Description
Technical field
The present invention relates to a kind of preparation method of nano paint.
Background technology
Nano material has skin effect, small-size effect, optical effect, quantum size effect, macroscopic quantum size effect
Special nature should be waited, coating can be made to obtain new function.
Due to the small-size effect of nanoparticle, skin effect, quantum size effect and macroscopic quantum tunnel in nano paint
Channel effect etc. causes the characteristic that they do not possess in magnetic, light, electricity, sensitivity etc. presentation conventional material.Therefore nanoparticle exists
Magnetic material, electronic material, optical material, the sintering of high compactedness material, catalysis, sensing, ceramic toughening etc. have wide
Application prospect.In general, nano paint must is fulfilled for two conditions：First, at least grain size of a phase in coating
In the particle size range of 1-100nm；Secondly, the presence of nanometer phase makes the performance of coating be significantly improved or has new work(
Energy.But current nano paint also has the disadvantage that, such as poor performance, the characteristics of stability is not strong.
The content of the invention
The purpose of patent of the present invention is to provide a kind of preparation method of nano paint, of the invention to use following technical side
Case：
A kind of preparation method of nano paint, it is characterised in that this method comprises the following steps：
Step 1: nano-TiO2Powder active material
By nano-TiO2Powder and polyethylene glycol oxide powder are 2-5 in mass ratio:10-20 is placed in ground and mixed in ball mill
1-12h, mixture is placed in heating furnace under the conditions of being warming up to 100-500 DEG C after heating 0.5-10h and naturally cools to room temperature and obtain
To nano-TiO2Powder active material；
Step 2: nano-TiO2The surface of powder active material is modified
By nano-TiO2Powder active material, potassium peroxydisulfate, n,N-Dimethylformamide, P2O5With deionized water with quality
Than for 2-4:3‐6:1‐5:0.5‐1:15-50 is mixed, and is controlled the pH value of the mixture between 3 and 6 using the concentrated sulfuric acid, heating
1-2h is stirred to 40-70 DEG C, is cooled to after room temperature and uses deionized water to be dried to obtain solid powder after cleaning 3-6 times sediment
End, distilled water and H are added by solid powder2O2Maintain the temperature at 40-60 DEG C of reaction 0.5-3h；Product is carried out after reaction
Centrifuge 15-30min to clean obtained product 3-6 times using deionized water, receiving for surface modification had both been obtained by dry
Rice TiO2Powder active material；The solid powder, distilled water and H2O2Mass ratio 3-6:20‐30:1‐6；
Step 3: the preparation of coating
The nano-TiO that octadecyl acrylate, surface prepared by polystyrene emulsion, step 2 are modified2Powder is lived
Property material and acid anhydrides are using mass ratio as 4-7:3-10:2-6:1-10, which is uniformly mixed, both obtains nano paint.
2nd, a kind of preparation method of nano paint as claimed in claim 1, it is characterised in that TiO described in step 12
Powder is 3 in mass ratio with polyethylene glycol oxide powder:15.
3rd, a kind of preparation method of nano paint as claimed in claim 1, it is characterised in that nanometer described in step 2
TiO2Powder active material, potassium peroxydisulfate, n,N-Dimethylformamide, P2O5With deionized water using mass ratio as 3:4.5:2:
0.6:35 mixing.
4th, a kind of preparation method of nano paint as claimed in claim 1, it is characterised in that nanometer described in step 1
TiO2The particle diameter of particle is 1-50nm.
5th, a kind of preparation method of nano paint as claimed in claim 1, it is characterised in that by acrylic acid in step 3
Stearyl, the nano-TiO that surface prepared by polystyrene emulsion, step 2 is modified2Powder active material and acid anhydrides are with matter
Amount is than being 5:7:4:2 be uniformly mixed both obtain nano paint.
Beneficial effect：
1st, preparation method of the invention is with technique is simple and convenient, pollution-free, environmental-friendly, film quality is high, input production
Go out the advantages that more extensive than high, of low cost and application prospect；
2nd, the coating intensity is big, and corrosion resistance is good.
Embodiment
With reference to specific embodiment, the present invention is further explained.
Step 1: nano-TiO2Powder active material
By nano-TiO2Powder and polyethylene glycol oxide powder are 2-5 in mass ratio:10-20 is placed in ground and mixed in ball mill
1-12h, mixture is placed in heating furnace under the conditions of being warming up to 100-500 DEG C after heating 0.5-10h and naturally cools to room temperature and obtain
To TiO_2 nanoparticles active material；The active material is the TiO of surface coating nano carbon2Powder active material.
Step 2: nano-TiO2The surface of powder active material is modified
By nano-TiO2Powder active material, potassium peroxydisulfate, n,N-Dimethylformamide, P2O5With deionized water with quality
Than for 2-4:3‐6:1‐5:0.5‐1:15-50 is mixed, and is controlled the pH value of the mixture between 3 and 6 using the concentrated sulfuric acid, heating
1-2h is stirred to 40-70 DEG C, is cooled to after room temperature and uses deionized water to be dried to obtain solid powder after cleaning 3-6 times sediment
End, distilled water and H are added by solid powder2O2Maintain the temperature at 40-60 DEG C of reaction 0.5-3h；Product is carried out after reaction
Centrifuge 15-30min to clean obtained product 3-6 times using deionized water, receiving for surface modification had both been obtained by dry
Rice TiO2Powder active material；The solid powder, distilled water and H2O2Mass ratio 3-6:20‐30:1‐6；
Step 3: the preparation of coating
The nano-TiO that octadecyl acrylate, surface prepared by polystyrene emulsion, step 2 are modified2Powder is lived
Property material and acid anhydrides are using mass ratio as 4-7:3-10:2-6:1-10, which is uniformly mixed, both obtains nano paint.
2nd, a kind of preparation method of nano paint as claimed in claim 1, it is characterised in that TiO described in step 12
Powder is 3 in mass ratio with polyethylene glycol oxide powder:15.
3rd, a kind of preparation method of nano paint as claimed in claim 1, it is characterised in that nanometer described in step 2
TiO2Powder active material, potassium peroxydisulfate, n,N-Dimethylformamide, P2O5With deionized water using mass ratio as 3:4.5:2:
0.6:35 mixing.
4th, a kind of preparation method of nano paint as claimed in claim 1, it is characterised in that nanometer described in step 1
TiO2The particle diameter of particle is 1-50nm.
5th, a kind of preparation method of nano paint as claimed in claim 1, it is characterised in that by acrylic acid in step 3
Stearyl, the nano-TiO that surface prepared by polystyrene emulsion, step 2 is modified2Powder active material and acid anhydrides are with matter
Amount is than being 5:7:4:2 be uniformly mixed both obtain nano paint.
(1) heretofore described polystyrene emulsion is prepared with the following method：
A, the preparation of styrene emulsion
Styrene and ammonium persulfate are placed in the container equipped with 40-55 DEG C of water, 20-60min is stirred, is passed through nitrogen, stirs
Azo-bis-isobutyrate hydrochloride and ammonium hydrogen carbonate are added while mixing, 40-55 DEG C of stirring 30-60min is kept, is warming up to 60~90
DEG C, reaction 3-15h is obtained, styrene emulsion；
The mass ratio of the styrene, ammonium persulfate, azo-bis-isobutyrate hydrochloride and ammonium hydrogen carbonate is 10-20:2-6:
1-3:3-7；
B, the preparation of cyclodextrine derivatives
(1) pretreatment of beta-cyclodextrin：
Distilled water is added in a reservoir, is heated to 90-100 DEG C, takes beta-cyclodextrin to be placed in heated steaming under agitation
Dissolved in distilled water, keep temperature control to be filtered at 90-95 DEG C, 10-20h at a temperature of filtrate is placed in -5-5 DEG C so that
Crystal separates out, and the crystal of precipitation, which is placed on, to dry when 6 is small in 80 DEG C of vacuum drying chambers must crystallize beta-cyclodextrin；The distillation
The mass ratio of water and beta-cyclodextrin is 100-200:20-30；
(2) preparation of cyclodextrine derivatives
Beta-cyclodextrin of the step (1) by pretreatment is placed in anhydrous pyridine, 15- is stirred in -5-0 DEG C of ice-water bath
Mixed liquor is made in 60min, NaOH and deionized water is added in mixed liquor the liquid that pH value is 9-11 is made, be warming up to 25-30
Butyrolactone DEG C is added in the liquid, reacts 15-30min, is cooled to -5-0 DEG C again, 1,2- epoxy butanes is added and keeps temperature
3-6h is reacted, adds second eyeball solution sustained response 10-15h, after completion of the reaction, pH value is adjusted to neutrality using hydrochloric acid, is used
Vacuum rotary steam removes water and pyridine, and solid particle is placed in dimethylformamide and is stirred evenly, is consolidated using acetone precipitation
Body product, is dried in vacuo 3-6h at 70-90 DEG C by the product and obtains solid particle, is cyclodextrine derivatives；
The beta-cyclodextrin of the pretreatment, anhydrous pyridine, butyrolactone, 1,2- epoxy butane, the mass ratio of second eyeball is 10-
20:30-60:2-5:3-6:1-3；
C, the preparation of polystyrene emulsion
Cyclodextrine derivatives and deionized water prepared by styrene emulsion, step B prepared by step A are mixed equal
It is even, n-butanol and n,N-dimethylacetamide are added, is passed through nitrogen temperature to 50 DEG C, when reaction 3-6 is small, stops heating and stirring
Mix down and be cooled to room temperature, obtain polystyrene emulsion；
The mass ratio of the styrene emulsion, cyclodextrine derivatives, deionized water, n-butanol and n,N-dimethylacetamide
For 5-10:1-3:30-60:2-4:3-5；
(2) research is found
1st, cyclodextrine derivatives prepared in the present invention are 2-O- (2- hydroxybutyls)-cyclodextrin, and yield can reach
12-16%, far more than the yield of 6-9% on the market, this is because the beta-cyclodextrin of pretreatment is placed in nothing first in the present invention
In water pyridine, mixed at a temperature of -5-0 DEG C of ice-water bath, by adding butyrolactone after heating, be cooled to -5-0 DEG C of ice again
1,2- epoxy butanes under water-bath, research are found, are added different materials by the change of this temperature, can effectively be lifted pre- place
The reactivity of the beta-cyclodextrin of reason, so as to lift the yield of cyclodextrine derivatives by about one time；
2nd, in addition research is found, is spread out using the beta-cyclodextrin of pretreatment compared to direct using beta-cyclodextrin production cyclodextrin
Biology, its yield can lift 1-2%；
3rd, find by research, lifted by adding cyclodextrine derivatives polystyrene emulsion shelf stability, with
Do not add cyclodextrin as a comparison embodiment 1, add beta-cyclodextrin embodiment 2 as a comparison, adding cyclodextrin with the present invention spreads out
Biology is compared, referring specifically to table 1.Table 1
4th, found by studying, the reaction time of polystyrene emulsion can effectively be lifted by adding cyclodextrine derivatives；With benzene
The mass ratio of vac emulsion, cyclodextrine derivatives, deionized water, n-butanol and n,N-dimethylacetamide is 6:1.5:50:3:
The conversion ratio that styrene is tested exemplified by 3.5 is shown in Table 2.
Table 2
| Comparative example 1 | Comparative example 2 | Add cyclodextrine derivatives | |
| React 3h | 30% | 76% | 92% |
| React 5h | 65% | Less than 95% | More than 98% |
| React 6h | 65% | Less than 95% | More than 98% |
5th, first to nano-TiO in the present invention2Powder surface activates to obtain the TiO of surface coating nano carbon2Powder active material
Material, then carries out surface modification to the nano-powder active material, is found by numerous studies, pass through modified nano-powder
Material can be even closer with the bond conjunction between heretofore described polystyrene emulsion, can effectively strengthen coating
Can, far more than the coating for using hydroxyl surface modified on the market or other surfaces are modified, referring specifically to table 3.
Table 3
It is to be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it should also be understood that,
After reading the content taught by the present invention, those skilled in the art can make various modifications or changes to the present invention, these
Equivalent form is also fallen within the scope of the appended claims of the present application.
Claims (5)
1. a kind of preparation method of nano paint, it is characterised in that this method comprises the following steps：
Step 1: nano-TiO2Powder active material
By nano-TiO2Powder and polyethylene glycol oxide powder are 2-5 in mass ratio:10-20 is placed in ground and mixed 1- in ball mill
12h, mixture is placed in heating furnace under the conditions of being warming up to 100-500 DEG C after heating 0.5-10h and naturally cools to room temperature and obtain
Nano-TiO2Powder active material；
Step 2: nano-TiO2The surface of powder active material is modified
By nano-TiO2Powder active material, potassium peroxydisulfate, n,N-Dimethylformamide, P2O5With deionized water using mass ratio as
2‐4:3‐6:1‐5:0.5‐1:15-50 is mixed, and is controlled between 3 and 6 the pH value of the mixture using the concentrated sulfuric acid, is warming up to 40-
1-2h is stirred at 70 DEG C, is cooled to after room temperature and uses deionized water to be dried to obtain solid powder after cleaning 3-6 times sediment, will
Solid powder adds distilled water and H2O2Maintain the temperature at 40-60 DEG C of reaction 0.5-3h；Product is subjected to centrifugation point after reaction
Obtained product is cleaned 3-6 times using deionized water from 15-30min, by the dry nano-TiO for both having obtained surface modification2
Powder active material；The solid powder, distilled water and H2O2Mass ratio 3-6:20‐30:1‐6；
Step 3: the preparation of coating
The nano-TiO that octadecyl acrylate, surface prepared by polystyrene emulsion, step 2 are modified2Powder active material
With acid anhydrides using mass ratio as 4-7:3-10:2-6:1-10, which is uniformly mixed, both obtains nano paint.
A kind of 2. preparation method of nano paint as claimed in claim 1, it is characterised in that TiO described in step 12Powder
Mass ratio with polyethylene glycol oxide powder is 3:15.
A kind of 3. preparation method of nano paint as claimed in claim 1, it is characterised in that nano-TiO described in step 22
Powder active material, potassium peroxydisulfate, n,N-Dimethylformamide, P2O5With deionized water using mass ratio as 3:4.5:2:0.6:35
Mixing.
A kind of 4. preparation method of nano paint as claimed in claim 1, it is characterised in that nano-TiO described in step 12
The particle diameter of particle is 1-50nm.
5. a kind of preparation method of nano paint as claimed in claim 1, it is characterised in that by acrylic acid 18 in step 3
Arrcostab, the nano-TiO that surface prepared by polystyrene emulsion, step 2 is modified2Powder active material and acid anhydrides are with mass ratio
For 5:7:4:2 be uniformly mixed both obtain nano paint.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4234641A1 (en) | 2022-02-25 | 2023-08-30 | Basf Se | Compositions, comprising modified titanium dioxide nanoparticles and uses thereof |
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|---|---|---|---|---|
| CN1162969A (en) * | 1994-11-10 | 1997-10-22 | 瓦克化学有限公司 | Redispersable polymer powder compositions containing cyclodextrin or cyclodextrin derivatives |
| CN101139410A (en) * | 2007-10-11 | 2008-03-12 | 江苏大学 | Polyphenylacetylene stabilization emulsion and preparation method thereof |
| CN104673028A (en) * | 2013-11-27 | 2015-06-03 | 胡建辉 | Waterproof nanometer aqueous coating |
| CN104725971A (en) * | 2015-03-25 | 2015-06-24 | 常州大学 | Multifunctional thermal insulation coating containing titanium dioxide/attapulgite nanocomposite material and preparation method thereof |
| CN104974572A (en) * | 2015-06-23 | 2015-10-14 | 苏州博利迈新材料科技有限公司 | Nano particle compound type anticorrosive coating and preparation method therefor |
| CN105694625A (en) * | 2016-02-05 | 2016-06-22 | 南京锎巴新材料科技有限公司 | Exterior wall waterproofing heat-insulating decorating integrated material and preparation method thereof |
-
2017
- 2017-12-07 CN CN201711284005.1A patent/CN107974114A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1162969A (en) * | 1994-11-10 | 1997-10-22 | 瓦克化学有限公司 | Redispersable polymer powder compositions containing cyclodextrin or cyclodextrin derivatives |
| CN101139410A (en) * | 2007-10-11 | 2008-03-12 | 江苏大学 | Polyphenylacetylene stabilization emulsion and preparation method thereof |
| CN104673028A (en) * | 2013-11-27 | 2015-06-03 | 胡建辉 | Waterproof nanometer aqueous coating |
| CN104725971A (en) * | 2015-03-25 | 2015-06-24 | 常州大学 | Multifunctional thermal insulation coating containing titanium dioxide/attapulgite nanocomposite material and preparation method thereof |
| CN104974572A (en) * | 2015-06-23 | 2015-10-14 | 苏州博利迈新材料科技有限公司 | Nano particle compound type anticorrosive coating and preparation method therefor |
| CN105694625A (en) * | 2016-02-05 | 2016-06-22 | 南京锎巴新材料科技有限公司 | Exterior wall waterproofing heat-insulating decorating integrated material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4234641A1 (en) | 2022-02-25 | 2023-08-30 | Basf Se | Compositions, comprising modified titanium dioxide nanoparticles and uses thereof |
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