CN107011707A - A kind of preparation method of the novel nano-material of antifogging self-cleaning - Google Patents
A kind of preparation method of the novel nano-material of antifogging self-cleaning Download PDFInfo
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- CN107011707A CN107011707A CN201710264736.3A CN201710264736A CN107011707A CN 107011707 A CN107011707 A CN 107011707A CN 201710264736 A CN201710264736 A CN 201710264736A CN 107011707 A CN107011707 A CN 107011707A
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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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
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Abstract
The invention discloses a kind of preparation method of the novel nano-material of antifogging self-cleaning, TiO 2 sol is made annealing treatment, titania powder is obtained after furnace cooling, ball milling 30 hours distributes it in deionized water, obtains titania solution；Tetraethyl orthosilicate is hydrolyzed under ammonia-catalyzed, suspension is prepared, under stirring at room temperature and hydrochloric acid solution is added dropwise, ageing, which becomes to be put into after gel, to be dried, drying sample is made annealing treatment again, SiO 2 powder is obtained after furnace cooling, ball milling 20 hours adds titania solution in solvent, it is sufficiently stirred for, silica is added, mixing is stirred at a temperature of 72 DEG C, solution system is obtained；Base catalyst is added, it is 11 to make solution system pH value, adds fluoro alkyl-silane, titanate esters coupling, ethylene glycol, polyethylene glycol, neutralization reagent is added after stirring, it is 6.5 to make solution ph, filters reaction product.
Description
Technical field
The present invention relates to a kind of nano material, and in particular to a kind of preparation method of the novel nano-material of antifogging self-cleaning.
Background technology
At present, nano material turns into focus of concern as important Disciplinary Frontiers.In our daily lifes,
Vehicle glass, building glass, ambetti etc., are required for us frequently to go to safeguard and clean, can be caused when safeguarding and cleaning
It is the larger wasting of resources, such as water, electricity, artificial, it also there is larger potential safety hazard in high-rise building cleaning.It is same with this
When, in sleety weather, vehicle glass is easy to produce fog, influences pilot's line of vision, this is a multiple weight of car accident
Want factor.Therefore, antifog, self-cleaning nano material preparation is most important for the sustainable development of China's economy.With
It is antifog, self-cleaning nano materials demand become increasingly conspicuous, there are some antifog, self-cleaning products in the market.However, most of anti-
Mist, self-cleaning product not only have complex manufacturing technology, the problems such as stability is poor, and the cementability between base material is poor, hold
It is easy to fall off.Accordingly, it is difficult to keep permanent antifog, self-cleaning effect.The problem of being existed based on above-mentioned antifog, self-cleaning product, we
Have developed one kind has anti misting capability strong, and self-cleaning effect persistently, is constructed simply, antifog, the self-cleaning nano material of low cost and other advantages
Material.
The content of the invention
The technical problems to be solved by the invention are the cementability difference and stability of existing antifogging self-cleaning nano material
Also it is poor, it is unfavorable for being used for a long time, it is therefore intended that provide a kind of preparation method of the novel nano-material of antifogging self-cleaning, solves existing
What is had has the problem of nano material cementability and stability are poor.
The present invention is achieved through the following technical solutions：
A kind of preparation method of the novel nano-material of antifogging self-cleaning, comprises the following steps：
(1) butyl titanate is added drop-wise in absolute ethyl alcohol under agitation, is sufficiently stirred for and then sequentially adds acetic acid, nitre to it
Acid and deionized water, continue to stir, finally give stable TiO 2 sol；
(2) obtained TiO 2 sol is made annealing treatment, annealing temperature is 480-520 DEG C, and soaking time 5-7 is small
When, then furnace cooling obtains titania powder, ball milling 30 hours, and the titanium dioxide granule size in powder sample is
4nm, weighs titania powder sample, distributes it in deionized water, obtain titania solution；
(3) tetraethyl orthosilicate is hydrolyzed under ammonia-catalyzed, prepares and spherical received for 25nm silica containing particle diameter
The suspension of rice corpuscles, under stirring at room temperature and is added dropwise hydrochloric acid solution, is aged 30 hours, becomes to be put into drying box after gel
Row drying, then drying sample is made annealing treatment, annealing temperature is 480-520 DEG C, soaking time 5-7 hours, then with stove
Cooling, obtains SiO 2 powder, ball milling 20 hours, and the silica particle sizes in powder sample are in below 10nm；
(4) titania solution will be obtained to add in solvent, be sufficiently stirred for, add silica, in 65-75 DEG C of temperature
Lower stirring mixing, obtains solution system；
(5) at a temperature of 65-75 DEG C, base catalyst is added in solution system, it is 11 to make solution system pH value；
(6) fluoro alkyl-silane, titanate esters coupling, ethylene glycol, polyethylene glycol are added in step (5), in 50-55 DEG C of temperature
Degree is lower to continue stirring reaction 5h；
(7) neutralization reagent is added in step (6), it is 6.5 to make solution ph, filters reaction product.
A kind of annealing temperature in the preparation method of the novel nano-material of antifogging self-cleaning, the step (2) and step (3)
For 500 DEG C, soaking time 6 hours.Temperature is 70 DEG C in the step (4) and step (5).The neutralization reagent be ammonium chloride and
Acetic acid.The solvent includes the one or more in isopropanol or n-butanol or ethylene glycol ethyl ether.
Further, nano material is with substrate surface with chemical bonds in the present invention, and it has stronger adhesive force, and
And all there is preferable adhesive force on glass, ceramics, metal, plastics, rubber, electronic component surface, according to GB/T 9286-
1998 are tested, and adhesive force reaches 0 grade.
The present invention compared with prior art, has the following advantages and advantages：
1st, a kind of preparation method of the novel nano-material of antifogging self-cleaning of the invention, the present invention contains silicon fluoride, titanium dioxide
Silicon and nano material, performance are stable, and storage stability is good, possesses the excellent resistance to height that inorganic material and organosilicon material have
Low temperature, ageing-resistant performance, while also as the introducing of fluoro-containing group and impart coating solvent resistant, chemically stable, lower table
The excellent properties such as face energy；
2nd, the preparation method of the novel nano-material of a kind of antifogging self-cleaning of the invention, nano titanium oxide of the present invention and nanometer
Silica is combined, and the composite nano materials not only maintain photocatalysis and the super hydrophilicity of original titanium dioxide, Er Qieti
High cementability between composite nano materials and base material, it is ensured that antifog on base material, self-cleaning nano material fastness and resistance to
Mill property；
3rd, a kind of preparation method of the novel nano-material of antifogging self-cleaning of the invention, preparation technology of the present invention is simple, is easy to
Operation.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, with reference to embodiment, to present invention work
Further to describe in detail, exemplary embodiment and its explanation of the invention is only used for explaining the present invention, is not intended as to this
The restriction of invention.
Embodiment 1
A kind of preparation method of the novel nano-material of antifogging self-cleaning of the present invention, nothing is added drop-wise to by butyl titanate under agitation
In water-ethanol, it is sufficiently stirred for and then sequentially adds acetic acid, nitric acid and deionized water to it, continues to stir, finally give stabilization
TiO 2 sol.
Obtained TiO 2 sol is made annealing treatment, annealing temperature is 500 DEG C, soaking time 6 hours, Ran Housui
Stove is cooled down, and obtains titania powder, ball milling 30 hours, and the titanium dioxide granule size in powder sample is 4nm, weighs dioxy
Change titanium powder sample, distribute it in deionized water, obtain titania solution；
Tetraethyl orthosilicate is hydrolyzed under ammonia-catalyzed, prepared containing the spherical nanoparticle of silica that particle diameter is 25nm
The suspension of son, under stirring at room temperature and is added dropwise hydrochloric acid solution, is aged 30 hours, becomes to be put into drying box after gel and done
It is dry, then drying sample is made annealing treatment, annealing temperature is 500 DEG C, and soaking time 6 hours, then furnace cooling obtains two
Silicon oxide powder, ball milling 20 hours, the silica particle sizes in powder sample are in below 10nm.
Titania solution will be obtained to add in solvent, be sufficiently stirred for, add silica, stirred at a temperature of 72 DEG C
Mixing, obtains solution system；Keep the temperature and add base catalyst, it is 11 to make solution system pH value, adds fluothane
Base silane, titanate esters coupling, ethylene glycol, polyethylene glycol, continue stirring reaction 5h at a temperature of 52 DEG C, obtain clear solution；Plus
Enter neutralization reagent, it is 6.5 to make solution ph, filtering reaction product obtains the nano material of the present invention.
The adhesive force of obtained nano material is 0 grade in the present embodiment, and better than existing antifogging self-cleaning function
The adhesive force 6% of nano material, also, the high-low temperature resistant and ageing-resistant performance of nano material in the present embodiment are also preferable.
Wherein, the present invention is made up of the component of following parts by weight：31 parts of butyl titanate, 132 parts of absolute ethyl alcohol, acetic acid 12
Part, 7 parts of nitric acid, 51 parts of deionized water, 39 parts of tetraethyl orthosilicate, 62 parts of hydrochloric acid solution, 108 parts of solvent, titanate esters are coupled 5 parts,
11 parts of ethylene glycol, 12 parts of polyethylene glycol, 8 parts of ammoniacal liquor, 8 parts of base catalyst, 7 parts of neutralization reagent, 12 parts of fluoro alkyl-silane.It is described
Base catalyst is the one or more in sodium hydroxide or caustic alcohol.The neutralization reagent is ammonium chloride and acetic acid.It is described molten
Agent includes the one or more in isopropanol or n-butanol or ethylene glycol ethyl ether.
Above-described embodiment, has been carried out further to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail, should be understood that the embodiment that the foregoing is only the present invention, be not intended to limit the present invention
Protection domain, within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc. all should be included
Within protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the novel nano-material of antifogging self-cleaning, it is characterised in that comprise the following steps：
(1) butyl titanate is added drop-wise in absolute ethyl alcohol under agitation, be sufficiently stirred for then to its sequentially add acetic acid, nitric acid and
Deionized water, continues to stir, finally gives stable TiO 2 sol；
(2) obtained TiO 2 sol is made annealing treatment, annealing temperature is 480-520 DEG C, soaking time 5-7 hours,
Then furnace cooling, obtains titania powder, ball milling 30 hours, the titanium dioxide granule size in powder sample is 4nm, is claimed
Titania powder sample is taken, is distributed it in deionized water, titania solution is obtained；
(3) tetraethyl orthosilicate is hydrolyzed under ammonia-catalyzed, prepared containing the spherical nanoparticle of silica that particle diameter is 25nm
The suspension of son, under stirring at room temperature and is added dropwise hydrochloric acid solution, is aged 30 hours, becomes to be put into drying box after gel and done
It is dry, then drying sample is made annealing treatment, annealing temperature is 480-520 DEG C, soaking time 5-7 hours, then furnace cooling,
Obtain SiO 2 powder, ball milling 20 hours, the silica particle sizes in powder sample are in below 10nm；
(4) titania solution will be obtained to add in solvent, be sufficiently stirred for, add silica, stirred at a temperature of 65-75 DEG C
Mixing is mixed, solution system is obtained；
(5) at a temperature of 65-75 DEG C, base catalyst is added in solution system, it is 11 to make solution system pH value；
(6) fluoro alkyl-silane, titanate esters coupling, ethylene glycol, polyethylene glycol are added in step (5), at a temperature of 50-55 DEG C
Continue stirring reaction 5h；
(7) neutralization reagent is added in step (6), it is 6.5 to make solution ph, filters reaction product.
2. the preparation method of the novel nano-material of a kind of antifogging self-cleaning according to claim 1, it is characterised in that described
Annealing temperature in step (2) and step (3) is 500 DEG C, soaking time 6 hours.
3. the preparation method of the novel nano-material of a kind of antifogging self-cleaning according to claim 1, it is characterised in that described
Temperature is 70 DEG C in step (4) and step (5).
4. the preparation method of the novel nano-material of a kind of antifogging self-cleaning according to claim 1, it is characterised in that described
Neutralization reagent is ammonium chloride and acetic acid.
5. a kind of nano material with antifogging self-cleaning effect according to claim 1, it is characterised in that the solvent bag
Include the one or more in isopropanol or n-butanol or ethylene glycol ethyl ether.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710264736.3A CN107011707A (en) | 2017-04-21 | 2017-04-21 | A kind of preparation method of the novel nano-material of antifogging self-cleaning |
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| CN201710264736.3A CN107011707A (en) | 2017-04-21 | 2017-04-21 | A kind of preparation method of the novel nano-material of antifogging self-cleaning |
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| CN107011707A true CN107011707A (en) | 2017-08-04 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107570134A (en) * | 2017-10-27 | 2018-01-12 | 成都瞬科仪器仪表有限公司 | A kind of preparation method of the novel nano-material of antifogging self-cleaning |
| CN107603316A (en) * | 2017-09-08 | 2018-01-19 | 常州达奥新材料科技有限公司 | A kind of preparation method of antifogging self-cleaning nano material |
| CN109796869A (en) * | 2018-12-08 | 2019-05-24 | 英鸿纳米科技股份有限公司 | A kind of antifog, self-cleaning nano material preparation method |
| CN110591555A (en) * | 2019-09-09 | 2019-12-20 | 福建中美友拓科技发展有限公司 | Preparation method of self-cleaning antifogging astronomical telescope lens |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817858A (en) * | 2015-05-14 | 2015-08-05 | 北京中科佰卓纳米材料科技有限公司 | Preparation method of antifog and self-cleaning nanomaterial |
-
2017
- 2017-04-21 CN CN201710264736.3A patent/CN107011707A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817858A (en) * | 2015-05-14 | 2015-08-05 | 北京中科佰卓纳米材料科技有限公司 | Preparation method of antifog and self-cleaning nanomaterial |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107603316A (en) * | 2017-09-08 | 2018-01-19 | 常州达奥新材料科技有限公司 | A kind of preparation method of antifogging self-cleaning nano material |
| CN107570134A (en) * | 2017-10-27 | 2018-01-12 | 成都瞬科仪器仪表有限公司 | A kind of preparation method of the novel nano-material of antifogging self-cleaning |
| CN109796869A (en) * | 2018-12-08 | 2019-05-24 | 英鸿纳米科技股份有限公司 | A kind of antifog, self-cleaning nano material preparation method |
| CN110591555A (en) * | 2019-09-09 | 2019-12-20 | 福建中美友拓科技发展有限公司 | Preparation method of self-cleaning antifogging astronomical telescope lens |
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Application publication date: 20170804 |
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