CN109504277A - A kind of nano hybridization ceramic resin and preparation method thereof - Google Patents
A kind of nano hybridization ceramic resin and preparation method thereof Download PDFInfo
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- CN109504277A CN109504277A CN201811257934.8A CN201811257934A CN109504277A CN 109504277 A CN109504277 A CN 109504277A CN 201811257934 A CN201811257934 A CN 201811257934A CN 109504277 A CN109504277 A CN 109504277A
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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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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- 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
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The present invention provides a kind of preparation methods of nano hybridization ceramic resin, comprising the following steps: prepares nano oxidized suspension first, is prepared by mixing into nano alumina sol by nano aluminium oxide suspension and unitary strong acid;Nano alumina sol is subjected to synthetic reaction in the silicone intermediates with functional group, it is final to synthesize nano hybridization ceramic resin.Nano hybridization ceramics film prepared by the present invention, the performance indexess such as corrosion resistance, heat-resisting quantity, thermal stability, cold and hot hardness, scratch resistance, resistance to abrasion and anti-ultraviolet ageing, it is superior to individual organic coating or inorganic coating, performance is significantly improved and improved.
Description
Technical field
The invention belongs to new chemical materials technical fields, and in particular to a kind of nano hybridization ceramic resin and its preparation side
Method.
Background technique
Nano material technology is always the project that industry is concerned;Applications to nanostructures is also that scientific worker grinds
The hot spot studied carefully.Using silica, aluminium oxide as raw material, the nano silicon oxide of nanosizing process technique exploitation, nano aluminium oxide are utilized
The products such as powder, sol-gel, hybridized polymer are not any strange thing.The modeling prepared with nano-material modified technology
The products such as material, coating, also deep national economy every field.In aerospace, high-end manufacture, rail traffic, dark blue work
The every aspects such as industry or even new energy, frontier science and technology have the appearance of the figure of nanosecond science and technology and nano material.As household electric
The products for civilian use such as device, life kitchen tools also enjoy welfare brought by nanotechnology and nano material.
Nano aluminium oxide has extremely extensive purposes with its excellent physicochemical properties in production and living, by with
In production catalyst, fine ceramics, composite reinforcing material, new coating etc..It is solidifying about exploitation nano alumina sol-both at home and abroad
The report of glue research is considerably less, is studied according to correlation study, main cause is that the solubility of aluminium oxide in water is very limited
's.Currently, some patents about nano alumina sol are mostly the technologies of preparing being related in nano alumina sol both at home and abroad.
In the preparation method of alumina sol, a kind of method is that organic alkoxide raw material method is (such as former by the organic salt of raw material of aluminium isopropoxide
Material), prepare nano alumina sol.This kind of method preparation cost is high, expensive, so that the products application of sol-gel method
It is subject to certain restrictions;Another method is inorganic salt raw material method, metallic aluminium is dissolved in hydrochloric acid or aluminium chloride, obtains colourless
Transparent Aluminum sol, or aluminum nitrate and ammonium citrate is soluble in water according to a certain ratio, it is adjusted with concentrated nitric acid or concentrated ammonia liquor molten
Liquid pH value, can be obtained Aluminum sol.Both preparation method preparation process are big to environmental hazard, at high cost, and are finally made
Nano alumina sol solid content is low (general < 20wt%), such as Chinese patent CN201210120945.8 discloses a kind of lead to
The nanometer alumina slurry of sol-gel method preparation stable dispersion is crossed, the solid content of alumina sol is up to 13wt%;China
Patent CN201010274945.4 disclose one kind using boehmite as raw material, disperse and adjust solution ph to 2~5 be made receive
Rice alumina sol, but the maximum concentration of nano aluminium oxide is also less than 25wt%.
And it is miscellaneous to be synthetically prepared inorganic-organic nanocomposite using nano alumina sol or gel modified polyorganosiloxane intermediate
The example for changing ceramic resin has not been reported, also not disclosed patent document, to find out its cause, may with the research direction of colleague or
The application direction of target product is related.
Summary of the invention
A kind of nano hybridization ceramic resin is provided it is an object of the invention to overcome above-mentioned the deficiencies in the prior art place,
High performance film forming basis material is provided for manufacture sapecial coating and functional paint, nano hybridization ceramic resin of the invention is pair
Ecology green product that is friendly, free from environmental pollution, not endangering human health.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of nano hybridization ceramic resin, comprising the following steps:
(1) prepare nano oxidized suspension: by nano alumina powder jointed and deionized water by 25~30: 70~75 weight
Than being mixed by mechanical force, nano aluminium oxide initial mixing liquid is obtained, is added and receives in the nano aluminium oxide initial mixing liquid
Rice material dispersing agent, coupling agent, pH adjusting agent and cosolvent, are uniformly mixed, obtain nano aluminium oxide suspension;
(2) it prepares nano alumina sol: unitary strong acid being added in the nano aluminium oxide suspension made from step (1),
The molar ratio of the unitary strong acid and nano aluminium oxide suspension is 0.02: 1, is stirred evenly, and 1~3h is 25 to get solid content
The nano alumina sol of~30wt%;
(3) be synthetically prepared nano hybridization ceramic resin: it is anti-to be placed in synthesis for the nano alumina sol for taking step (2) to prepare
It answers in kettle, under 40 DEG C of stirrings of constant temperature, the silicone intermediates for having functional group is at the uniform velocity added dropwise, are dripped in 1~2h
It is complete, keep constant temperature until solution is completely limpid, reaction is completed, and pH value is finally adjusted, pH value is adjusted to 6~7 with pH adjusting agent,
Obtain nanometer alumina modified polysiloxanes.
Preferably, the partial size of the nano aluminium oxide of the step (1) is 10~20nm.
Preferably, the weight ratio of the nano material dispersing agent and nano aluminium oxide of the step (1) is 1: 0.5~1.
Preferably, the coupling agent of the step (1) is silane coupling agent, titanate coupling agent or aluminate coupling agent, is added
Dosage is the 1~3% of nano aluminium oxide mixed liquor quality.
Preferably, the coupling agent of the step (1) is titanate coupling agent.
Preferably, the pH adjusting agent of the step (1) is lactic acid, and additive amount is nano aluminium oxide mixed liquor mass parts
0.2~0.5 part, the pH value of reaction system is adjusted to 2~5.
Preferably, the cosolvent of the step (1) is ether alcohols solvent, and additive amount is nano aluminium oxide mixed liquor mass parts
1~3 part.
Preferably, the unitary strong acid of the step (2) is hydrochloric acid or nitric acid.
Preferably, the unitary strong acid of the step (2) is hydrochloric acid.
Preferably, the pH adjusting agent of the step (3) is organic amine multifunctional assistant.
Preferably, the functional group of the silicone intermediates with functional group of the step (3) is carboxyl, hydroxyl
Base, epoxy group, alkoxy or amide groups.
Preferably, silicone intermediates of the step (3) with functional group are among methyl phenyl silicone
Body;It selects methyl phenyl silicone intermediate as raw material, finally obtains the nano hybridization ceramic resin of not hydroxyl.
Preferably, silicone intermediates of the step (3) with functional group are hydroxy-terminated polysiloxane intermediate;
It selects hydroxy-terminated polysiloxane intermediate as raw material, finally obtains the nano hybridization ceramic resin of hydroxyl.
The beneficial effects of the present invention are:
By controlling the reactive group and nano alumina sol dosage of polymer, available receiving with different performance
Rice hydridization ceramic resin, both can air drying film forming, also heating curable form a film;Both it is good, high glaze clear that transparency can have been prepared
Paint;The colored paint with good covering power and weatherability can also be prepared;Both one-component coating can be prepared, bi-component painting can also be prepared
Material.
The nano hybridization ceramics film of preparation, corrosion resistance, heat-resisting quantity, thermal stability, cold and hot hardness, scratch resistance,
The performance indexess such as resistance to abrasion and anti-ultraviolet ageing, are superior to individual organic coating or inorganic coating, and performance obtains
It significantly improves and improves.
Specific embodiment
For more concise displaying technical solution of the present invention, objects and advantages, combined with specific embodiments below
The present invention is described in further detail.
Embodiment 1
(1) nano aluminium oxide dispersion suspension is prepared:
It is added in 4kg deionized water by high-speed stirred by 2.5kg is nano alumina powder jointed, it is mixed obtains nano aluminium oxide
Close liquid;CI-913 nanometers of hyper-dispersant 1.5kg, 311W titanate coupling agent 0.3kg, two are added in nano aluminium oxide mixed liquor
Propylene glycol monomethyl ether 1.5kg, with lactic acid 0.2kg, regulation system pH value to 2~5;After being uniformly mixed, with homogenizer or ultrasound
Wave ancillary equipment is dispersed to disperse suspension to get to nano aluminium oxide.
(2) nano alumina sol is prepared:
Using hydrochloric acid as peptizing agent, calculated by the molar ratio 0.02 of hydrochloric acid and nano aluminium oxide, it will be obtained nano oxidized
Aluminium dispersion suspension is added technical grade (36%) hydrochloric acid 6g and the nano oxygen of 25wt% content can be obtained in 20 DEG C of 1~3h of dispersion
Change Aluminum sol.
(3) it is synthetically prepared nano hybridization ceramic resin:
30 parts of nano alumina sol of 25% content of the above metering (wt%) are taken, are placed in synthesis reaction vessel, in perseverance
Under warm 40 DEG C of stirrings, corresponding 70 parts of Silres IC-368 methyl phenyl silicone intermediate are added dropwise, and in 2h
It drips off, keeps constant temperature until solution is completely limpid;Make pH adjusting agent with AMP-95 organic amine, dosage is the 0.1% of system, is adjusted
Whole system pH 6~7 (slightly sour to neutral) is to get the nano hybridization ceramic resin for arriving not hydroxyl.
Embodiment 2
Unique difference of the present embodiment and embodiment 1 are as follows: 40 parts of the nano alumina sol of 25% content.
Embodiment 3
Unique difference of the present embodiment and embodiment 1 are as follows: 50 parts of the nano alumina sol of 25% content.
Embodiment 4
Unique difference of the present embodiment and embodiment 1 are as follows: the corresponding poly- silicon oxygen of Silres IC-368 aminomethyl phenyl is added dropwise
60 parts of alkane intermediate.
Embodiment 5
Unique difference of the present embodiment and embodiment 1 are as follows: the corresponding poly- silicon oxygen of Silres IC-368 aminomethyl phenyl is added dropwise
50 parts of alkane intermediate.
By prepared by Examples 1 to 5 not the nano hybridization ceramic resin of hydroxyl carry out its appearance, viscosity, index of refraction,
The performance tests such as heat resistance, performance indicator meet in 1 range of table, can determine whether as qualified products.
The nano hybridization ceramic resin performance indicator range of the not hydroxyl of table 1
The not nano hybridization ceramic resin testing result such as table 2 of hydroxyl prepared by Examples 1 to 5.
Not nano hybridization ceramic resin the performance test results of hydroxyl prepared by 2 Examples 1 to 5 of table
As seen from the above table, the nano hybridization ceramic resin performance indicator of the not hydroxyl in Examples 1 to 5 is set in qualification
Within the scope of fat prod performance indicator, therefore, the product of the preparation of the embodiment of the present invention 1~5 be can determine whether as qualified products.Its
Middle embodiment 1,2,3 show in the increase nano hybridization ceramic resin with nano oxidized aluminium content nano oxidized aluminium content also with
Increase, embodiment 1,4,5 compares, and shows the reduction with methyl phenyl silicone intermediates content, and viscosity is also therewith
It reduces, illustrates that the content of methyl phenyl silicone intermediate influences the viscosity of nano hybridization ceramic resin.
Embodiment 6
The step of the present embodiment (1), (2) are same as Example 1;
Step (3) uses following methods:
35 parts of nano alumina sol of 30% content of the above metering (wt%) are taken, are placed in synthesis reaction vessel, in perseverance
Under warm 40 DEG C of stirrings, it is added dropwise corresponding watt gram70 parts of WS62M hydroxy-terminated polysiloxane intermediate, and
It is dripped off in 2h, keeps constant temperature until solution is completely limpid;Make pH adjusting agent with AMP-95 organic amine, dosage is system
0.1%, system pH 6~7 (slightly sour to neutral) is adjusted to get the nano hybridization ceramic resin of hydroxyl is arrived.
Embodiment 7
Unique difference of the present embodiment and embodiment 6 are as follows: 45 parts of the nano alumina sol of 35% content.
Embodiment 8
Unique difference of the present embodiment and embodiment 6 are as follows: 55 parts of the nano alumina sol of 35% content.
Embodiment 9
Unique difference of the present embodiment and embodiment 6 are as follows: be added dropwise correspondingWS62M hydroxy-terminated polysiloxane
60 parts of intermediate.
Embodiment 10
Unique difference of the present embodiment and embodiment 6 are as follows: be added dropwise correspondingWS62M hydroxy-terminated polysiloxane
50 parts of intermediate.
By the nano hybridization ceramic resin of hydroxyl prepared by embodiment 6~10 carry out its appearance, viscosity, index of refraction,
The performance tests such as heat resistance, performance indicator meet in 3 range of table, can determine whether as qualified products.
The nano hybridization ceramic resin performance indicator range of 3 hydroxyl of table
The nano hybridization ceramic resin testing result such as table 4 of hydroxyl prepared by embodiment 6~10.
Hydroxyl nano hybridization ceramic resin the performance test results prepared by 4 embodiment 6~10 of table
As seen from the above table, the nano hybridization ceramic resin performance indicator of the hydroxyl in embodiment 6~10 is set in qualification
Within the scope of fat prod performance indicator, therefore, the product of the preparation of the embodiment of the present invention 6~10 be can determine whether as qualified products.
Wherein embodiment 6,7,8 shows nano oxidized aluminium content in the increase nano hybridization ceramic resin with nano oxidized aluminium content
Increase therewith, embodiment 6,9,10 is compared, show the reduction with methyl phenyl silicone intermediates content, viscosity also with
Reduction, illustrate that the content of methyl phenyl silicone intermediate influences the viscosity of nano hybridization ceramic resin, while with end
The content for reducing hydroxyl in resin of hydroxyl polysiloxane intermediate is also opposite to be reduced.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of nano hybridization ceramic resin, which comprises the following steps:
(1) it prepares nano oxidized suspension: nano aluminium oxide and deionized water is passed through into machinery by the weight ratio of 25-30:70-75
Power mixing, obtains nano aluminium oxide initial mixing liquid, and nano material dispersion is added in the nano aluminium oxide initial mixing liquid
Agent, coupling agent, pH adjusting agent and cosolvent, are uniformly mixed, and obtain nano aluminium oxide suspension;
(2) it prepares nano alumina sol: unitary strong acid being added in the nano aluminium oxide suspension made from step (1), it is described
The molar ratio of unitary strong acid and nano aluminium oxide suspension is 0.02: 1, is stirred evenly, 1~3h to get solid content be 25~
The nano alumina sol of 30wt%;
(3) prepare nano hybridization ceramic resin: the nano alumina sol for taking step (2) to prepare is placed in synthesis reaction vessel,
Under 40 DEG C of stirrings of constant temperature, the silicone intermediates for having functional group are at the uniform velocity added dropwise, are dripped off in 1~2h, keeps permanent
Temperature until solution is completely limpid, complete by reaction, finally adjusts pH value, pH value is adjusted to 6~7 with pH adjusting agent, obtains nanometer
Hydridization ceramic resin.
2. the preparation method of nano hybridization ceramic resin as described in claim 1, which is characterized in that the nanometer of the step (1)
The partial size of aluminium oxide is 10~20nm.
3. the preparation method of nano hybridization ceramic resin as described in claim 1, which is characterized in that the nanometer of the step (1)
The weight ratio of material dispersing agent and nano aluminium oxide is 1: 0.5~1.
4. the preparation method of nano hybridization ceramic resin as described in claim 1, which is characterized in that the coupling of the step (1)
Agent is silane coupling agent, titanate coupling agent or aluminate coupling agent, and additive amount is that additive amount is nano aluminium oxide initial mixing
The 1~3% of liquid quality.
5. the preparation method of nano hybridization ceramic resin as described in claim 1, which is characterized in that the coupling of the step (1)
Agent is titanate coupling agent.
6. the preparation method of nano hybridization ceramic resin as described in claim 1, which is characterized in that the pH tune of the step (1)
Section agent is lactic acid, and additive amount is the 0.2~0.5% of nano aluminium oxide initial mixing liquid mass parts, by the pH value tune of reaction system
To 2~5;The cosolvent of the step (1) is ether alcohols solvent, and additive amount is the 1 of nano aluminium oxide initial mixing liquid mass parts
~3%.
7. the preparation method of nano hybridization ceramic resin as described in claim 1, which is characterized in that the unitary of the step (2)
Strong acid is hydrochloric acid or nitric acid.
8. the preparation method of nano hybridization ceramic resin as described in claim 1, which is characterized in that the step (3) is with active
The functional group of the silicone intermediates of energy group is carboxyl, hydroxyl, epoxy group, alkoxy or amide groups.
9. the preparation method of nano hybridization ceramic resin as described in claim 1, which is characterized in that the step (3) is with active
The silicone intermediates of energy group are methyl phenyl silicone intermediate;Select the conduct of methyl phenyl silicone intermediate
Raw material finally obtains the nano hybridization ceramic resin of not hydroxyl.
10. the preparation method of nano hybridization ceramic resin as described in claim 1, which is characterized in that the step (3) is with active
The silicone intermediates of energy group are hydroxy-terminated polysiloxane intermediate;Select hydroxy-terminated polysiloxane intermediate as former
Material, finally obtains the nano hybridization ceramic resin of hydroxyl.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116023810A (en) * | 2023-01-29 | 2023-04-28 | 深圳市纳能科技有限公司 | Cold-resistant high-temperature-resistant inorganic heat reflection coating for building and metal surfaces and preparation method thereof |
Citations (3)
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CN102010620A (en) * | 2010-11-04 | 2011-04-13 | 广州慧谷化学有限公司 | Method for preparing high-concentration nano aluminum hydroxide aqueous dispersion and prepared product |
CN103496724A (en) * | 2013-08-30 | 2014-01-08 | 航天特种材料及工艺技术研究所 | Preparation method of nano alumina sol and gel |
CN106398333A (en) * | 2016-09-10 | 2017-02-15 | 上海大学 | Preparation method of nano sol hybrid polysiloxane magnesium alloy surface preservative |
-
2018
- 2018-10-26 CN CN201811257934.8A patent/CN109504277A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102010620A (en) * | 2010-11-04 | 2011-04-13 | 广州慧谷化学有限公司 | Method for preparing high-concentration nano aluminum hydroxide aqueous dispersion and prepared product |
CN103496724A (en) * | 2013-08-30 | 2014-01-08 | 航天特种材料及工艺技术研究所 | Preparation method of nano alumina sol and gel |
CN106398333A (en) * | 2016-09-10 | 2017-02-15 | 上海大学 | Preparation method of nano sol hybrid polysiloxane magnesium alloy surface preservative |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116023810A (en) * | 2023-01-29 | 2023-04-28 | 深圳市纳能科技有限公司 | Cold-resistant high-temperature-resistant inorganic heat reflection coating for building and metal surfaces and preparation method thereof |
CN116023810B (en) * | 2023-01-29 | 2024-03-26 | 深圳市纳能科技有限公司 | Cold-resistant high-temperature-resistant inorganic heat reflection coating for building and metal surfaces and preparation method thereof |
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Application publication date: 20190322 |