CN108192484A - A kind of preparation method of the mould proof polyester coating of sulfhydryl modified silica - Google Patents
A kind of preparation method of the mould proof polyester coating of sulfhydryl modified silica Download PDFInfo
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- CN108192484A CN108192484A CN201711459918.2A CN201711459918A CN108192484A CN 108192484 A CN108192484 A CN 108192484A CN 201711459918 A CN201711459918 A CN 201711459918A CN 108192484 A CN108192484 A CN 108192484A
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/58—Epoxy resins
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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
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a kind of preparation methods of the sulfhydryl modified mould proof polyester coating of silica, nano silicon dioxide is dispersed in toluene, it is carried out using mercaptopropyl trimethoxysilane sulfhydryl modified, it is dispersed in distilled water after being processed into powder later, acetic acid is added dropwise, add in chitosan, algal polysaccharides are reacted, it is mixed after post processing with montmorillonite, nano bamboo fiber, obtain mixed-powder, water-soluble poly ester monomer is subjected to reaction later, polyester is made, mixed powder with polyester is mixed, is added after other ingredients after ball milling removal solvent both.The present invention prepares the sulfhydryl modified nano silicon dioxide of microencapsulation, applies in the preparation of coating so that the coating of preparation has the performances such as mould proof, wear-resisting scratch resistance.
Description
Technical field
The invention belongs to coating material fields, and in particular to a kind of preparation of the sulfhydryl modified mould proof polyester coating of silica
Method.
Background technology
Small molecule sulfhydryl compound is because its unique resistance to the oxygen inhibiting polymerization performance is concerned in curing field, but small molecule
The stink of sulfhydryl compound limits its practical application in photocureable coating system, therefore, grafting how is carried out to it and is changed
Property with reduce its odor problem be one merit attention the technical issues of.As the curing organic-inorganic hybridized system of ultraviolet light is ground
Small molecule sulfhydryl compound is grafted on inorganic nanoparticles surface and prepared based on sulfydryl-double bond by the rise studied carefully and gradual perfection
The hybrid material of click-reaction is possibly realized.
Invention content
The present invention provides a kind of preparation method of the sulfhydryl modified mould proof polyester coating of silica, and the present invention prepares microcapsules
Change sulfhydryl modified nano silicon dioxide, apply in the preparation of coating so that the coating of preparation has mould proof, wear-resisting scratch resistance etc.
Performance.
The present invention is achieved by the following technical solutions：
A kind of preparation method of the mould proof polyester coating of sulfhydryl modified silica, which is characterized in that include the following steps：
（1）Sulfhydryl modified silica
By the nano silicon dioxide after the vacuum drying of 2-5 parts by weight, mechanical agitation and ultrasonic disperse 20-30 divide in q. s. toluene
Clock is warming up to reflux state, continues stirring 20-30 minutes, and it is anhydrous that 2-10 parts by weight of deionized water, 2-10 parts by weight are added dropwise later
Ethyl alcohol and 2-3 parts by weight formic acid and 10-20 parts by weight mercaptopropyl trimethoxysilanes after being refluxed 4-5 hours, are crossed and are filtered dry
It is dry, it extracts 12 hours, it is 12 hours dry under vacuum, for use；
（2）Microencapsulation and mixed-powder
By step（1）Gains dissolving is in the 5-10 times of distilled water measured that a concentration of 35wt% is added dropwise after 30-40 minutes in stirring
Acetic acid, after adjusting pH value to 4-5, add in 5-10 parts by weight chitosans, 5-10 parts by weight algal polysaccharides, be heated to 55-65 DEG C
It after isothermal reaction 3-4 hours, after supersound process, is dried using freeze drier, with the montmorillonite of 5-15 parts by weight, 5-15 parts by weight
Nano bamboo fiber mixes, and obtains mixed-powder, for use；
（3）The preparation of polyester
By 10-15 parts by weight aqueous polyurethane monomers and 1-2 parts by weight Monobutyltins tin oxide, 1-5 parts by weight water-base epoxy trees
Fat is added in after distilled water is diluted and is added in reaction kettle, is risen to 165-175 DEG C and is kept the temperature 1-2 hours, rises to 175-185 DEG C of heat preservation
It 4-5 hours, rises to 185-195 DEG C and keeps the temperature 2-3 hours, rise to 195-205 DEG C and keep the temperature 2-3 hours, be cooled to room temperature, pour into ball milling
In tank, ball milling adds in 0.5-2 parts by weight wetting dispersing agents, for use after 2-3 hours after suitable water is added dropwise；
（4）Mixing
By step（2）Gains add in step（3）It in the component of middle completion, is added in dispersion, high speed dispersion is uniform, adds in matter
Score is measured as 20% mixed fillers, 2-5 parts by weight waterborne film-forming auxiliary agent butyl glycol ethers, 0.5-1 parts by weight O P-10 emulsifiers,
0.5-1 parts by weight antifoaming agent, 0.2-0.5 parts per weight dispersing agents, continuation ball milling adds in 2-3 parts by weight after 2-3 hours diluted solid
Agent (BH-620), then vacuumizes removal solvent, stirs evenly rear filtering and discharging, both obtains the sulfhydryl modified silica
Mould proof polyester coating.
The quality dosage of the toluene is that the solid content of the nano silicon dioxide is made to be 15-20 times.
The quality dosage of the water is that the solid content of the polyester is made to be 20wt%~55wt%.
The mixed fillers include talcum powder, barium sulfate, calcium carbonate.
The solvent be one kind in industrial alcohol, butanol, propylene glycol monomethyl ether, butyl glycol ether, pyruvic alcohol or
Several compounding compositions.
It is an advantage of the invention that：
Nano silicon dioxide is dispersed in toluene by the present invention, carried out using mercaptopropyl trimethoxysilane it is sulfhydryl modified, later
Be dispersed in distilled water after being processed into powder, acetic acid be added dropwise, added in chitosan, algal polysaccharides and reacted, after post processing with illiteracy
De- soil, nano bamboo fiber mixing, obtain mixed-powder, and water-soluble poly ester monomer is carried out reaction later is made polyester, by mixed powder
It mixes, is added after other ingredients after ball milling removal solvent both with polyester.Mercaptosilane coupling agents are connect by modification by coupling
Branch is prepared for the modified manometer silicon dioxide containing sulfydryl to nano-silica surface, and the sulfydryl on surface reduces oxygen inhibition and makees
With, have higher polymerization speed and conversion ratio, reduce agglomeration.Chitosan, algal polysaccharides are cross-linking, are formed apparent
Network blackboard coordinates sulfhydryl modified nano silicon dioxide to add, and forms microcapsule structure, can be improved using in coating
Coating ductility, by with have the water-soluble poly ester monomer of certain degree of cross linking with Long carbon chain flexibility aqueous epoxy resins match
It closes, improves wear-resisting scratch resistance capability, ball milling causes montmorillonite, nano bamboo fiber, the sulfhydryl modified nano silicon dioxide of microencapsulation
Disperse well in coating, form close anchor structure, improve mechanical property and water resistance.The present invention prepares microencapsulation
Sulfhydryl modified nano silicon dioxide is applied in the preparation of coating so that the coating of preparation has the property such as mould proof, wear-resisting scratch resistance
Energy.
Specific embodiment
A kind of preparation method of the mould proof polyester coating of sulfhydryl modified silica, which is characterized in that include the following steps：
（1）Sulfhydryl modified silica
Nano silicon dioxide after 4 parts by weight are dried in vacuo mechanical agitation and ultrasonic disperse 20 minutes in q. s. toluene, rise
Temperature continues stirring 30 minutes, 10 parts by weight of deionized water, 5 parts by weight absolute ethyl alcohols and 3 parts by weight is added dropwise later to reflux state
Formic acid and 15 parts by weight mercaptopropyl trimethoxysilanes, after being refluxed 4 hours, filtration drying extracts 12 hours, in vacuum
Under the conditions of dry 12 hours, for use；
（2）Microencapsulation and mixed-powder
By step（1）Gains dissolving is in the distilled water of 8 times of amounts that the acetic acid of a concentration of 35wt% is added dropwise in stirring after 35 minutes,
After adjusting pH value to 4-5,8 parts by weight chitosans, 8 parts by weight algal polysaccharides are added in, after being heated to 60 DEG C of isothermal reactions 3 hours,
It after supersound process, is dried using freeze drier, mixes, mixed with 10 parts by weight montmorillonites, 10 parts by weight nano bamboo fibers
Powder is closed, for use；
（3）The preparation of polyester
12 parts by weight aqueous polyurethane monomers and 2 parts by weight Monobutyltin tin oxide, 3 parts by weight aqueous epoxy resins are added in and steamed
Distilled water is added in after being diluted in reaction kettle, is risen to 170 DEG C and is kept the temperature 1 hour, is risen to 180 DEG C and is kept the temperature 4 hours, rises to 190 DEG C of guarantors
Temperature 2 hours rises to 200 DEG C and keeps the temperature 2 hours, is cooled to room temperature, pours into ball grinder, ball milling is after 2 hours, after suitable water is added dropwise
0.8 parts by weight wetting dispersing agent is added in, for use；
（4）Mixing
By step（2）Gains add in step（3）It in the component of middle completion, is added in dispersion, high speed dispersion is uniform, adds in matter
Score is measured as 20% mixed fillers, 3 parts by weight waterborne film-forming auxiliary agent butyl glycol ethers, 0.8 parts by weight O P-10 emulsifiers, 0.8
Parts by weight antifoaming agent, 0.3 parts per weight dispersing agent continue ball milling and the diluted curing agent of 2 parts by weight (BH-620) are added in after 2 hours,
Then removal solvent is vacuumized, stirs evenly rear filtering and discharging, both obtains the mould proof polyester coating of sulfhydryl modified silica.
The quality dosage of the toluene is that the solid content of the nano silicon dioxide is made to be 18 times.
The quality dosage of the water is that the solid content of the polyester is made to be 20wt%~55wt%.
The mixed fillers include talcum powder, barium sulfate, calcium carbonate.
The solvent be one kind in industrial alcohol, butanol, propylene glycol monomethyl ether, butyl glycol ether, pyruvic alcohol or
Several compounding compositions.
Claims (5)
1. a kind of preparation method of the mould proof polyester coating of sulfhydryl modified silica, which is characterized in that include the following steps：
Sulfhydryl modified silica
By the nano silicon dioxide after the vacuum drying of 2-5 parts by weight, mechanical agitation and ultrasonic disperse 20-30 divide in q. s. toluene
Clock is warming up to reflux state, continues stirring 20-30 minutes, and it is anhydrous that 2-10 parts by weight of deionized water, 2-10 parts by weight are added dropwise later
Ethyl alcohol and 2-3 parts by weight formic acid and 10-20 parts by weight mercaptopropyl trimethoxysilanes after being refluxed 4-5 hours, are crossed and are filtered dry
It is dry, it extracts 12 hours, it is 12 hours dry under vacuum, for use；
Microencapsulation and mixed-powder
By step（1）Gains dissolving is in the 5-10 times of distilled water measured that a concentration of 35wt% is added dropwise after 30-40 minutes in stirring
Acetic acid, after adjusting pH value to 4-5, add in 5-10 parts by weight chitosans, 5-10 parts by weight algal polysaccharides, be heated to 55-65 DEG C
It after isothermal reaction 3-4 hours, after supersound process, is dried using freeze drier, with the montmorillonite of 5-15 parts by weight, 5-15 parts by weight
Nano bamboo fiber mixes, and obtains mixed-powder, for use；
（3）The preparation of polyester
By 10-15 parts by weight aqueous polyurethane monomers and 1-2 parts by weight Monobutyltins tin oxide, 1-5 parts by weight water-base epoxy trees
Fat is added in after distilled water is diluted and is added in reaction kettle, is risen to 165-175 DEG C and is kept the temperature 1-2 hours, rises to 175-185 DEG C of heat preservation
It 4-5 hours, rises to 185-195 DEG C and keeps the temperature 2-3 hours, rise to 195-205 DEG C and keep the temperature 2-3 hours, be cooled to room temperature, pour into ball milling
In tank, ball milling adds in 0.5-2 parts by weight wetting dispersing agents, for use after 2-3 hours after suitable water is added dropwise；
（4）Mixing
By step（2）Gains add in step（3）It in the component of middle completion, is added in dispersion, high speed dispersion is uniform, adds in matter
Score is measured as 20% mixed fillers, 2-5 parts by weight waterborne film-forming auxiliary agent butyl glycol ethers, 0.5-1 parts by weight O P-10 emulsifiers,
0.5-1 parts by weight antifoaming agent, 0.2-0.5 parts per weight dispersing agents, continuation ball milling adds in 2-3 parts by weight after 2-3 hours diluted solid
Agent (BH-620), then vacuumizes removal solvent, stirs evenly rear filtering and discharging, both obtains the sulfhydryl modified silica
Mould proof polyester coating.
2. according to a kind of preparation method of the sulfhydryl modified mould proof polyester coating of silica of claim 1, which is characterized in that described
The quality dosage of toluene is that the solid content of the nano silicon dioxide is made to be 15-20 times.
3. according to a kind of preparation method of the sulfhydryl modified mould proof polyester coating of silica of claim 1, which is characterized in that described
The quality dosage of water is that the solid content of the polyester is made to be 20wt%~55wt%.
4. according to a kind of preparation method of the sulfhydryl modified mould proof polyester coating of silica of claim 1, which is characterized in that described
Mixed fillers include talcum powder, barium sulfate, calcium carbonate.
5. according to a kind of preparation method of the sulfhydryl modified mould proof polyester coating of silica of claim 1, which is characterized in that described
Solvent be one or several kinds of compounding compositions in industrial alcohol, butanol, propylene glycol monomethyl ether, butyl glycol ether, pyruvic alcohol.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711459918.2A CN108192484A (en) | 2017-12-28 | 2017-12-28 | A kind of preparation method of the mould proof polyester coating of sulfhydryl modified silica |
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| CN201711459918.2A CN108192484A (en) | 2017-12-28 | 2017-12-28 | A kind of preparation method of the mould proof polyester coating of sulfhydryl modified silica |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117070186A (en) * | 2023-10-18 | 2023-11-17 | 山东景茂新材料有限公司 | Preparation method of alcohol type silicone sealant |
| CN117064137A (en) * | 2023-08-18 | 2023-11-17 | 诚天科技实业(广东)有限公司 | Efficient breathable waterproof sports shoes and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914190A (en) * | 2010-08-17 | 2010-12-15 | 浙江理工大学 | Preparation method of modified nano-silica monomer dispersion liquid |
| CN104087126A (en) * | 2014-07-15 | 2014-10-08 | 南京航空航天大学 | Marine anticorrosive coating |
| CN106244102A (en) * | 2016-08-31 | 2016-12-21 | 安徽省阜阳沪千人造板制造有限公司 | A kind of mildew-resistant plate adhesive of bamboo fibre nanometer silver antimicrobial mildew-resistant potentiation |
| CN106928659A (en) * | 2017-03-15 | 2017-07-07 | 中南大学 | A kind of high wear resistant photo-cured aryl oxide based epoxy acrylate/nanometer silicon dioxide composite material and preparation method thereof |
-
2017
- 2017-12-28 CN CN201711459918.2A patent/CN108192484A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914190A (en) * | 2010-08-17 | 2010-12-15 | 浙江理工大学 | Preparation method of modified nano-silica monomer dispersion liquid |
| CN104087126A (en) * | 2014-07-15 | 2014-10-08 | 南京航空航天大学 | Marine anticorrosive coating |
| CN106244102A (en) * | 2016-08-31 | 2016-12-21 | 安徽省阜阳沪千人造板制造有限公司 | A kind of mildew-resistant plate adhesive of bamboo fibre nanometer silver antimicrobial mildew-resistant potentiation |
| CN106928659A (en) * | 2017-03-15 | 2017-07-07 | 中南大学 | A kind of high wear resistant photo-cured aryl oxide based epoxy acrylate/nanometer silicon dioxide composite material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117064137A (en) * | 2023-08-18 | 2023-11-17 | 诚天科技实业(广东)有限公司 | Efficient breathable waterproof sports shoes and preparation method thereof |
| CN117064137B (en) * | 2023-08-18 | 2024-04-19 | 诚天科技实业(广东)有限公司 | Efficient breathable waterproof sports shoes and preparation method thereof |
| CN117070186A (en) * | 2023-10-18 | 2023-11-17 | 山东景茂新材料有限公司 | Preparation method of alcohol type silicone sealant |
| CN117070186B (en) * | 2023-10-18 | 2023-12-26 | 山东景茂新材料有限公司 | Preparation method of alcohol type silicone sealant |
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Application publication date: 20180622 |