CN109251654A - A kind of preparation method of polyurethane-alumina composite coating material - Google Patents

A kind of preparation method of polyurethane-alumina composite coating material Download PDF

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Publication number
CN109251654A
CN109251654A CN201811016220.8A CN201811016220A CN109251654A CN 109251654 A CN109251654 A CN 109251654A CN 201811016220 A CN201811016220 A CN 201811016220A CN 109251654 A CN109251654 A CN 109251654A
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China
Prior art keywords
coating material
composite coating
polyurethane
alumina composite
conditions
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CN201811016220.8A
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Chinese (zh)
Inventor
陈伟
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Zhangjiagang City Fook New Mstar Technology Ltd
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Zhangjiagang City Fook New Mstar Technology Ltd
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Priority to CN201811016220.8A priority Critical patent/CN109251654A/en
Publication of CN109251654A publication Critical patent/CN109251654A/en
Withdrawn legal-status Critical Current

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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
    • C09D175/08—Polyurethanes from polyethers
    • 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
    • C08G18/48—Polyethers
    • 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
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
    • 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
    • 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
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a kind of polyurethane-alumina composite coating material preparation methods, it include: that three aluminium butoxides and surfactant are dissolved in organic solvent by (1), chelating agent is added, ultrasound keeps its evenly dispersed, then the isopropanol and distillation water mixed liquid that volume ratio is 3:1 is slowly added dropwise, at 60~80 DEG C reaction 12~for 24 hours, obtain alumina sol；(2) the pure and mild methyl diphenylene diisocyanate of polyether polyols is mixed, stirs evenly, adds a certain amount of dibutyl tin dilaurate and 1,4- butanediol, 3~8min is stirred under the conditions of 1000~1500rpm, 1~2h of vacuum outgas obtains polyaminoester emulsion；(3) alumina sol and polyaminoester emulsion are mixed, add curing agent, it stirs evenly, it pours into dry mold and is solidified, wherein, condition of cure are as follows: solidify 2~4h under the conditions of prior to 70~90 DEG C, solidify 2~4h under the conditions of 100~120 DEG C, obtain polyurethane-alumina composite coating material.Polyurethane-alumina composite coating material in the present invention has preferable tensile property and toughening effect.

Description

A kind of preparation method of polyurethane-alumina composite coating material
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation of polyurethane-alumina composite coating material Method.
Background technique
In recent years, problems of energy consumption is more severe, and demand of the people to energy-saving and emission-reduction material increasingly increases.It has both heat-insulated The multi-functional coatings of wear-resisting property can effectively reduce coating surface and internal temperature, extends equipment life, has ten to energy-saving Divide important meaning.Multi-functional coatings are made of film forming matter and functional filler.Film forming matter is mostly made of resin, and tradition is molten Dosage form resin includes a large amount of volatilizable organic compounds, endangers environment and water resistance is poor, significantly limit its application.Oxidation The functional fillers such as aluminium flake, titanium dioxide, silica, zinc oxide enhance the intensity of coating, hardness, resistance to a certain extent Mill, etc. mechanical properties and assign the characteristics such as the heat-insulated, antibacterial of coating.But it is light that the disadvantages of its density is high, uniformity is poor limits coating Application and the development of matter.
In the preparation method of alumina modified acrylic resin type powdery paints disclosed in the prior art, which has Excellent adhesive attraction, weatherability, corrosion resistance, but this method, using solid alumina as functional filler, gained coating density is larger And production process is complicated, is difficult to control.In addition, coating disclosed in the prior art with water-and acrylate lotion with it is aqueous Epoxy resin latex is compound to be used as organic binder, and nano-aluminum hydroxide, ceramic hollow microballon, titanium dioxide etc. are inorganic filler Prepare the heat-insulating, fire-preventing coating haveing excellent performance.But gained coating can decompose under heated environment and generate H2O forms stomata, Accelerate the failure of coating mechanical property, and makes the tensile property of the coating poor.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of polyurethane-alumina composite coating material, It is able to solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of polyurethane-alumina composite coating material preparation methods, existing to overcome There is the deficiency in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of polyurethane-alumina composite coating material, comprising:
(1) three aluminium butoxides and surfactant being dissolved in organic solvent, chelating agent is added, ultrasound keeps its evenly dispersed, Then be slowly added dropwise volume ratio be 3:1 isopropanol and distillation water mixed liquid, at 60~80 DEG C react 12~for 24 hours, obtain oxygen Change Aluminum sol；
(2) the pure and mild methyl diphenylene diisocyanate of polyether polyols is mixed, stirs evenly, adds a certain amount of February Dilaurylate and 1,4-butanediol, stir 3~8min under the conditions of 1000~1500rpm, and 1~2h of vacuum outgas is obtained Polyaminoester emulsion；
(3) alumina sol and polyaminoester emulsion are mixed, adds curing agent, stir evenly, pours into dry mold In solidified, wherein condition of cure are as follows: solidify 2~4h under the conditions of prior to 70~90 DEG C, it is solid under the conditions of 100~120 DEG C Change 2~4h, obtains polyurethane-alumina composite coating material.
Preferably, in step (1), the surfactant is cetyl trimethylammonium bromide or cetyl trimethyl Ammonium chloride, the chelating agent are ethyl acetoacetate.
Preferably, in step (1), three aluminium butoxide, the surfactant, the chelating agent molar ratio be 10~ 20:3~8:1.
Preferably, in step (2), the dibutyl tin dilaurate additional amount is the 0.01 of the polyether polyol quality ~0.1%.
Preferably, in step (3), the curing agent additional amount is the 5~10% of the polyurethane quality.
Preferably, in step (3), the mass fraction of the aluminium oxide in the polyurethane-alumina composite coating material is 1.0~10.0%.
Preferably, the mass fraction of the aluminium oxide in the polyurethane-alumina composite coating material is 5.0%.
Compared with the prior art, the advantages of the present invention are as follows: polyurethane-alumina composite coating material obtained in the present invention Material has preferable tensile property, makes the composite coating material have excellent toughening effect by the way that aluminium oxide is added.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of polyurethane-alumina composite coating material, comprising:
(1) three aluminium butoxides and surfactant being dissolved in organic solvent, chelating agent is added, ultrasound keeps its evenly dispersed, Then be slowly added dropwise volume ratio be 3:1 isopropanol and distillation water mixed liquid, at 60~80 DEG C react 12~for 24 hours, obtain oxygen Change Aluminum sol；
(2) the pure and mild methyl diphenylene diisocyanate of polyether polyols is mixed, stirs evenly, adds a certain amount of February Dilaurylate and 1,4-butanediol, stir 3~8min under the conditions of 1000~1500rpm, and 1~2h of vacuum outgas is obtained Polyaminoester emulsion；
(3) alumina sol and polyaminoester emulsion are mixed, adds curing agent, stir evenly, pours into dry mold In solidified, wherein condition of cure are as follows: solidify 2~4h under the conditions of prior to 70~90 DEG C, it is solid under the conditions of 100~120 DEG C Change 2~4h, obtains polyurethane-alumina composite coating material.
Wherein, in step (1), the surfactant is cetyl trimethylammonium bromide or cetyl trimethyl chlorine Change ammonium, the chelating agent is ethyl acetoacetate；The molar ratio of three aluminium butoxide, the surfactant, the chelating agent For 10~20:3~8:1, it is preferred that three aluminium butoxide, the surfactant, the chelating agent molar ratio be 15:5: 1。
Wherein, in step (2), the dibutyl tin dilaurate additional amount be the polyether polyol quality 0.01~ 0.1%, it is preferred that the dibutyl tin dilaurate additional amount is the 0.05% of the polyether polyol quality.
Wherein, in step (3), the curing agent additional amount is the 5~10% of the polyurethane quality, it is preferred that described Curing agent additional amount is the 7.5% of the polyurethane quality；Aluminium oxide in the polyurethane-alumina composite coating material Mass fraction is 1.0~10.0%, it is preferred that the quality of the aluminium oxide in the polyurethane-alumina composite coating material point Number is 5.0%.
It is following that polyurethane in the present invention-alumina composite coating material preparation side is illustrated with specifically embodiment Method.
Embodiment 1
(1) three aluminium butoxides and surfactant being dissolved in organic solvent, chelating agent is added, ultrasound keeps its evenly dispersed, Then the isopropanol and distillation water mixed liquid that volume ratio is 3:1 is slowly added dropwise, reacts 12h at 60 DEG C, obtains alumina sol, Wherein, three aluminium butoxide, the surfactant, the chelating agent molar ratio be 10:3:1；
(2) the pure and mild methyl diphenylene diisocyanate of polyether polyols is mixed, stirs evenly, adds a certain amount of February Dilaurylate and 1,4-butanediol stir 3min under the conditions of 1000rpm, and vacuum outgas 1h obtains polyaminoester emulsion, In, the dibutyl tin dilaurate additional amount is the 0.01% of the polyether polyol quality；
(3) alumina sol and polyaminoester emulsion are mixed, adds curing agent, stir evenly, pours into dry mold In solidified, wherein condition of cure are as follows: solidify 2h under the conditions of prior to 70 DEG C, solidify 2h under the conditions of 100 DEG C, gathered Urethane-alumina composite coating material, wherein the curing agent additional amount is the 5% of the polyurethane quality.
Embodiment 2
(1) three aluminium butoxides and surfactant being dissolved in organic solvent, chelating agent is added, ultrasound keeps its evenly dispersed, Then the isopropanol and distillation water mixed liquid that volume ratio is 3:1 is slowly added dropwise, reacts 18h at 70 DEG C, obtains alumina sol, Wherein, three aluminium butoxide, the surfactant, the chelating agent molar ratio be 15:5:1；
(2) the pure and mild methyl diphenylene diisocyanate of polyether polyols is mixed, stirs evenly, adds a certain amount of February Dilaurylate and 1,4-butanediol stir 5min under the conditions of 1200rpm, and vacuum outgas 1.5h obtains polyaminoester emulsion, Wherein, the dibutyl tin dilaurate additional amount is the 0.05% of the polyether polyol quality；
(3) alumina sol and polyaminoester emulsion are mixed, adds curing agent, stir evenly, pours into dry mold In solidified, wherein condition of cure are as follows: solidify 3h under the conditions of prior to 80 DEG C, solidify 3h under the conditions of 110 DEG C, gathered Urethane-alumina composite coating material, wherein the curing agent additional amount is the 7.5% of the polyurethane quality.
Embodiment 3
(1) three aluminium butoxides and surfactant being dissolved in organic solvent, chelating agent is added, ultrasound keeps its evenly dispersed, Then the isopropanol and distillation water mixed liquid that volume ratio is 3:1 is slowly added dropwise, is reacted at 80 DEG C for 24 hours, obtains alumina sol, Wherein, three aluminium butoxide, the surfactant, the chelating agent molar ratio be 20:8:1；
(2) the pure and mild methyl diphenylene diisocyanate of polyether polyols is mixed, stirs evenly, adds a certain amount of February Dilaurylate and 1,4-butanediol stir 8min under the conditions of 1500rpm, and vacuum outgas 2h obtains polyaminoester emulsion, In, the dibutyl tin dilaurate additional amount is the 0.1% of the polyether polyol quality；
(3) alumina sol and polyaminoester emulsion are mixed, adds curing agent, stir evenly, pours into dry mold In solidified, wherein condition of cure are as follows: solidify 4h under the conditions of prior to 90 DEG C, solidify 4h under the conditions of 120 DEG C, gathered Urethane-alumina composite coating material, wherein the curing agent additional amount is the 10% of the polyurethane quality.
Aluminium oxide in the polyurethane according to made from the method in above-described embodiment 1~3-alumina composite coating material Mass fraction is 1.0~10.0%.
Tension test is carried out to the composite coating material in the present invention using WDT-20 microcomputer controlled electronic universal tester, When the mass fraction of the aluminium oxide of material in composite coating is 5.0%, the tensile property of the composite coating material is best；Separately Outside, make the composite coating material that there is excellent toughening effect by the way that aluminium oxide is added.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.

Claims (7)

1. a kind of polyurethane-alumina composite coating material preparation method characterized by comprising
(1) three aluminium butoxides and surfactant are dissolved in organic solvent, chelating agent is added, ultrasound keeps its evenly dispersed, then Be slowly added dropwise volume ratio be 3:1 isopropanol and distillation water mixed liquid, at 60~80 DEG C react 12~for 24 hours, obtain aluminium oxide Colloidal sol；
(2) the pure and mild methyl diphenylene diisocyanate of polyether polyols is mixed, stirs evenly, adds a certain amount of tin dilaurate Dibutyl tin and 1,4-butanediol, stir 3~8min under the conditions of 1000~1500rpm, and 1~2h of vacuum outgas obtains poly- ammonia Ester lotion；
(3) alumina sol and polyaminoester emulsion are mixed, add curing agent, stir evenly, pour into dry mold into Row solidification, wherein condition of cure are as follows: solidify 2~4h under the conditions of prior to 70~90 DEG C, solidify 2 under the conditions of 100~120 DEG C ~4h obtains polyurethane-alumina composite coating material.
2. polyurethane according to claim 1-alumina composite coating material preparation method, which is characterized in that step (1) in, the surfactant is cetyl trimethylammonium bromide or hexadecyltrimethylammonium chloride, and the chelating agent is Ethyl acetoacetate.
3. polyurethane according to claim 1-alumina composite coating material preparation method, which is characterized in that step (1) in, three aluminium butoxide, the surfactant, the chelating agent molar ratio be 10~20:3~8:1.
4. polyurethane according to claim 1-alumina composite coating material preparation method, which is characterized in that step (2) in, the dibutyl tin dilaurate additional amount is the 0.01~0.1% of the polyether polyol quality.
5. polyurethane according to claim 1-alumina composite coating material preparation method, which is characterized in that step (3) in, the curing agent additional amount is the 5~10% of the polyurethane quality.
6. polyurethane according to claim 1-alumina composite coating material preparation method, which is characterized in that step (3) in, the mass fraction of the aluminium oxide in the polyurethane-alumina composite coating material is 1.0~10.0%.
7. polyurethane according to claim 6-alumina composite coating material preparation method, which is characterized in that described The mass fraction of aluminium oxide in polyurethane-alumina composite coating material is 5.0%.
CN201811016220.8A 2018-09-02 2018-09-02 A kind of preparation method of polyurethane-alumina composite coating material Withdrawn CN109251654A (en)

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Publication number Priority date Publication date Assignee Title
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CN105176366A (en) * 2015-07-17 2015-12-23 河南科技大学 Preparation method of wear-resistant anti-microbial coating for sports equipment
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KR20140081574A (en) * 2012-12-21 2014-07-01 주식회사 포스코 Cr-FREE SURFACE TREATMENT COMPOSITIONS AND SURFACE TREATED GALVANIZED STEEL SHEET USING THEREOF
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CN105176366A (en) * 2015-07-17 2015-12-23 河南科技大学 Preparation method of wear-resistant anti-microbial coating for sports equipment
CN106011799A (en) * 2016-05-31 2016-10-12 华南理工大学 Preparation method for corrosion-resistant and super-hydrophobic aluminum oxide membrane for zinc layer
CN108395742A (en) * 2018-05-12 2018-08-14 浙江大学 A kind of aperture is in obturator-type anti-corrosive metal coating, the preparation method and use of normal distribution

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