CN110079206A - A kind of aqueous polyurethane three-proofing coating and preparation method thereof - Google Patents
A kind of aqueous polyurethane three-proofing coating and preparation method thereof Download PDFInfo
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- CN110079206A CN110079206A CN201910380482.0A CN201910380482A CN110079206A CN 110079206 A CN110079206 A CN 110079206A CN 201910380482 A CN201910380482 A CN 201910380482A CN 110079206 A CN110079206 A CN 110079206A
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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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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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
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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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
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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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
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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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
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
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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
- C09D175/06—Polyurethanes from polyesters
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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
-
- 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
- C09D7/20—Diluents or solvents
Abstract
The present invention is a kind of aqueous polyurethane three-proofing coating, is made of the raw material of following parts by weight: 40-60 parts of polyaminoester emulsion, 30-50 parts of deionized water, 1-5 parts of auxiliary agent；The polyaminoester emulsion is prepared by the raw material of following parts by weight: 10-20 parts of polyester polyol, 1-4 parts of Water-borne modification monomer, 1-4 parts of small molecule polyol, 10-15 parts of polyisocyanates, 10-15 parts of solvent, 0.02-0.08 parts of catalyst, 0.005-0.03 parts of neutralizer, 50-60 parts of deionized water, 0.005-0.03 parts of chain extender.Aqueous polyurethane three-proofing coating of the present invention is water-soluble good, and aromatic-free class solvent is free of lead substance, energy conservation and environmental protection is nuisanceless, it is dry after electrical insulation capability it is good, the NBC protective performance of good " waterproof, moisture-proof, dust-proof " can be played, and it is without side-effects to human body, market application prospect is good.
Description
Technical field
The invention belongs to coating synthesis technical fields, and in particular to a kind of aqueous polyurethane three-proofing coating, and further relate to described
The preparation method of aqueous polyurethane three-proofing coating.
Background technique
Three-proofing coating is to form coast of paint film after dry coated in PCB circuit board, plays the three of " waterproof, moisture-proof, dust-proof "
The coating of anti-effect, impact property and electrical insulation capability are good, and acid-alkali-corrosive-resisting is had excellent performance.At present on the market, most of poly-
Urethane three-proofing coating system is all based on oiliness, and containing a large amount of volatile solvents, the influence to human body and environment is very big, makes three proofings
The application of paint, which receives, greatly to be limited.
CN108949006A discloses a kind of non-harmful influence high-flash polyurethane three-proofing coating and includes at least by weight
Following components: 40~60 parts of polyurethane resin, 35~40 parts of non-hydrogenated petroleum ether, 10~20 parts of isomery aliphatic alkane, levelling help
0.5~3 part of agent, 0.5~3 part of defoaming agent, 0.5~3 part of wetting agent, 0.5~3 part of fire retardant.The technical solution improves three proofings
The flash-point of paint, but it is difficult to meet the needs of environmentally friendly.
CN103756544B discloses a kind of polyurethane three-proofing coating, and the polyurethane three-proofing coating includes following weight percent
Component: urethane alkyd 80-90%, cobalt class drier 3-4%, zirconium class drier 6-7%, calcium class drier 3-
9%, methyl ethyl ketoxime 0.7-1.2%, fluorescent powder 0.15-0.30%；Wherein urethane alkyd is by following weight %
The component of content is prepared: alkyd resin 45-55, polyisocyanates ester 2-6, small molecule polyol 4-8, small molecule single methanol 2-
4, solvent 40-50.The technical solution acid-fast alkali-proof is had excellent performance, and adhesive force is excellent, and surface drying speed is fast, however is also difficult to meet ring
Guaranteed request.
Therefore, in order to solve the sustainable development requirement of the growing market demand of three-proofing coating and environment, one is developed
Kind of aqueous, environmental protective polyurethane three-proofing coating have become there is an urgent need to.
Summary of the invention
Object of the present invention is in view of the deficiencies of the prior art, provide a kind of high-performance, extremely low VOC, environment friendly and pollution-free water
Property polyurethane three-proofing coating.
It is described that technical scheme is as follows.
A kind of aqueous polyurethane three-proofing coating, is made of the raw material of following parts by weight: 40-60 parts of polyaminoester emulsion, deionization
30-50 parts of water, 1-5 parts of auxiliary agent；
The polyaminoester emulsion is prepared by the raw material of following parts by weight: 10-20 parts of polyester polyol, Water-borne modification monomer
1-4 parts, 1-4 parts of small molecule polyol, 10-15 parts of polyisocyanates, 10-15 parts of solvent, 0.02-0.08 parts of catalyst, neutralization
0.005-0.03 parts of agent, 50-60 parts of deionized water, 0.005-0.03 parts of chain extender；
The preparation method of the polyaminoester emulsion the following steps are included:
(1) in the case of stirring, polyester polyol, Water-borne modification monomer and small molecule polyol are heated to 80-90 DEG C,
It vacuumizes 1-3 hours；
(2) mixed solution of (1) is cooled to 60-65 DEG C, solvent is added, polyisocyanates, isothermal reaction is then added
1-2 hours；
(3) mixed solution of (2) is heated up 63-67 DEG C, addition catalyst, isothermal reaction 0.5-1 hours；
(4) mixed solution of (3) is cooled to 40-43 DEG C, neutralizer is added under the revolving speed of 800-1600r/min, stirs
Mix 20-30min；
(5) revolving speed 1200-1600r/min is kept, water and chain extender is added in the mixed solution of (4), stirs 40-50min,
Polyaminoester emulsion is obtained after filtering.
The three-proofing coating of the present invention compared with prior art is to have used water as solvent, and water emulsification of entering is added to be made into three proofings
Paint, and the prior art uses organic solvent, therefore, technical solution of the present invention is very environmentally friendly.In order to realize the program, this hair
There are Water-borne modification monomer, the Water-borne modifications such as dihydromethyl propionic acid (DMPA), dimethylolpropionic acid (DMBA) inside bright polyaminoester emulsion
Monomer contains carboxyl-COOH, can first be grafted on polyurethane molecular, dimethylethanolamine, triethylamine, ammonium hydroxide, triethanolamine
Equal neutralizers contain amido, and carboxyl-COOH is neutralized with amido, production macromolecular polyurethane salt, and macromolecular polyurethane salt
Water can be dissolved under high speed dispersion.In particular, the prior art is molecular weight synthesis to be settled at one go, and the present invention is control point
Son amount, later period make molecular weight reach requirement, therefore, macromolecular polyurethane salt can be enabled to fill by introducing chain extender
Divide and is dissolved in water.
The first step of polyaminoester emulsion of the present invention is the pretreatment of raw material, removes the extra water in raw material, and second step is
Polymerization reaction, the cyanic acid group of polyisocyanates contain with polyester polyol, Water-borne modification monomer and small molecule polyol in raw material
Hydroxyl initial reaction, key reaction be OCNRNCO+R ' (OH) n → OCNRNHCOOR ' OH；Third step is catalysis reaction, mainly
Reaction is OCNRNHCOOR ' OH → OCN (RNHCOOR ') n ' RNCO；4th step is acid-base neutralization reaction, and Water-borne modification monomer contains
Carboxyl and neutralizer occur acid-base neutralization reaction, key reaction be RCOOH+R ' NH2 → RCOOHNR '；5th step is that chain extension is anti-
It answers, chain extending reaction occurs for the remaining cyanic acid group of macromolecule and chain extender, and key reaction is OCN (RNHCOOR ') n ' RNCO+
H2NR″NH2→-[CN(RNHCOOR′)n′RNC NR″]-n。
By above-mentioned preparation method, the present invention can water-soluble good aqueous polyurethane three-proofing coating, aromatic-free class
Solvent, is free of lead substance, and energy conservation and environmental protection is nuisanceless.
Preferably, the Water-borne modification monomer is dihydromethyl propionic acid and/or dimethylolpropionic acid；The neutralizer is two
One or more of methylethanolamine, triethylamine, ammonium hydroxide, triethanolamine.
Preferably, the polyester polyol be polyethylene glycol adipate glycol, polyadipate diglycol ester,
One or more of poly- 6-caprolactone, polycarbonate glycol type.
Preferably, the small molecule polyol is diglycol, 1,4-butanediol, 1,2-PD, 2,2,4-
One or more of trimethylpentanediol (TMPD), 1,6-HD, neopentyl glycol, trimethylolpropane.
Preferably, the polyisocyanates is toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate
(MDI), hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI), dicyclohexyl methyl hydride diisocyanate
(HMDI) and one or more of benzene dimethylene diisocyanate (XDI).
Preferably, the catalyst is one of dibutyl tin dilaurate, stannous octoate, dibutyltin diacetate
Or it is several.
Preferably, the chain extender is ethylenediamine, in 1,6- hexamethylene diamine, Isosorbide-5-Nitrae-cyclohexane diamine and isophorone diamine
One or more.
Preferably, the auxiliary agent includes one of defoaming agent, levelling agent, thickener, wetting agent or a variety of.
Preferably, the solvent is ketones solvent and/or amide solvent.
The present invention also protects the preparation method of three-proofing coating, and deionized water and auxiliary agent are stirred 10- in 1000-1500r/min
Polyaminoester emulsion is then added in 20min, and continues to stir 20-50min, and aqueous polyurethane three-proofing coating can be obtained.
The beneficial effects of the present invention are as follows:
(1) aqueous polyurethane three-proofing coating of the present invention is water-soluble good, aromatic-free class solvent, is free of lead substance, energy conservation
Environmental protection and public nuisance free；
(2) three-proofing coating of the invention is formed by paint film water-tolerant, and rub resistance can be excellent, electrical insulation capability after drying
It is good, the NBC protective performance of good " waterproof, moisture-proof, dust-proof " can be played；
(3) three-proofing coating simple production process of the invention, drying can also be dried from dry, and VOC is lower, and to human body without pair
Effect, market application prospect are good.
Specific embodiment
Specific embodiments of the present invention will be further explained below:
Embodiment 1 prepares three-proofing coating
(1) in the case of stirring, by 15kg polyethylene glycol adipate glycol (PEA), 2kg dihydromethyl propionic acid
(DMBA) and 3kg 1,4-butanediol is heated to 80 DEG C, vacuumizes 2 hours；
(2) mixed solution of (1) is cooled to 60 DEG C, 13kg butanone is added, 12kg toluene di-isocyanate(TDI) is then added
(TDI), isothermal reaction 2 hours；
(3) mixed solution of (2) is heated up 63 DEG C, addition 0.02kg stannous octoate, isothermal reaction 1 hour；
(4) mixed solution of (3) is cooled to 40 DEG C, 0.1kg dimethyl ethanol is added under the revolving speed of 1600r/min
Amine stirs 30min；
(5) keep revolving speed 1600r/min, the mixed solution of (4) be added 55kg deionized water and 0.01kg 1,6- oneself two
Amine stirs 40min, obtains polyaminoester emulsion after filtering；
(6) deionized water of 43kg is added in a reservoir, 4kg auxiliary agent is added and adds in 1500r/min high speed dispersion 10min
Enter the polyaminoester emulsion of (5) of 55kg, disperses 50min, aqueous polyurethane three-proofing coating A1 can be obtained.
Embodiment 2
(1) in the case of stirring, by 16kg polyadipate diglycol ester (PDA), 1.5kg dimethylolpropionic acid
(DMPA) and 3kg trimethylolpropane (TMP) is heated to 80 DEG C, vacuumizes 2 hours；
(2) mixed solution of (1) is cooled to 60 DEG C, 12kg dimethyl acetamide is added, the different Fo Er of 14kg is then added
Ketone diisocyanate, isothermal reaction 2 hours；
(3) mixed solution of (2) is heated up 63 DEG C, addition 0.01kg dibutyl tin dilaurate, isothermal reaction 1 hour；
(4) mixed solution of (3) is cooled to 40 DEG C, 0.15kg triethylamine, stirring is added under the revolving speed of 1600r/min
30min；
(5) revolving speed 1600r/min is kept, 55kg deionized water and 0.015kg ethylenediamine is added in the mixed solution of (4),
40min is stirred, obtains polyaminoester emulsion after filtering；
(6) deionized water of 46kg is added in a reservoir, 4kg auxiliary agent is added and adds in 1500r/min high speed dispersion 10min
Enter the polyaminoester emulsion of (5) of 56kg, disperses 50min, aqueous polyurethane three-proofing coating A2 can be obtained.
Embodiment 3 prepares three-proofing coating
(1) in the case of stirring, by 20kg polyethylene glycol adipate glycol (PEA), 4kg dihydromethyl propionic acid
(DMBA) and 4kg 1,4-butanediol is heated to 80 DEG C, vacuumizes 2 hours；
(2) mixed solution of (1) is cooled to 60 DEG C, 13kg butanone is added, 12kg toluene di-isocyanate(TDI) is then added
(TDI), isothermal reaction 2 hours；
(3) mixed solution of (2) is heated up 63 DEG C, addition 0.02kg stannous octoate, isothermal reaction 1 hour；
(4) mixed solution of (3) is cooled to 40 DEG C, 0.1kg dimethyl ethanol is added under the revolving speed of 1600r/min
Amine stirs 30min；
(5) keep revolving speed 1600r/min, the mixed solution of (4) be added 55kg deionized water and 0.01kg 1,6- oneself two
Amine stirs 40min, obtains polyaminoester emulsion after filtering；
(6) deionized water of 43kg is added in a reservoir, 4kg auxiliary agent is added and adds in 1500r/min high speed dispersion 10min
Enter the polyaminoester emulsion of (5) of 55kg, disperses 50min, aqueous polyurethane three-proofing coating A3 can be obtained.
Embodiment 4
(1) in the case of stirring, by 10kg polyadipate diglycol ester (PDA), 1kg dimethylolpropionic acid
(DMPA) and 1kg trimethylolpropane (TMP) is heated to 80 DEG C, vacuumizes 2 hours；
(2) mixed solution of (1) is cooled to 60 DEG C, 12kg dimethyl acetamide is added, the different Fo Er of 14kg is then added
Ketone diisocyanate, isothermal reaction 2 hours；
(3) mixed solution of (2) is heated up 63 DEG C, addition 0.01kg dibutyl tin dilaurate, isothermal reaction 1 hour；
(4) mixed solution of (3) is cooled to 40 DEG C, 0.15kg triethylamine, stirring is added under the revolving speed of 1600r/min
30min；
(5) revolving speed 1600r/min is kept, 55kg deionized water and 0.015kg ethylenediamine is added in the mixed solution of (4),
40min is stirred, obtains polyaminoester emulsion after filtering；
(6) deionized water of 46kg is added in a reservoir, 4kg auxiliary agent is added and adds in 1500r/min high speed dispersion 10min
Enter the polyaminoester emulsion of (5) of 56kg, disperses 50min, aqueous polyurethane three-proofing coating A4 can be obtained.
Comparative example
Comparative example 1
(1) in the case of stirring, by 15kg polyethylene glycol adipate glycol (PEA), 0.2kg dihydromethyl propionic acid
(DMBA) and 0.3kg 1,4-butanediol is heated to 80 DEG C, vacuumizes 2 hours；
(2) mixed solution of (1) is cooled to 60 DEG C, 13kg butanone is added, 12kg toluene di-isocyanate(TDI) is then added
(TDI), isothermal reaction 2 hours；
(3) mixed solution of (2) is heated up 63 DEG C, addition 0.02kg stannous octoate, isothermal reaction 1 hour；
(4) mixed solution of (3) is cooled to 40 DEG C, 0.1kg dimethyl ethanol is added under the revolving speed of 1600r/min
Amine stirs 30min；
(5) keep revolving speed 1600r/min, the mixed solution of (4) be added 55kg deionized water and 0.01kg 1,6- oneself two
Amine stirs 40min, obtains polyaminoester emulsion after filtering；
(6) deionized water of 43kg is added in a reservoir, 4kg auxiliary agent is added and adds in 1500r/min high speed dispersion 10min
Enter the polyaminoester emulsion of (5) of 55kg, disperses 50min, aqueous polyurethane three-proofing coating B1 can be obtained.
Comparative example 2
(1) in the case of stirring, by 20kg polyadipate diglycol ester (PDA), 0.5kg dimethylolpropionic acid
(DMPA) and 0.5kg trimethylolpropane (TMP) is heated to 80 DEG C, vacuumizes 2 hours；
(2) mixed solution of (1) is cooled to 60 DEG C, 12kg dimethyl acetamide is added, the different Fo Er of 14kg is then added
Ketone diisocyanate, isothermal reaction 2 hours；
(3) mixed solution of (2) is heated up 63 DEG C, addition 0.01kg dibutyl tin dilaurate, isothermal reaction 1 hour；
(4) mixed solution of (3) is cooled to 40 DEG C, 0.15kg triethylamine, stirring is added under the revolving speed of 1600r/min
30min；
(5) revolving speed 1600r/min is kept, 55kg deionized water and 0.015kg ethylenediamine is added in the mixed solution of (4),
40min is stirred, obtains polyaminoester emulsion after filtering；
(6) deionized water of 46kg is added in a reservoir, 4kg auxiliary agent is added and adds in 1500r/min high speed dispersion 10min
Enter the polyaminoester emulsion of (5) of 56kg, disperses 50min, aqueous polyurethane three-proofing coating B2 can be obtained.
Comparative example 3
(1) in the case of stirring, by 10kg polyethylene glycol adipate glycol (PEA), 5kg dihydromethyl propionic acid
(DMBA) and 5kg 1,4-butanediol is heated to 80 DEG C, vacuumizes 2 hours；
(2) mixed solution of (1) is cooled to 60 DEG C, 13kg butanone is added, 12kg toluene di-isocyanate(TDI) is then added
(TDI), isothermal reaction 2 hours；
(3) mixed solution of (2) is heated up 63 DEG C, addition 0.02kg stannous octoate, isothermal reaction 1 hour；
(4) mixed solution of (3) is cooled to 40 DEG C, 0.1kg dimethyl ethanol is added under the revolving speed of 1600r/min
Amine stirs 30min；
(5) keep revolving speed 1600r/min, the mixed solution of (4) be added 55kg deionized water and 0.01kg 1,6- oneself two
Amine stirs 40min, obtains polyaminoester emulsion after filtering；
(6) deionized water of 43kg is added in a reservoir, 4kg auxiliary agent is added and adds in 1500r/min high speed dispersion 10min
Enter the polyaminoester emulsion of (5) of 55kg, disperses 50min, aqueous polyurethane three-proofing coating B3 can be obtained.
Comparative example 4
(1) raw material moisture is removed: in the case of stirring, by 20kg polyadipate diglycol ester (PDA), 10kg
Dimethylolpropionic acid (DMPA) and 10kg trimethylolpropane (TMP) are heated to 100 DEG C, vacuumize 2 hours；
(2) mixed solution of (1) is cooled to 60 DEG C, 12kg dimethyl acetamide is added, the different Fo Er of 14kg is then added
Ketone diisocyanate, isothermal reaction 2 hours；
(3) mixed solution of (2) is heated up 63 DEG C, addition 0.01kg dibutyl tin dilaurate, isothermal reaction 1 hour；
(4) mixed solution of (3) is cooled to 40 DEG C, 0.15kg triethylamine, stirring is added under the revolving speed of 1600r/min
30min；
(5) revolving speed 1600r/min is kept, 55kg deionized water and 0.015kg ethylenediamine is added in the mixed solution of (4),
40min is stirred, obtains polyaminoester emulsion after filtering；
(6) deionized water of 46kg is added in a reservoir, 4kg auxiliary agent is added and adds in 1500r/min high speed dispersion 10min
Enter the polyaminoester emulsion of (5) of 56kg, disperses 50min, aqueous polyurethane three-proofing coating B4 can be obtained.
Comparative example 5
The polyurethane three-proofing coating bought in the market embodiment 5 as a comparison are selected, B5 is denoted as.
Testing example
By aqueous polyurethane three-proofing coating prepared by embodiment 1-2 and commercially available polyurethane three-proofing coating, tested as follows,
Testing standard is as shown in table 1, and test result is as shown in table 2.
1 testing standard of table
Table 2: test result
It was found from embodiment A1-A4 in upper table and comparative example B1-B4: polyester polyol that the present invention designs, aqueous
Change monomer, small molecule polyol ratio appropriate mix, obtained volume resistivity and substrate adhesive force are preferable, particularly, implement
The ratio effect of example is best.
It was found from embodiment A1-A4 in upper table and comparative example B5: aqueous polyurethane three-proofing coating prepared by the present invention
Reaching commercially available standard in performance, but there is commercially available incomparable advantage in environmental protection.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and is modified.Therefore, the invention is not limited to the specific embodiments disclosed and described above, to the one of invention
A little modifications and changes should also be as falling into the scope of the claims of the present invention.In addition, although being used in this specification
Some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.
Claims (10)
1. a kind of aqueous polyurethane three-proofing coating, which is characterized in that be made of the raw material of following parts by weight: polyaminoester emulsion 40-60
Part, 30-50 parts of deionized water, 1-5 parts of auxiliary agent；
The polyaminoester emulsion is prepared by the raw material of following parts by weight: 10-20 parts of polyester polyol, Water-borne modification monomer 1-4
Part, 1-4 parts of small molecule polyol, 10-15 parts of polyisocyanates, 10-15 parts of solvent, 0.02-0.08 parts of catalyst, neutralizer
0.005-0.03 parts, 50-60 parts of deionized water, 0.005-0.03 parts of chain extender；
The preparation method of the polyaminoester emulsion the following steps are included:
(1) in the case of stirring, polyester polyol, Water-borne modification monomer and small molecule polyol are heated to 80-90 DEG C, taken out true
It is 1-3 hours empty；
(2) mixed solution of (1) is cooled to 60-65 DEG C, solvent is added, polyisocyanates is then added, isothermal reaction 1-2 is small
When；
(3) mixed solution of (2) is heated up 63-67 DEG C, addition catalyst, isothermal reaction 0.5-1 hours；
(4) mixed solution of (3) is cooled to 40-43 DEG C, neutralizer is added under the revolving speed of 800-1600r/min, stir 20-
30min；
(5) revolving speed 1200-1600r/min is kept, water and chain extender is added in the mixed solution of (4), 40-50min is stirred, obtains
Polyaminoester emulsion.
2. three-proofing coating according to claim 1, which is characterized in that the Water-borne modification monomer be dihydromethyl propionic acid and/or
Dimethylolpropionic acid；The neutralizer is one or more of dimethylethanolamine, triethylamine, ammonium hydroxide, triethanolamine.
3. three-proofing coating according to claim 2, which is characterized in that the polyester polyol is polyethylene glycol adipate two
One or more of alcohol, polyadipate diglycol ester, poly- 6-caprolactone, polycarbonate glycol type.
4. three-proofing coating according to claim 2 or 3, which is characterized in that the small molecule polyol be diglycol,
1,4- butanediol, 1,2- propylene glycol, 2,2,4- trimethylpentanediol (TMPD), 1,6-HD, neopentyl glycol, trihydroxy methyl third
One or more of alkane.
5. three-proofing coating according to claim 2, which is characterized in that the polyisocyanates is toluene di-isocyanate(TDI)
(TDI), methyl diphenylene diisocyanate (MDI), hexamethylene diisocyanate (HDI), isophorone diisocyanate
(IPDI), one or more of dicyclohexyl methyl hydride diisocyanate (HMDI) and benzene dimethylene diisocyanate (XDI).
6. three-proofing coating according to claim 2, which is characterized in that the catalyst is dibutyl tin dilaurate, octanoic acid
One or more of stannous, dibutyltin diacetate.
7. three-proofing coating according to claim 2, which is characterized in that the chain extender is ethylenediamine, 1,6- hexamethylene diamine, Isosorbide-5-Nitrae-
One or more of cyclohexane diamine and isophorone diamine.
8. three-proofing coating according to claim 2, which is characterized in that the auxiliary agent include defoaming agent, levelling agent, thickener,
One of wetting agent is a variety of.
9. three-proofing coating according to claim 2, which is characterized in that the solvent is ketones solvent and/or amide solvent.
10. a kind of preparation method of the described in any item three-proofing coatings of claim 1-9, which is characterized in that by deionized water and help
Agent stirs 10-20min in 1000-1500r/min, and polyaminoester emulsion is then added, and continues to stir 20-50min, can be obtained
Aqueous polyurethane three-proofing coating.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113956431A (en) * | 2021-12-06 | 2022-01-21 | 南雄西顿化工有限公司 | Waterborne polyurethane for woodware with high alcohol resistance and preparation method thereof |
| CN114045101A (en) * | 2021-12-21 | 2022-02-15 | 河北慧科电子科技有限公司 | Waterborne polyurethane three-proofing paint and preparation method thereof |
| CN115651513A (en) * | 2022-09-15 | 2023-01-31 | 江苏矽时代材料科技有限公司 | Water-based three-proofing coating and preparation method and application thereof |
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| CN106188478A (en) * | 2016-07-26 | 2016-12-07 | 巨石集团有限公司 | A kind of modified polyurethane emulsion film former and its preparation method and application |
| CN107573831A (en) * | 2017-09-11 | 2018-01-12 | 亿铖达（深圳）新材料有限公司 | A kind of wiring board anti-corrosion aqueous polyurethane three-proofing coating |
| CN108102061A (en) * | 2017-11-24 | 2018-06-01 | 南雄市金鸿泰化工新材料有限公司 | A kind of synthetic method of aqueous three-proofing coating polyurethane |
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| CN106188478A (en) * | 2016-07-26 | 2016-12-07 | 巨石集团有限公司 | A kind of modified polyurethane emulsion film former and its preparation method and application |
| CN107573831A (en) * | 2017-09-11 | 2018-01-12 | 亿铖达（深圳）新材料有限公司 | A kind of wiring board anti-corrosion aqueous polyurethane three-proofing coating |
| CN108102061A (en) * | 2017-11-24 | 2018-06-01 | 南雄市金鸿泰化工新材料有限公司 | A kind of synthetic method of aqueous three-proofing coating polyurethane |
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| CN113956431A (en) * | 2021-12-06 | 2022-01-21 | 南雄西顿化工有限公司 | Waterborne polyurethane for woodware with high alcohol resistance and preparation method thereof |
| CN114045101A (en) * | 2021-12-21 | 2022-02-15 | 河北慧科电子科技有限公司 | Waterborne polyurethane three-proofing paint and preparation method thereof |
| CN115651513A (en) * | 2022-09-15 | 2023-01-31 | 江苏矽时代材料科技有限公司 | Water-based three-proofing coating and preparation method and application thereof |
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