CN104987821B - A kind of environment-friendly water-based inner wall polyurethane emulsion paint and preparation method thereof - Google Patents
A kind of environment-friendly water-based inner wall polyurethane emulsion paint and preparation method thereof Download PDFInfo
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- CN104987821B CN104987821B CN201510451144.3A CN201510451144A CN104987821B CN 104987821 B CN104987821 B CN 104987821B CN 201510451144 A CN201510451144 A CN 201510451144A CN 104987821 B CN104987821 B CN 104987821B
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- 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
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- C09D175/06—Polyurethanes from polyesters
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- 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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- C08G18/30—Low-molecular-weight compounds
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- C08G18/40—High-molecular-weight compounds
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- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
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- C08G18/40—High-molecular-weight compounds
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- C08G18/40—High-molecular-weight compounds
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- 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
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- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
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- 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
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- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6648—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6651—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
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- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
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- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- 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
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- 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
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
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- 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
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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Abstract
The present invention relates to a kind of environment-friendly water-based inner wall polyurethane emulsion paint, using aqueous polyurethane dispersion, water, pigment and filler as primary raw material, the auxiliary agent processing such as addition wetting agent, dispersant, thickener, defoamer, preservative, pH adjusting agent is prepared from.The invention also discloses the preparation method of environment-friendly water-based inner wall polyurethane emulsion paint.The characteristics of aqueous polyurethane interiro wall latex paint prepared using the present invention has ultralow absolute VOC content, odorlessness, environmental protection, excellent scrub performance, good hand touch, good decoration performance.
Description
Technical field
The present invention relates to building coating field, a kind of aqueous polyurethane interiro wall latex paint is more particularly related to.
Background technology
In China, interiro wall latex paint experienced development for many years, more and more be applied to interior wall building decoration dress
In repairing.But some interiro wall latex paints can discharge such as formaldehyde and benezene material in production, construction and application process to be harmful to
Material, easily induces breathing problem and leukaemia, therefore people focus more on the green environmental protection of interiro wall latex paint in recent years
Can be such as VOC content.
VOC is volatile organic compound, and country variant and area have differences for VOC definition, such as China's rule
It is that nonpolar chromatographic column (polarity index is less than 10) is analyzed, during reservation using Tenax GC and Tenax TA samplings to determine VOC
Between VOC between n-hexane and hexadecane；DIN is then defined under normal pressure, boiling point or initial boiling point
Any organic compound less than or equal to 250 DEG C is VOC.That above standard is defined is relative VOC, and definitely VOC is also wrapped
Include the volatile organic compound that boiling point is higher than 250 DEG C.Such as commonly use coalescents OE-300 alcohol esters (Yi Shiman) boiling point be
281 DEG C, it is not belonging to relative VOC, but belongs to absolute VOC.
The Diamond Search that in the market is sold/net taste Aqueous acrylic latex's paint, its emulsion is typically larger than with respect to VOC content
1000ppm, absolute VOC content is then higher, is difficult to thoroughly clearly because aqueous acrylic emulsion is introduced in radical polymerization process
The small molecular organic compounds removed, including unreacted monomer, introduced by monomer organic impurities, by surfactant or initiator
Decompose the organic matter produced.And because of aqueous acrylic emulsion own structural characteristics, need to balance coalescents in latex paint formulation
With the selection of antifreeze auxiliary agent, it is not added with coalescents and then haves the shortcomings that paint film is tacky, contaminated resistance is poor, and add coalescents
The absolute VOC content of emulsion paint is more than 10000ppm afterwards.
CN1414045A discloses a kind of environmentally friendly acrylic emulsion paint of Diamond Search, and film formation at low temp is good, with respect to VOC content
It is relatively low, but its feel is tacky, and freeze-thaw stability is poor.CN101343451A discloses a kind of healthy interiro wall latex paint of Diamond Search, but
It is to introduce coalescents during it is formulated, therefore, it is difficult to reach ultralow absolute VOC content.Therefore, a kind of absolute VOC content is developed
Close to zero, odorlessness, the aqueous polyurethane interiro wall latex paint of health environment-friendly, the environment-protective water of whole industry will certainly will be further lifted
It is flat.
The content of the invention
It is an object of the invention to provide a kind of environment-friendly water-based inner wall polyurethane emulsion paint, the film forming matter of use is aqueous poly-
Urethane dispersion is prepared by condensation polymerization.Need not add coalescents can in 5 DEG C of film forming, and coating surface it is smooth,
Spot-resistant performance and contaminated resistance are excellent, and the absolute VOC content of inner wall polyurethane emulsion paint that the present invention is provided is extremely low, with nothing
Smell, health environment-friendly, scrub performance are excellent, soft handle, the advantage for decorating excellent performance.
The present invention also provides a kind of production method of the environment-friendly water-based inner wall polyurethane emulsion paint.
To realize above technical purpose, the present invention is adopted the following technical scheme that：
A kind of environment-friendly water-based inner wall polyurethane emulsion paint, it includes：Based on the total restatement of emulsion paint,
It is preferred that, emulsion paint of the present invention, including：Based on the total restatement of emulsion paint,
Polyurethane in aqueous polyurethane dispersion of the present invention is the product prepared comprising following components：
(a1) 10wt%-35wt%, preferably 15wt%-35wt% polyisocynate monomer,
(a2) 50wt%-85wt%, preferably 60wt%-80wt% polyalcohol,
(a3) 0.1wt%-8wt%, preferably 0.1wt%-6wt% chain extender,
(a4) 0.1wt%-5wt%, preferably 0.1wt%-3wt% non-ionic hydrophilic monomer,
(a5) 0.1wt%-5wt%, preferably 0.5wt%-3wt% ionic hydrophilic monomer；Each component content is based on
The weight of the polyurethane of (a) aqueous polyurethane dispersion is calculated.
The nonvolatile matter composition of aqueous polyurethane dispersion of the present invention is that the content of polyurethane is 30wt%-
70wt%, remaining composition is water.
Polyisocynate monomer of the present invention is in aromatic series, araliphatic, aliphatic and alicyclic polyisocyanates
One or two or more；The example of suitable polyisocynate monomer has 1,6- hexamethylene diisocyanates (HDI), different
Isophorone diisocyanate (IPDI), toluene di-isocyanate(TDI) (TDI), double-(4,4 '-isocyanatocyclohexyl) methane
(HMDI), 4,4 '-methyl diphenylene diisocyanate (MDI).
The one kind or two of polyalcohol of the present invention in PPG, PEPA and polycarbonate polyol
Plant or a variety of.The polyalcohol has more than 2 degrees of functionality, and molecular weight is 500-5000.
It is preferred that, polyalcohol of the present invention is in polyester diol, polyether Glycols and PCDL
It is one or two or more kinds of.
One or both of the preferred polyethylene glycol of polyether Glycols, polypropylene glycol and PTMG or
It is a variety of.
The polyester diol is made with diol reaction or prepared by lactone, institute by dicarboxylic acids or dicarboxylic acid anhydride
State lactone and be preferably but not limited to caprolactone.
It is preferred that, the polyester diol is based on adipic acid, phthalic acid, M-phthalic acid and terephthalic acid (TPA) and neighbour
One or both of phthalate anhydride or a variety of and ethylene glycol, 1,4- butanediols, 1,3 butylene glycol, 1,6-HD and new penta
One or both of glycol or a variety of preparations.
It is furthermore preferred that polyalcohol of the present invention is the polyester prepared based on adipic acid, 1,6- hexylene glycols and neopentyl glycol
The mixture of dihydric alcohol (PNHA) and PTMG, wherein described be based on adipic acid, 1,6- hexylene glycols and new penta 2
The number-average molecular weight 500-3000 of polyester diol prepared by alcohol, preferably 1000-2000, the number of PTMG is divided equally
Son amount is 500-3000, preferably 1000-2000；The polyester two prepared based on adipic acid, 1,6-HD and neopentyl glycol
The mass ratio of first alcohol and PTMG is 9:1-1:1, preferably 9:1-7:3.
It is further preferred that new in the polyester diol prepared based on adipic acid, 1,6- hexylene glycols and neopentyl glycol
Pentanediol consumption is 1,6- hexylene glycols and the 5wt%~100wt%, preferably 10wt%~80wt% of neopentyl glycol gross mass.
PEPA of the present invention can effectively improve paint film strength, and provide good feel, be based on simultaneously
Asymmetrical neopentyl glycol is introduced in the polyester diol of adipic acid, 1,6- hexylene glycols and neopentyl glycol, structure, effectively reduction is poly-
The interaction of soft segment structure itself, lifts itself and pigment, the combination of filler in the symmetry of ester structure, reduction polyurethane.Together
When, PTMG cohesive force is small, and hydrolysis resistance is strong, effectively the durability of lifting paint film.PTMG two
Alcohol and the special ratios of polyester diol are used in mixed way, and can further reduce the interaction between polyalcohol, enhancing polyurethane with
The combination of pigment, filler, effectively the lifting durability of emulsion paint, cracking resistance effect and and scrub performance, ensureing emulsion paint
While environmental-protecting performance, the overall applicability performance of emulsion paint is lifted.
The one kind or two of chain extender of the present invention in low molecular polylol, low molecule polyamine and low molecule hydramine
Plant or a variety of；The example of suitable chain extender has 1,3- propane diols, 1,4- butanediols (BDO), neopentyl glycol, a contracting diethyl two
Alcohol, 1,6-HD, 1,4 cyclohexane dimethanol, ethylenediamine, hexamethylene diamine, five methylene diamine, diethylenetriamines,
IPD, 4,4 '-diphenylmethanediamiand, MEA, diethanol amine.
It is preferred that, chain extender of the present invention is selected from least one low molecular polylol and at least one low molecule polyamine.
Non-ionic hydrophilic monomer of the present invention, there is the degree of functionality of isocyanate-reactive group to be 1 or 2, institute for it
State and be selected from hydroxyl, amino etc. with isocyanate-reactive group.
It is preferred that, non-ionic hydrophilic monomer of the present invention is selected from simple function polyalkylene oxide and/or contains polyalkylene oxide
The bifunctionality molecule of side chain.
The preferred main chain carbon number of bifunctionality molecule containing polyalkylene oxide sidechain of the present invention is 2-20, and side chain contains
PEO ether or the molecule containing oxirane segment, the number of the bifunctionality molecule of the polyalkylene oxide sidechain are divided equally
Son amount is 200-2000, and preferred number average molecular weight is 500-1500.
Simple function polyalkylene oxide preferred number average molecular weight of the present invention is 200-3000 terminal hydroxy group PEO list
Methyl ether and/or Amino End Group PEO monomethyl ether.
Ionic hydrophilic monomer of the present invention is one in dihydric alcohol, diamine and hydramine containing hydrophilic stability group
Plant or two or more, the hydrophilic stability group is selected from carboxyl, sulfonic group, phosphate groups, tertiary amine group or quaternary ammonium group
Group.
It is preferred that, ionic hydrophilic monomer of the present invention be selected from dihydromethyl propionic acid (DMPA), 1,3- dihydroxy butane-
1- carboxylic acids, 1,2- dihydroxy butane -1- sulfonic acid, 1,3- dihydroxy butyl-trimethylammonium chloride andOne or both of or it is a variety of, wherein m, n is separate for 1-
20 natural number；More preferablyWherein m, n are separate for 1-6's
Natural number；The sodium salt and/or N- (2- amino-ethyls) -2- aminopropans of further preferred N- (2 amino-ethyl)-Tau
The sodium salt of sulfonic acid.
The preparation technology of the aqueous polyurethane dispersion comprises the following steps：Proportionally, by polyalcohol, polyisocyanic acid
Ester monomer, low molecular polylol chain extender and non-ionic hydrophilic monomer are reacted at 60~100 DEG C in acetone, during supervise
The isocyanate radical content of reaction system is controlled, to judge reaction end；Reduction reaction temperature adds acetone to 30~50 DEG C afterwards
Reacted with low molecule polyamine chain extender and ionic hydrophilic monomer to terminating.After the completion of reaction, in rapid mixing conditions
Lower that water is gradually added into system, phase reversal forms dispersion, disperseed, and removes acetone, forms particle diameter in 50~1000nm
Aqueous polyurethane dispersion.
Need to use acetone as solvent in aqueous polyurethane dispersion building-up process, obtained in the last removing acetone of production
Obtain aqueous polyurethane dispersion.For traditional product, acetone residue amount therein is in thousands of ppm or higher content.For
VOC content effectively in control emulsion paint, it is desirable to content of acetone≤200ppm in aqueous polyurethane dispersion.
Pigment of the present invention is titanium dioxide.
One kind in talcum powder, coarse whiting, fine particle calcium carbonate, mica powder, diatomite and kaolin of filler of the present invention or
Two or more.
Emulsion paint of the present invention can also contain 0-10wt%, preferably 1-8wt% opacity polymer；Described cover is gathered
Compound preferably is selected from particle diameter 200-600nm polystyrene hollow microballoons, the Unihub E hollow polymer microspheres of more preferably DOW chemistry.
Auxiliary agent of the present invention, including following component：Based on the total restatement of emulsion paint, dispersant 0.1wt%-3wt%, profit
Humectant 0.1wt%-0.5%, thickener 0.1wt%-2.0wt%, preservative 0-0.5wt%, defoamer 0.1wt%-
1.5wt%, pH adjusting agent 0-0.5wt%.
Dispersant of the present invention be selected from one or both of polyacrylamide, equal polycarboxylate, co-poly carboxylic acid salt or
A variety of, preferably acrylic acid and other monomer copolymers, sodium salt, the sylvite of maleic anhydride and other monomer copolymers can assign painting
The more preferable patience of layer and environmental protection characteristic.Example including but not limited to：The Orotan of Nuo Puke SN5040, SN5027, DOW chemistry
1124th, Orotan fast easily, Orotan 731A, Vesmody C20, BYK the company DISPERBYK-182 of ten thousand China's chemistry etc..
Wetting agent of the present invention can be that polyphosphate or nonionic surfactant are one or two kinds of or many
Kind.The preferred hydrophobic side carbon number of nonionic surfactant in 8-20, water-wet side be PEO or oxirane with
The copolymer of expoxy propane.Example including but not limited to：Calgon, Triton CF10, the Triton CF- of DOW chemistry
405、Triton BD-109；Ke Laien LCN407, Nuo Pu sections SN-WET990, SN-WET991, wetting agent PE100 etc..
Thickener of the present invention is in cellulose ethers thickener, alkali swelling type thickener and polyurethane-type thickener
One or two or more.The alkali soluble type thickener that rises can select simple alkali soluble to rise type thickener or hydrophobically modified
Alkali soluble rises type thickener, and the cellulose ethers thickener can select the product of different molecular weight size or hydrophobically modified.
Example including but not limited to：Cellulose ethers thickener is as pressed the HEC classes across hydroxyethyl cellulose 250HBR, the DOW chemistry of dragon
Cellulose ethers thickener；The non-swelling thickener of alkali is such as DOW chemistry
Ten thousand China's chemistryDeng；Polyurethane-type thickener is such as ten thousand China's chemistryDOW chemistry Deng.
Heretofore described preservative is not specifically limited, as long as the goal of the invention to the present invention does not produce limitation,
Example is including but not limited to 1,2- benzisothiazole-3-ketones, methylisothiazolinone, 5- chloro-2-methyl -4- isothiazolines -3-
Ketone, KATHON LXE of ROHM AND HAAS etc..
Defoamer of the present invention is selected from mineral oil defoaming agent, organic silicon defoamer and organic silicon modified by polyether froth breaking
One or both of agent etc. is a variety of, preferably is selected from polysiloxane-polyether copolymer type of latex type, polypropylene glycol-hydrophobic solid-poly-
Mixture of siloxanes class, polyethylene glycol-hydrophobic solid-one or both of polysiloxane mixture class and mineral oil base class or
It is a variety of.Example including but not limited to：Nuo Puke NXZ, the high Tego1488 of enlightening, 825, BYK BYK-028, the DC-65 of DOW CORNING
Deng.
PH adjusting agent of the present invention is preferably sodium hydroxide and/or potassium hydroxide.
The present invention also provides a kind of preparation method of environment-friendly water-based inner wall polyurethane emulsion paint, comprises the steps of：
(1) preparation of slurry
Water, dispersant, wetting agent, thickener, preservative, defoamer, pH adjusting agent, pigment, filler, screening are weighed in proportion
Lid polymer, stirs, and slurry is made standby；
(2) preparation of emulsion paint
Slurry, aqueous polyurethane dispersion, thickener, defoamer made from step (1) are weighed in proportion, after stirring
Discharging obtains environment-friendly water-based inner wall polyurethane emulsion paint.
Emulsion paint of the present invention is not required to addition coalescents can be in 5 DEG C and temperatures above good filming, and paint film is dry and comfortable
Do not glue, soft handle, and scrub performance is excellent, spot-resistant performance and contaminated resistance are excellent, and low-temperature stability is good, definitely
Organic volatile gas (including boiling point is less than, the small molecule organic volatile equal to 250 DEG C and higher than 250 DEG C) content is less than
500ppm, preferably shorter than 300ppm, odorlessness belong to Green Product decoration excellent performance, easy construction.
Embodiment
The following is embodiments of the invention, but it is not limited to the embodiment.
(1) synthesis of aqueous polyurethane dispersion
Embodiment 1
In the case where drying N2 protection, to equipped with addition in reflux condensing tube, thermometer and churned mechanically four-hole boiling flask
400g PEPAs PNHA1500 (Hua Da chemistry, Mn=1500, neopentyl glycol：1,6-HD mass ratio=1:2),
16.06g neopentyl glycols, 8.8g YmerTMN120 (non-ionic hydrophilic monomer), stirs 30min under the conditions of 60 DEG C, adds 86gAnd 56gReacted under the conditions of 80 DEG C of 56g acetone.When NCO content reaches
During to theoretical value 3.12wt%, prepolymer is cooled to 40 DEG C, is dissolved in 800g acetone, mixing adds 9.6g second after 10 minutes
Diamines, 14gA95 (sulfamic acid sodium salt, the 50wt% aqueous solution), continues to stir after 30min, in shearing point
Addition 575g deionized waters under machine are dissipated to be disperseed；By above emulsion, vacuum rotary steam removes acetone in 1 hour at 50 DEG C, can obtain
Milky 1# aqueous polyurethane dispersion emulsion；The emulsion particle diameter 280nm, solid content 50wt%.
Embodiment 2
Drying N2Protection under, to equipped with reflux condensing tube, thermometer and churned mechanically four-hole boiling flask add
357g PEPAs PNHA2000 (Hua Da chemistry, Mn=2000, neopentyl glycol：1,6-HD mass ratio=1:2), 45g
PTMEG2000,14g1,4- butanediol, 6g YmerTMN120 (non-ionic hydrophilic monomer), 30min is stirred under the conditions of 60 DEG C,
Add 72gAnd 46gReacted under the conditions of 80 DEG C of 49g acetone.When
When NCO content reaches theoretical value 2.65wt%, prepolymer is cooled to 40 DEG C, is dissolved in 692g acetone, after mixing 10 minutes
Add 6g ethylenediamines, 14g(sulfamic acid sodium salt, the 50wt% aqueous solution), continues to stir 30min
Afterwards, 501g deionized waters are added under shearing dispersion machine to be disperseed；By above emulsion, vacuum rotary steam is removed for 1 hour at 50 DEG C
Acetone, can obtain milky 2# aqueous polyurethane dispersion emulsion；The emulsion particle diameter 332nm, solid content 50wt%.
Embodiment 3
Drying N2Protection under, to equipped with reflux condensing tube, thermometer and churned mechanically four-hole boiling flask add
397g PCDLs NPU-964 (Mn=2000), 98g PTMEG2000,8g neopentyl glycol, 6g YmerTMN120 is (non-
Ionic hydrophilic monomer), 30min is stirred under the conditions of 60 DEG C, 68.3g is addedAnd 43.8gReacted under the conditions of 80 DEG C of 52g acetone.When NCO content reaches theoretical value 2.38wt%, by pre-polymerization
Thing is cooled to 40 DEG C, is dissolved in 732g acetone, and mixing adds the different Buddhist diketone diamines of 17.5g, 16g after 10 minutes(sulfamic acid sodium salt, the 50wt% aqueous solution), continues to stir after 30min, under shearing dispersion machine
541g deionized waters are added to be disperseed；By above emulsion, vacuum rotary steam removes acetone in 1 hour at 50 DEG C, can obtain milky
3# aqueous polyurethane dispersion emulsions；The emulsion particle diameter 307nm, solid content 50wt%.
Embodiment 4
Drying N2Protection under, to equipped with reflux condensing tube, thermometer and churned mechanically four-hole boiling flask add
280g PEPAs PNHA1500 (Hua Da chemistry, Mn=1500, neopentyl glycol：1,6-HD mass ratio=1:2), 120g
PTMEG2000,30g1,6- hexylene glycol, 11g YmerTMN120 (non-ionic hydrophilic monomer), is stirred under the conditions of 60 DEG C
30min, adds 107.6gAnd 69.2g80 DEG C of conditions of 50g acetone
Lower reaction.When NCO content reaches theoretical value 3.91wt%, prepolymer is cooled to 40 DEG C, is dissolved in 697g acetone, mixed
12g ethylenediamines, 13.5g are added after 10 minutes(sulfamic acid sodium salt), continues to stir after 30min,
510g deionized waters are added under shearing dispersion machine to be disperseed；By above emulsion, vacuum rotary steam removes third in 1 hour at 50 DEG C
Ketone, can obtain milky 4# aqueous polyurethane dispersion emulsion；The emulsion particle diameter 250nm, solid content 50wt%.
Embodiment 5
In the case where drying N2 protection, to equipped with addition in reflux condensing tube, thermometer and churned mechanically four-hole boiling flask
400g PEPAs PNHA1500 (Hua Da chemistry, Mn=1500, neopentyl glycol：1,6-HD mass ratio=1:2),
16.6g neopentyl glycols, 6gMPEG1200 stirs 30min under the conditions of 60 DEG C, adds 86gWith
56gReacted under the conditions of 80 DEG C of 6g acetone., will be pre- when NCO content reaches theoretical value 3.15wt%
Polymers is cooled to 40 DEG C, is dissolved in 790g acetone, and mixing adds 8.3g ethylenediamines, 14g after 10 minutes(sulfamic acid sodium salt, the 50wt% aqueous solution), continues to stir after 30min, under shearing dispersion machine
573g deionized waters are added to be disperseed；By above emulsion, vacuum rotary steam removes acetone in 1 hour at 50 DEG C, can obtain milky
5# aqueous polyurethane dispersion emulsions；The emulsion particle diameter 230nm, solid content 50wt%.
Embodiment 6
Drying N2Protection under, to equipped with reflux condensing tube, thermometer and churned mechanically four-hole boiling flask add
413g PEPAs PNHA2000 (Hua Da chemistry, Mn=2000, neopentyl glycol：1,6-HD mass ratio=1:2), 15g
Neopentyl glycol, 3gMPEG1200 stirs 30min under the conditions of 60 DEG C, adds 70.3gWith
45.2gReacted under the conditions of 80 DEG C of 54g acetone.When-NCO content reaches theoretical value 2.59wt%,
Prepolymer is cooled to 40 DEG C, is dissolved in 765g acetone, mixing adds 5.6g ethylenediamines, 17g after 10 minutes(sulfamic acid sodium salt, the 50wt% aqueous solution), continues to stir after 30min, under shearing dispersion machine
552g deionized waters are added to be disperseed；By above emulsion, vacuum rotary steam removes acetone in 1 hour at 50 DEG C, it can obtain milky white
The 6# aqueous polyurethane resin dispersion emulsions of color；The emulsion particle diameter 260nm, solid content 50wt%.
Embodiment 7
Drying N2Protection under, to equipped with reflux condensing tube, thermometer and churned mechanically four-hole boiling flask add
280g PEPAs PNHA1500 (Mn=1500, neopentyl glycol：1,6-HD mass ratio=1:9), 120g
PTMEG2000,30g1,6- hexylene glycol, 11g YmerTMN120 (non-ionic hydrophilic monomer), is stirred under the conditions of 60 DEG C
30min, adds 107.6gAnd 69.2g80 DEG C of conditions of 50g acetone
Lower reaction.When NCO content reaches theoretical value 3.91wt%, prepolymer is cooled to 40 DEG C, is dissolved in 697g acetone, mixed
12g ethylenediamines, 13.5g are added after 10 minutes(sulfamic acid sodium salt), continues to stir after 30min,
510g deionized waters are added under shearing dispersion machine to be disperseed；By above emulsion, vacuum rotary steam removes third in 1 hour at 50 DEG C
Ketone, can obtain milky 7# aqueous polyurethane dispersion emulsion；The emulsion particle diameter 280nm, solid content 50wt%.
Embodiment 8
Drying N2Protection under, to equipped with reflux condensing tube, thermometer and churned mechanically four-hole boiling flask add
280g PEPAs PNHA1500 (Mn=1500, neopentyl glycol：1,6-HD mass ratio=4:1), 120g
PTMEG2000,30g1,6- hexylene glycol, 11g YmerTMN120 (non-ionic hydrophilic monomer), is stirred under the conditions of 60 DEG C
30min, adds 107.6gAnd 69.2g80 DEG C of conditions of 50g acetone
Lower reaction.When NCO content reaches theoretical value 3.91wt%, prepolymer is cooled to 40 DEG C, is dissolved in 697g acetone, mixed
12g ethylenediamines, 13.5g are added after 10 minutes(sulfamic acid sodium salt), continues to stir after 30min,
510g deionized waters are added under shearing dispersion machine to be disperseed；By above emulsion, vacuum rotary steam removes third in 1 hour at 50 DEG C
Ketone, can obtain milky 8# aqueous polyurethane dispersion emulsion；The emulsion particle diameter 230nm, solid content 50wt%.
(2) preparation of environment-friendly water-based inner wall polyurethane emulsion paint
Embodiment 9
138.8g water is added in the straight body bottles of 1000ml, stirring 800rpm is opened, sequentially adds the thickening of 1g cellulose etherses
Agent 250HBR, 2g the pH adjusting agent 10wt%NaOH aqueous solution, 1g wetting agents BD-109,10g dispersant 731A, 3g defoamer
NXZ, 1g preservative LXE, 220g titanium dioxide R-902+, 60g1000 mesh talcum powder, 120g800 mesh coarse whitings, 40g opacity polymers
Unihub E, improves mixing speed and disperses 30 minutes to 1500rpm, mixing speed is down into 800rpm, 1g defoamers are sequentially added
NXZ, 400g1# aqueous polyurethane dispersion, 4g thickener A401, stirring discharge after 20 minutes, and the pigment volume concentration of the emulsion paint is dense
It is 45% to spend (PVC).
Embodiment 10-16
Described environment-friendly water-based inner wall polyurethane emulsion paint from embodiment 1 preparation difference is that PVC is different, water, pigment,
Filler, opacity polymer are different with aqueous polyurethane dispersion and auxiliary dosage, and embodiment 10~16 is aqueous using 2~8# successively
Dispersions of polyurethanes, other process conditions are consistent with embodiment 9, and specific formula is shown in Tables 1 and 2.
Comparative example 1
As different from Example 9 its film forming matter be net taste aqueous acrylic emulsion (glass transition temperature is 15 DEG C, admittedly contain
Measure as 45%), and need to add coalescents in emulsion paint preparation process, specific preparation process is as follows：In the straight body bottles of 1000ml
113g water is added, stirring 800rpm is opened, sequentially adds 2g cellulose ethers thickener 250HBR, 2g pH adjusting agents 10wt%
The NaOH aqueous solution, 2g wetting agents BD-109,10g dispersant 731A, 2g defoamer NXZ, 1g preservative LXE, 220g titanium dioxide R-
902+, 60g1000 mesh talcum powder, 120g800 mesh coarse whitings, 40g opacity polymer Unihub E, raising mixing speed is to 1500rpm points
Dissipate 30 minutes, mixing speed is down to 800rpm, 1g defoamers NXZ, 400g aqueous acrylic emulsion, 10g film forming is sequentially added
Auxiliary agent Texanol, 4g thickener A401, stirring discharges after 20 minutes, and the pigment volume concentration (PVC) (PVC) of the emulsion paint is 45%.
Comparative example 2
Its film forming matter is that (glass transition temperature is -22 DEG C, solid content to aqueous acrylic emulsion as different from Example 9
For 52%), specific preparation process is as follows：163g water is added in the straight body bottles of 1000ml, stirring 800rpm is opened, sequentially adds 2g
Cellulose ethers thickener 250HBR, 2gpH the conditioning agent 10%NaOH aqueous solution, 2g wetting agents BD-109,10g dispersant 731A,
2g defoamers NXZ, 1g preservative LXE, 220g titanium dioxide R-902+, 60g1000 mesh talcum powder, 120g800 mesh coarse whitings, 40g screenings
Lid polymer Unihub E, improves mixing speed and disperses 30 minutes to 1500rpm, mixing speed is down into 800rpm, 1g is sequentially added
Defoamer NXZ, 350g aqueous acrylic emulsion, 4g thickener A401, stirring discharges after 20 minutes, the pigment volume concentration of the emulsion paint
Concentration (PVC) is 45%.
Table 1：The PVC and specific formula of embodiment 9-16 aqueous polyurethane emulsion paints
Table 2：Auxiliary agent addition is detailed
Performance test
The performance parameter of embodiment 9-16 and comparative example 1-2 environment-friendly water-based interiro wall latex paint is shown in Table 2.
Table 2：Embodiment 9-16 and the contrast of comparative example 1-2 performance parameters
From the above it can be seen that, its absolute VOC of the aqueous polyurethane interiro wall latex paint of the various PVC in embodiment contains
Emulsion paint of the amount far below comparative example general in the market；There is no obvious smell, be much better than comparative example esters of acrylic acid
Emulsion paint；Its contaminated resistance is also significantly better than comparative example.In terms of scrubbing resistance, scrub performance of middle low PVC embodiment etc.
In comparative example, only in the high PVC system of seldom aqueous polyurethane addition (low-grade emulsion paint), scrubbing resistance level is just less than
Comparative example.Its spot-resistant performance is also substantially approximate with comparative example, is maintained at a relatively good level.
Note：Absolute VOC content presses GB18582-2008《Harmful substance is limited in indoor decorating and refurnishing materials-interiro wall latex paint
Amount》Method is tested.
Scrub performance presses GB/T9756-2009《Synthetic resin emulsion interiro wall latex paint》Test.
Spot-resistant performance presses HG/T4756-2014《Interior wall spot-resistant latex emulsion paint》Test.
Contaminated resistance presses GB/T 9780-2013《Test method for dirt resistance of film of architectural coatings and paint》Test.
Elongation at break presses GB/T528-2009《Vulcanize the measure of rubber or thermoplastic elastomer tensile stress-strain performance》
Test.
Claims (18)
1. a kind of environment-friendly water-based inner wall polyurethane emulsion paint, it includes：Based on the total restatement of emulsion paint,
Polyurethane in described aqueous polyurethane dispersion is the product prepared comprising following components：
(a1) 10wt%-35wt% polyisocynate monomer；
(a2) 50wt%-85wt% polyalcohol, the polyalcohol is to be prepared based on adipic acid, 1,6- hexylene glycols and neopentyl glycol
Polyester diol and PTMG mixture；It is described to be based on adipic acid, 1,6-HD and neopentyl glycol system
Standby polyester diol and the mass ratio of PTMG are 9:1-1:1；
(a3) 0.1wt%-8wt% chain extender；
(a4) 0.1wt%-5wt% non-ionic hydrophilic monomer；
(a5) 0.1wt%-5wt% ionic hydrophilic monomer；
(a1)~(a5) each component content is based on the weight calculating of the polyurethane of described (a) aqueous polyurethane dispersion.
2. emulsion paint according to claim 1, it is characterised in that it includes：Based on the total restatement of emulsion paint,
3. emulsion paint according to claim 1, it is characterised in that the polyurethane in described aqueous polyurethane dispersion is
The product prepared comprising following components：
(a1) 15wt%-35wt% polyisocynate monomer；
(a2) 60wt%-80wt% polyalcohol；
(a3) 0.1wt%-6wt% chain extender；
(a4) 0.1wt%-3wt% non-ionic hydrophilic monomer；
(a5) 0.5wt%-3wt% ionic hydrophilic monomer；
(a1)~(a5) each component content is based on the weight calculating of the polyurethane of described (a) aqueous polyurethane dispersion.
4. emulsion paint according to claim 1, it is characterised in that described to be based on adipic acid, 1,6- hexylene glycols and new penta 2
The number-average molecular weight of polyester diol prepared by alcohol is 500-3000；The number-average molecular weight of the PTMG is
500-3000。
5. emulsion paint according to claim 4, it is characterised in that described to be based on adipic acid, 1,6- hexylene glycols and new penta 2
The number-average molecular weight of polyester diol prepared by alcohol is 1000-2000；The number-average molecular weight of the PTMG is
1000-2000；The polyester diol prepared based on adipic acid, 1,6-HD and neopentyl glycol and PTMG two
The mass ratio of alcohol is 9:1-7:3.
6. emulsion paint according to claim 1, it is characterised in that described to be based on adipic acid, 1,6- hexylene glycols and new penta 2
Neopentyl glycol consumption is 1,6-HD and 5wt%~100wt% of neopentyl glycol gross mass in polyester diol prepared by alcohol.
7. emulsion paint according to claim 6, it is characterised in that described to be based on adipic acid, 1,6- hexylene glycols and new penta 2
In polyester diol prepared by alcohol neopentyl glycol consumption be 1,6-HD and neopentyl glycol gross mass 10wt%~
80wt%.
8. emulsion paint according to claim 1, it is characterised in that the non-ionic hydrophilic monomer is selected from simple function polycyclic
Oxygen alkane and/or the bifunctionality compound containing polyalkylene oxide sidechain.
9. emulsion paint according to claim 8, it is characterised in that the bifunctionality chemical combination containing polyalkylene oxide sidechain
The main chain carbon number of thing is 2-20, and side chain contains ethylene oxide unit, the bifunctionality compound containing polyalkylene oxide sidechain
Number-average molecular weight is 200-2000；The simple function polyalkylene oxide is the terminal hydroxy group polycyclic oxygen second that number-average molecular weight is 200-3000
Alkane monomethyl ether and/or Amino End Group PEO monomethyl ether.
10. emulsion paint according to claim 9, it is characterised in that the bifunctionality containing polyalkylene oxide sidechain
The number-average molecular weight of compound is 500-1500.
11. emulsion paint according to claim 1, it is characterised in that the ionic hydrophilic monomer is to contain hydrophilic stability
One or more in dihydric alcohol, diamine and the hydramine of group, the hydrophilic stability group is selected from carboxyl, sulfonic group, phosphorus
Sulfonate groups, tertiary amine group or quaternary ammonium group.
12. emulsion paint according to claim 11, it is characterised in that described ionic hydrophilic monomer is selected from dihydroxymethyl
Propionic acid, 1,3- dihydroxy butane -1- carboxylic acids, 1,2- dihydroxy butane -1- sulfonic acid, 1,3- dihydroxy butyl-trimethyl ammonium chlorination
Thing andIn one or more, wherein m, n is separate for 1-20's
Natural number.
13. emulsion paint according to claim 12, it is characterised in that described ionic hydrophilic monomer is selected fromThe separate natural number for 1-6 of wherein m, n.
14. emulsion paint according to claim 13, it is characterised in that described ionic hydrophilic monomer is selected from N- (2 amino
Ethyl)-Tau sodium salt and/or the sodium salt of N- (2- amino-ethyls) -2- aminopropanesulfonic acids.
15. emulsion paint according to claim 1, it is characterised in that the pigment is titanium dioxide；The filler, which is selected from, to be slided
One or more in stone flour, coarse whiting, fine particle calcium carbonate, mica powder, diatomite and kaolin.
16. emulsion paint according to claim 1, it is characterised in that the auxiliary agent includes following component：It is total based on emulsion paint
Restatement, dispersant 0.1wt%-3wt%, wetting agent 0.1wt%-0.5wt%, thickener 0.1wt%-2.0wt%, preservative 0-
0.5wt%, defoamer 0.1wt%-1.5wt%, pH adjusting agent 0-0.5wt%.
17. emulsion paint according to claim 1, it is characterised in that the emulsion paint contains 0-10wt% covering polymerization
Thing；The opacity polymer is selected from polystyrene hollow microballoon.
18. emulsion paint according to claim 17, it is characterised in that the emulsion paint contains 1-8wt% covering polymerization
Thing.
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| CN105601197B (en) * | 2015-12-21 | 2017-10-13 | 潍坊市宏源防水材料有限公司 | A kind of two component polyurethane emulsion waterproofing paint and its production technology |
| CN105885668A (en) * | 2016-06-08 | 2016-08-24 | 胡军 | Zero-VOC waterborne soft-feel coating and preparation method thereof |
| CN105969158A (en) * | 2016-07-13 | 2016-09-28 | 李水金 | Low-cost environment-friendly internal wall paint |
| CN106280950A (en) * | 2016-08-17 | 2017-01-04 | 柳州市亿廷贸易有限责任公司 | Waterborne wall surface paint preparation method |
| CN107216786A (en) * | 2017-05-12 | 2017-09-29 | 巢湖市荷花渔网有限公司 | A kind of natural antifouling paint of fishing net |
| CN109721717B (en) * | 2017-10-31 | 2021-12-10 | 万华化学（广东）有限公司 | Waterborne epoxy modified saturated polyester resin and preparation method and application thereof |
| CN108822711A (en) * | 2018-06-26 | 2018-11-16 | 深圳市天之科技开发有限公司 | A kind of waterborne wall surface paint and preparation method thereof |
| CN109897523A (en) * | 2019-02-20 | 2019-06-18 | 张建初 | A kind of preparation method of environmental protection scratch-resistant hand-feeling coating |
| CN111500172A (en) * | 2020-03-27 | 2020-08-07 | 江苏华彩化学科技有限公司 | Water-based environment-friendly anti-cracking interior wall coating for building and preparation method thereof |
| CN115820095B (en) * | 2022-12-01 | 2023-12-12 | 福建省三棵树新材料有限公司 | High-brushing-resistance and stain-resistance skin-feel interior wall finish emulsion paint and preparation method thereof |
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| CN102690404A (en) * | 2011-02-18 | 2012-09-26 | 中国石油化工股份有限公司 | Nonionic waterborne polyurethane dispersoid and preparation method thereof |
| CN102746784A (en) * | 2012-07-30 | 2012-10-24 | 江苏瑞丰科技实业有限公司 | Energy-saving insulated flame-retardant water-proof corrosion-proof functional coating and preparation method thereof |
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