CN104497221A - Waterborne acrylic modified alkyd resin and preparation method of aqueous dispersion of alkyd resin - Google Patents
Waterborne acrylic modified alkyd resin and preparation method of aqueous dispersion of alkyd resin Download PDFInfo
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Abstract
The invention belongs to the field of water-based paints, and in particular discloses waterborne acrylic modified alkyd resin and a preparation method of aqueous dispersion of the alkyd resin. The formula of the alkyd resin consists of the following materials: 11-30 parts of fatty acid, 11-40 parts of polyhydric alcohol, 0.5-2 parts of maleic anhydride, 12-30 parts of binary acid, 0-0.033 part of a catalyst, 17-30 parts of a solvent, 2-6 parts of a (methyl) acrylic monomer, 5-30 parts of a (methyl) acrylic or styrene monomer and 0.3-3 parts of an initiator. The waterborne acrylic modified alkyd resin is prepared by reacting the various materials, wherein the acid value of the resin is 18-25mgKOH/g and the solid content is 75-85%, so that the resin is strong in stability in water. The resin is diluted by propylene glycol monomethyl ether at the ratio of 1 to 1, and viscosity after diluting is 50-200cp. 4-6 parts of a neutralizing agent and 80-150 parts of water are added to 100 parts of the prepared waterborne acrylic modified alkyd resin, an obtained mixture is stirred and dispersed in water, and thus the aqueous dispersion is formed. The aqueous dispersion is added with methylated amino resin, a substrate wetting agent and the like, so that waterborne alkyd amino baking-type varnish is prepared, or the aqueous dispersion is added with various pigments and fillers as well as accessories so as to prepare colored paints in different colors through proper processes; a paint film is good in hardness, adhesion and water resistance, and the emission of a volatile organic compound (VOC) is greatly reduced during a construction process.
Description
Technical field
The present invention belongs to water-borne coatings field, and it is the preparation method of a kind of waterborne acrylic modified alkyd resins and water dispersion thereof.
Background technology
Water-borne coatings replaces solvent with water, can reduce the discharge of VOC to a great extent, be reduced to less than 15% from about 70% of solvent-thinned paint, its environmental acceptability is much higher than solvent type coating, and save petroleum resources, reduce disaster hidden-trouble, improve operating environment.
Alkyd baking vanish occupies very large share at Coating Market, alkyd baking vanish application is originally with dimethylbenzene always, vinyl acetic monomer, N-BUTYL ACETATE equal solvent is diluent solvent type coating, has very large smell, the health of serious harm people, and be easy to initiation fire, and these risks evaded by water-borne coatings, greatly reduced the discharge of VOC, replacing solvent also greatly to save petroleum resources with water, is the novel product of environmental protection always.
As the main film forming matter of alkyd baking vanish, resin plays conclusive effect.Even if the present invention is so always for the waterborne acrylic modified alkyd resins of water alcohol acid baking vanish, can well replace solvent based coating Synolac, its performance can meet the demands.
Summary of the invention
The invention provides a kind of formula of waterborne acrylic modified alkyd resins and the preparation method of water dispersion.
The present invention belongs to water-borne coatings field, relates to a kind of waterborne acrylic modified alkyd resins and water dispersion thereof.Lipid acid 11-30 part in its synthesizing formula, polyvalent alcohol 11-40 part, MALEIC ANHYDRIDE 0.5-2 part, diprotic acid 12-30 part, catalyzer 0-0.033 part, solvent 17-30 part, (methyl) Acrylic Acid Monomer 2-6 part, (methyl) esters of acrylic acid or styrene monomer 5-30 part, initiator 0.3-3 part.
Preferred fatty acid 13-25 part in formula, polyvalent alcohol 13-32 part, MALEIC ANHYDRIDE 0.7-1.5 part, diprotic acid 14-24 part, catalyzer 0-0.03 part, solvent 17-30 part, (methyl) Acrylic Acid Monomer 2-4 part, (methyl) esters of acrylic acid or styrene monomer 7-17 part, initiator 0.5-2 part.
A preparation method for waterborne acrylic modified alkyd resins and water dispersion thereof, concrete steps are:
(1) by lipid acid 11-30 part, polyvalent alcohol 11-40 part, MALEIC ANHYDRIDE 0.5-2 part, diprotic acid 12-30 part, catalyzer 0-0.033 part adds in reaction vessel, is under agitation progressively warming up to 180-240 DEG C, deviates from micromolecular water in reaction process, control column temperature 98-105 DEG C, react to acid number and be less than 10mgKOH/g;
(2) be cooled to below solvent boiling point, add solvent 7-10 part and stir, and temperature is remained on 110-150 DEG C;
(3) mixture of (methyl) vinylformic acid 2-6 part and (methyl) acrylic ester monomer, styrene monomer 5-30 part and initiator 0.3-1 part is at the uniform velocity dripped with 2.5-3hr, after dripping, residue initiator 0-2 part is become 3 parts, per hourly add portion, finally continue at 110-150 DEG C of reaction 3hr;
(4) be cooled to below added solvent boiling point, add remaining 10-20 part solvent, stir, obtain waterborne acrylic modified alkyd resins.Wherein the acid number of resin is at 18-25mgKOH/g, admittedly containing 75-85%.
The preparation method of waterborne acrylic modified alkyd resins water dispersion, the resin obtained 100 parts, adds neutralizing agent 4-6 part, water 80-150 part, and dispersed with stirring forms waterborne acrylic modified alkyd resins water dispersion.
Add methyl-etherified aminoresin, substrate wetting agents etc. by waterborne acrylic modified alkyd resins water dispersion, the amino baking-type varnish of water alcohol acid can be obtained, or add various color stuffing and the auxiliary agent colored paint through suitable technique furnishing shades of colour.The hardness that various paint class paint film has had, sticking power, water tolerance, greatly reduces VOC discharge in construction process.
The molecular formula of resin or skeleton symbol
Lipid acid described in formula is behenic acid, cocinic acid, linolenic acid, one or more in tall oil acid.
Polyvalent alcohol described in formula is TriMethylolPropane(TMP), tetramethylolmethane, glycerine, neopentyl glycol, one or more in propylene glycol.
Diprotic acid described in formula is phthalic anhydride, hexanodioic acid, m-phthalic acid, one or more in terephthalic acid.
Described catalyzer is titanium tetraethoxide, four n-propyl alcohol titaniums, four n-butyl titaniums, four (20 ethylhexanol) titanium, butyl titanium isopropylate, Mono-n-butyltin, one or more of Dibutyltin oxide.
Described solvent is butyl glycol ether, butanols, butyl, propandiol butyl ether, dipropylene, propylene glycol monomethyl ether, Virahol, sec-butyl alcohol, one or more in the water-soluble alcohol ether solvents such as ethanol.
Described Acrylic Acid Monomer is one or both of acrylic or methacrylic acid, provides resin water-soluble.
Described (methyl) acrylic ester monomer is (methyl) butyl acrylate, vinylbenzene, (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, isobornyl methacrylate, several in methyl methacrylate.
Described initiator is perbenzoic acid, the benzoyl peroxide tert-butyl ester, ditertiary butyl peroxide, two t-amyl peroxy compounds, hydrogen phosphide cumene, one or both in peroxidation (2 ethyl hexanoic acid) tert-butyl ester.
Described neutralizing agent is N, N-dimethylethanolamine, triethylamine, N-ethylmorpholine, ammoniacal liquor, one or several in AMP95 (2-amino-2-methyl-1-propanol).
Advantage of the present invention
The present invention with a kind of Synolac for core, shell is become with (methyl) acrylic acid and propynoic acid ester class monomer copolymerization of band acidic group, carboxyl on vinylformic acid provides water soluble group, in and salify after be distributed in water, Synolac is caused to be core, ester bond is well protected, be conducive to the raising of the stability to hydrolysis of ester bond, make resin in water, have good stability, hydroxyl in the remaining hydroxyl of Synolac and acrylics monomer provides a large amount of oh groups, can be cross-linked with the carrying out of the linking agents such as aminoresin, after making the temperature baking of prepared paint more than 120 DEG C, form film, there is certain protectiveness and decorative effect.
Resin is made water soluble resin by the present invention, is thinner, greatly reduces the discharge of VOC, be reduced to less than 15%, improve environment from about 70% of solvent-thinned paint, reduce the injury to human body, also reduce the hidden danger of fire simultaneously with water.
So product of the present invention can be applied to aminoresin, urea-formaldehyde resin etc. are crosslinked makes baking-type coating, the hardness had, sticking power, water tolerance, and construction process gather greatly reduce VOC discharge, have very large benefit to environment protection.
Embodiment
Embodiment 1
By soy(a)-bean oil fatty acid 23 parts, TriMethylolPropane(TMP) 20 parts, MALEIC ANHYDRIDE 0.93 part, phthalic anhydride 10 parts, hexanodioic acid 5.5 parts, add in reaction vessel, stir and be progressively warming up to 220 DEG C, control column temperature less than 105 DEG C, reaction to acid number is less than 10mgKOH/g, be cooled to 160 DEG C, add butyl glycol ether 7 parts to stir, and temperature is remained on 115 DEG C, then 2 parts, vinylformic acid and methyl methacrylate 11 parts is at the uniform velocity dripped with 2.5-3hr, butyl acrylate 1.8 parts, Hydroxyethyl acrylate 1.6 parts, the mixture that initiator perbenzoic acid is 0.5 part, at 130 DEG C, initiator peroxidized t-butyl perbenzoate 0.99 part is divided into 3 parts after dripping, per hourly add portion, finally continue at reaction 3hr at 130 DEG C, be cooled to 80 DEG C, add remaining 11 parts of butanols, stir, obtain aqueous acrylic acid modified alkyd resin, wherein the acid number of resin is at about 18mgKOH/g, admittedly containing 80%.Get the above waterborne acrylic modified alkyd resins obtained, dilute according to the ratio propylene glycol monomethyl ether of 1:1, viscosity 50-200cp after dilution.The resin obtained 100 parts, adds neutralizing agent N, N-dimethylethanolamine 5 parts, then dispersed with stirring is in 120 parts of water, then adds 15 parts, part methyl-etherified aminoresin, substrate wetting agents 0.4 part, alcohol acid amido baking varnish can be obtained, be sprayed on the tinplate after polishing, 140 DEG C of baking 30min, gained hardness of paint film H, impacts 50cm, snappiness 1mm, adhesion 1 grade, water-fast, salt spray resistance 120hr is non-foaming, non-corrosive, VOC can be controlled in less than 15%, and stability in storage can reach half a year more than.
Embodiment 2
By cocinic acid 17 parts, TriMethylolPropane(TMP) 21 parts, MALEIC ANHYDRIDE 1 part, phthalic anhydride 10.5 parts, hexanodioic acid 6.5 parts, add in reaction vessel, stir and be progressively warming up to 220 DEG C, control column temperature less than 105 DEG C, reaction to acid number is less than 10mgKOH/g, be cooled to 160 DEG C, add butyl glycol ether 8 parts to stir, and temperature is remained on 115 DEG C, then 2.2 parts, vinylformic acid and methyl methacrylate 12 parts is at the uniform velocity dripped with 2.5-3hr, butyl acrylate 1.9 parts, Hydroxyethyl acrylate 1.7 parts, the mixture that initiator perbenzoic acid is 0.6 part, at 130 DEG C, initiator peroxidized t-butyl perbenzoate 1 part is divided into 3 parts after dripping, per hourly add portion, finally continue at reaction 3hr at 130 DEG C, be cooled to 80 DEG C, add remaining 12 parts of butanols, stir, obtain aqueous acrylic acid modified alkyd resin, wherein the acid number of resin is at about 19mgKOH/g, solid content 79%.Get the above waterborne acrylic modified alkyd resins obtained, dilute according to the ratio propylene glycol monomethyl ether of 1:1, viscosity 50-200cp after dilution.The resin obtained 100 parts, add neutralizing agent N, N-dimethylethanolamine 5 parts, then dispersed with stirring is in 100-part water, then adds 20 parts, part methyl-etherified aminoresin, substrate wetting agents 0.4 part, alcohol acid amido baking varnish can be obtained, be sprayed on the tinplate after polishing, 140 DEG C of bakings 30min, gained hardness of paint film H, impact 50cm, snappiness 1mm, adhesion 1 grade, water-fast, salt spray resistance 120hr is non-foaming, non-corrosive, VOC can be controlled in less than 15%, and resin stability in storage can reach half a year more than.
Embodiment 3
By soy(a)-bean oil fatty acid 14.2 parts, TriMethylolPropane(TMP) 13.4 parts, neopentyl glycol 10.4 parts, MALEIC ANHYDRIDE 1 part, phthalic anhydride 16.2 parts, hexanodioic acid 5.8 parts, organotin catalysts 0.03 part, add in reaction vessel, stir and be progressively warming up to 220 DEG C, control column temperature less than 105 DEG C, reaction to acid number is less than 10mgKOH/g, be cooled to 160 DEG C, add butyl glycol ether 9 parts to stir, and temperature is remained on 145 DEG C, then 2.5 parts, vinylformic acid and methyl methacrylate 5.6 parts is at the uniform velocity dripped with 2.5-3hr, vinylbenzene 5.6 parts, Hydroxyethyl acrylate 1.6 parts, the mixture that initiator ditertiary butyl peroxide is 0.6 part, at 145 DEG C of reaction 3hr after dripping, be cooled to 80 DEG C, add 11 parts of propylene glycol monomethyl ethers, stir. obtain aqueous acrylic acid modified alkyd resin, wherein the acid number of resin is at about 22mgKOH/g, admittedly containing 79%.Get the above waterborne acrylic modified alkyd resins obtained, dilute according to the ratio propylene glycol monomethyl ether of 1:1, viscosity 50-200cp after dilution.The resin obtained 100 parts, adds neutralizing agent N, N-dimethylethanolamine 5 parts, then dispersed with stirring is in 100 parts of water, then adds 20 parts, part methyl-etherified aminoresin, substrate wetting agents 0.4 part, alcohol acid amido baking varnish can be obtained, be sprayed on the tinplate after polishing, 140 DEG C of baking 30min, gained hardness of paint film H, impacts 50cm, snappiness 1mm, adhesion 1 grade, water-fast, salt spray resistance 120hr is non-foaming, non-corrosive.VOC can be controlled in less than 15%.The resin stability in storage that this formula obtains can reach half a year more than.
Embodiment 4
By soy(a)-bean oil fatty acid 24 parts, glycerine 14 parts, MALEIC ANHYDRIDE 0.9 part, phthalic anhydride 16.7 parts, add in reaction vessel, stir and be progressively warming up to 220 DEG C, control column temperature 105 DEG C, reaction to acid number is less than 10mgKOH/g, be cooled to 115 DEG C, then 4 parts, vinylformic acid and methyl methacrylate 7.7 parts is at the uniform velocity dripped with 2.5-3hr, the mixture that initiator perbenzoic acid is 0.6 part, after dripping, peroxidized t-butyl perbenzoate 0.2 part is added in 130 DEG C of reaction 3hr, be cooled to 80 DEG C, add 10 parts of butanols, 5 parts of butyl glycol ethers, stir, obtain aqueous acrylic acid modified alkyd resin, wherein the acid number of resin is at about 18mgKOH/g, admittedly containing 80%.Get the above waterborne acrylic modified alkyd resins obtained, dilute according to the ratio propylene glycol monomethyl ether of 1:1, viscosity 50-200cp after dilution.The resin obtained 100 parts, adds neutralizing agent N, N-dimethylethanolamine 5 parts, then dispersed with stirring is in 100 parts of water, then adds 15 parts, part methyl-etherified aminoresin, substrate wetting agents 0.4 part, alcohol acid amido baking varnish can be obtained, be sprayed on the tinplate after polishing, 140 DEG C of baking 30min, gained hardness of paint film H, impacts 50cm, snappiness 1mm, adhesion 1 grade, water-fast, salt spray resistance 120hr is non-foaming, non-corrosive.The resin VOC that this formula obtains controls below 15%, and stability in storage can reach half a year more than.
Claims (10)
1. a preparation method for waterborne acrylic modified alkyd resins, concrete steps are:
(1) by lipid acid 11-30 part, polyvalent alcohol 11-40 part, MALEIC ANHYDRIDE 0.5-2 part, diprotic acid 12-30 part, catalyzer 0-0.033 part adds in reaction vessel, is under agitation progressively warming up to 180-240 DEG C, deviates from micromolecular water in reaction process, control column temperature 98-105 DEG C, react to acid number and be less than 10mgKOH/g;
(2) be cooled to below solvent boiling point, add solvent 7-10 part and stir, and temperature is remained on 110-150 DEG C;
(3) mixture of (methyl) vinylformic acid 2-6 part and (methyl) acrylic ester monomer, styrene monomer 5-30 part and initiator 0.3-1 part is at the uniform velocity dripped with 2.5-3hr, after dripping, residue initiator 0-2 part is become 3 parts, per hourly add portion, finally continue at 110-150 DEG C of reaction 3hr;
(4) be cooled to below added solvent boiling point, add remaining 10-20 part solvent, stir, obtain waterborne acrylic modified alkyd resins.
2. the preparation method of a kind of waterborne acrylic modified alkyd resins as claimed in claim 1, it is characterized in that: raw material range is lipid acid 13-25 part, polyvalent alcohol 13-32 part, MALEIC ANHYDRIDE 0.7-1.5 part, diprotic acid 14-24 part, catalyzer 0-0.03 part, solvent 17-30 part, (methyl) Acrylic Acid Monomer 2-4 part, (methyl) esters of acrylic acid or styrene monomer 7-17 part, initiator 0.5-2 part.
3. the preparation method of a kind of waterborne acrylic modified alkyd resins as claimed in claim 1, is characterized in that: described lipid acid is behenic acid, cocinic acid, linolenic acid, one or more in tall oil acid; Described polyvalent alcohol is TriMethylolPropane(TMP), tetramethylolmethane, glycerine, neopentyl glycol, one or more in propylene glycol.
4. the preparation method of a kind of waterborne acrylic modified alkyd resins as claimed in claim 1, is characterized in that: described diprotic acid is phthalic anhydride, hexanodioic acid, m-phthalic acid, one or more in terephthalic acid.
5. the preparation method of a kind of waterborne acrylic modified alkyd resins as claimed in claim 1, it is characterized in that: described catalyzer is titanium tetraethoxide, four n-propyl alcohol titaniums, four n-butyl titaniums, four (20 ethylhexanol) titanium, butyl titanium isopropylate, Mono-n-butyltin, one or more of Dibutyltin oxide.
6. the preparation method of a kind of waterborne acrylic modified alkyd resins as claimed in claim 1, it is characterized in that: described solvent is butyl glycol ether, butanols, butyl, propandiol butyl ether, dipropylene, propylene glycol monomethyl ether, Virahol, sec-butyl alcohol, one or more in the water-soluble alcohol ether solvents such as ethanol.
7. the preparation method of a kind of waterborne acrylic modified alkyd resins as claimed in claim 1, is characterized in that: described Acrylic Acid Monomer is one or both of acrylic or methacrylic acid; Described (methyl) acrylic ester monomer is (methyl) butyl acrylate, vinylbenzene, (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, isobornyl methacrylate, several in methyl methacrylate.
8. the preparation method of a kind of waterborne acrylic modified alkyd resins as claimed in claim 1, it is characterized in that: described initiator is perbenzoic acid, the benzoyl peroxide tert-butyl ester, ditertiary butyl peroxide, two t-amyl peroxy compounds, hydrogen phosphide cumene, one or both in peroxidation (2 ethyl hexanoic acid) tert-butyl ester.
9. the preparation method of a waterborne acrylic modified alkyd resins dispersion, it adopts arbitrary formula range in claim 1-8 to obtain waterborne acrylic modified alkyd resins, get 100 parts, add neutralizing agent 4-6 part, water 80-150 part, dispersed with stirring forms waterborne acrylic modified alkyd resins water dispersion.
10. the preparation method of waterborne acrylic modified alkyd resins dispersion as claimed in claim 9, wherein neutralizing agent is N, N-dimethylethanolamine, triethylamine, N-ethylmorpholine, ammoniacal liquor, one or several in AMP95 (2-amino-2-methyl-1-propanol).
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| CN104877514A (en) * | 2014-12-04 | 2015-09-02 | 北京金汇利应用化工制品有限公司 | Amino resin stoving varnish containing water-borne acrylic modified alkyd resin and preparation method thereof |
| CN104945567A (en) * | 2015-05-20 | 2015-09-30 | 安徽省金盾涂料有限责任公司 | Modified waterborne alkyd resin and preparation method thereof |
| CN105131263A (en) * | 2015-08-19 | 2015-12-09 | 盘锦辽河油田金宇建筑材料有限公司 | Organosilicon epoxy acrylic acid modified waterborne alkyd resin emulsion and coating thereof |
| CN108976399A (en) * | 2018-08-17 | 2018-12-11 | 重庆南方漆业有限公司 | A kind of aqueous alkide resin and preparation method thereof |
| CN109306037A (en) * | 2018-09-19 | 2019-02-05 | 江苏三木化工股份有限公司 | A kind of waterborne acrylic modified alkyd resins and preparation method |
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| CN104945567B (en) * | 2015-05-20 | 2019-02-15 | 安徽省金盾涂料有限责任公司 | A kind of modified water-based alkyd resin and preparation method thereof |
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| CN109486379A (en) * | 2018-09-10 | 2019-03-19 | 上海大学 | Acrylic acid modified alkyd resin secondary breakup system and preparation method thereof |
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Application publication date: 20150408 |