CN104513385A - Preparation method for waterborne alkyd resin and aqueous dispersion thereof - Google Patents
Preparation method for waterborne alkyd resin and aqueous dispersion thereof Download PDFInfo
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- CN104513385A CN104513385A CN201410736206.0A CN201410736206A CN104513385A CN 104513385 A CN104513385 A CN 104513385A CN 201410736206 A CN201410736206 A CN 201410736206A CN 104513385 A CN104513385 A CN 104513385A
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Abstract
Belonging to the field of waterborne paint, the invention relates to a preparation method for waterborne alkyd resin and a dispersion thereof. The method includes: subjecting trimethylolpropane and benzoic acid to catalytic reaction, then adding fatty acid, phthalic anhydride or isophthalic acid to carry out catalytic reaction, then adding trimellitic anhydride to carry out catalytic reaction, then adding a cosolvent and stirring the materials evenly to obtain waterborne alkyd resin; taking the reaction obtained resin, adding 4-6 parts of a neutralizing agent into every 100 parts of the resin, and performing stirring dispersion into 100-150 parts of water to obtain the alkyd resin aqueous dispersion; and adding 2-8 parts of a drier, filler and pigment, assistants and the like into the dispersion to prepare waterborne primer or finish paint. Benzoic acid is employed to replace part of fatty acid in alkyd resin so as to enhance the hardness and dryness of alkyd resin. And the resin is water soluble resin, during use, water is adopted as the diluent, the emission of VOC is greatly reduced from about 70% of solvent based paint to less than 15%, the environment is improved, the harm to human body is reduced, and the hidden danger of fire is also reduced at the same time.
Description
Technical field
The present invention relates to the preparation method of a kind of aqueous alkide resin resin and dispersion thereof, belong to water-borne coatings field.
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 paint occupies very large share at Coating Market, alkyd paint application is originally with dimethylbenzene always, vinyl acetic monomer, N-BUTYL ACETATE equal solvent is diluent solvent type coating, there is very large smell, the health of serious harm people, and be easy to initiation fire, and these risks evaded by water-borne coatings, greatly reduce the discharge (from about 70% near less than 15% of solvent-thinned paint) of VOC, replace solvent also greatly to save petroleum resources with water, reducing solvent cost, is the novel product of an environmental protection.
As the main film forming matter of alkyd paint, resin plays conclusive effect.Even if the present invention is so always for water-based type, the Synolac of water alcohol acid baking vanish, can well replace solvent based coating Synolac, its performance can meet the demands.
Summary of the invention
Goal of the invention is formula providing a kind of aqueous alkide resin and water dispersion thereof and preparation method thereof.
The invention belongs to water-borne coatings field, it is a kind of aqueous alkide resin, unsaturated fatty acids 18-33 part in the formula of synthesis material, TriMethylolPropane(TMP) 17-26 part, phenylformic acid 1-8.8 part, catalyzer 0-0.055 part, phthalic anhydride or m-phthalic acid 14-20 part, trimellitic acid 1,2-anhydride 5-7.7 part, solubility promoter 20-25 part.
The preferred version of each synthesis material is unsaturated fatty acids 20-30 part, TriMethylolPropane(TMP) 18-23 part, phenylformic acid 1-8 part, catalyzer 0-0.05 part, phthalic anhydride or m-phthalic acid 16-19 part, trimellitic acid 1,2-anhydride 5-7 part, solubility promoter 20-25 part.
A preparation method for aqueous alkide resin, comprises the following steps:
(1) by TriMethylolPropane(TMP) 17-26 part, phenylformic acid 1-8.8 part, 25 ~ 50% catalyzer add reaction vessel, start stirring, with in the middle of material, stirring velocity occurs that whirlpool is advisable, slowly heat up, with 3hr, temperature is risen to 220-240 DEG C, keep column temperature at 98-105 DEG C, react to acid number and be less than 3mgKOH/g;
(2) add unsaturated fatty acids 18-33 part, phthalic anhydride or m-phthalic acid 14-20 part, 25 ~ 50% catalyst levelss, rise to 220-240 DEG C of reaction ester below acid number 5mgKOH/g;
(3) be cooled to less than 170 DEG C, add trimellitic acid 1,2-anhydride and residual catalyst, 170-180 DEG C of reaction is to acid number 40-50mgKOH/g;
(4) be cooled to below added solvent boiling point and add solubility promoter, stirring velocity is advisable there to be whirlpool in the middle part of material, stirs, obtains aqueous alkide resin.
This resinous acid value 32-38mgKOH/g, solids content 73-76%.
Get the resin 100 parts that aforesaid method obtains, then add 4-6 part neutralizing agent, dispersed with stirring, in 100-150 part water, obtains aqueous alkide resin water dispersion.This dispersion adds siccative 2-8 part again, color stuffing, and auxiliary agent etc. make water self-drying type priming paint or finish paint.
Described unsaturated fatty acids is dehydrated castor oleic acid, linolenic acid, Bristol oleic acid, eleostearic acid, one or more in behenic acid.
Described solubility promoter is butanols, propylene glycol monomethyl ether, butyl glycol ether, propandiol butyl ether, Virahol, sec-butyl alcohol, ethanol, one or more of ethylene glycol ethyl ether etc.
Described catalyzer is 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 neutralizing agent neutralizing agent is N, N-dimethylethanolamine, triethylamine, N-ethylmorpholine,
Ammoniacal liquor, one or several in AMP95 (2-amino-2-methyl-1-propanol).
Resin structure formula of the present invention is:
Advantage of the present invention
The present invention is a kind of Synolac and water dispersion thereof of water-based, wherein replaces partial fatty acid with phenylformic acid, improves hardness and the dryness of Synolac.
Resin is made water soluble resin by the present invention, and be thinner with water during use, greatly reduce the discharge of VOC, VOC is down to less than 15% from about 70% of solvent-thinned paint, improves environment, reduces the injury to human body, also reduces the hidden danger of fire simultaneously.
So water dispersion of the present invention adds siccative, auxiliary agent, color stuffing etc. can be made into water self-drying type alkyd paint.
Embodiment
Embodiment 1
By TriMethylolPropane(TMP) 22 parts, 8 parts, phenylformic acid, organotin catalysts 0.01 part adds reaction flask, heat up, be raised to from 170 DEG C to 230 DEG C with 3hr, column temperature is kept to be less than 105 DEG C, reaction to acid number is less than 3mgKOH/g, add dehydrated castor oleic acid 22 parts, m-phthalic acid 17 parts, organotin catalysts 0.02 part, progressively be warming up to 230 DEG C, control column temperature less than 105 DEG C, reaction to acid number is less than 5mgKOH/g, be cooled to 170 DEG C, add trimellitic acid 1,2-anhydride 6.5 parts, catalyzer 0.01 part, 180 DEG C of reactions are to acid number 45-50mgKOH/g, be cooled to 160 DEG C, add butyl glycol ether 21 parts, 1.4 parts, butanols, stir, obtain aqueous Synolac, wherein the acid number of resin is at about 33mgKOH/g, admittedly containing about 75%.Dilute according to the Dilution ratio propylene glycol monomethyl ether of 1:1, obtain viscosity 50-100cp, the resin obtained 100 parts, add neutralizing agent N, N-dimethylethanolamine 5 parts, dispersed with stirring is in 100 parts of water, add 8 parts, Jin Huili company siccative (model C G01), 0.4 part, Bi Ke company substrate wetting agents (model BYK346) stirs, water self-drying type alkyd varnish can be obtained, paint film is made in spraying, Air drying 7 days, gained paint film pendulum-rocker hardness 0.22, impact 50cm, snappiness 1mm, adhesion 1 grade, water-fast, salt spray resistance 48hr is non-foaming, non-corrosive, and the VOC of varnish can be controlled in less than 15%.
Embodiment 2
By TriMethylolPropane(TMP) 18 parts, 1.1 parts, phenylformic acid, add reaction flask, heat up, be raised to from 170 DEG C to 230 DEG C with 3hr, column temperature is kept to be less than 105 DEG C, reaction to acid number is less than 3mgKOH/g, add behenic acid 24.5 parts, eleostearic acid 3.8 parts, phthalic anhydride 17 parts, progressively be warming up to 230 DEG C, control column temperature less than 105 DEG C, reaction to acid number is less than 5mgKOH/g, be cooled to 170 DEG C, add trimellitic acid 1,2-anhydride 4.9 parts, 180 DEG C of reactions are to acid number 45-50mgKOH/g, be cooled to 160 DEG C, add ethylene glycol ethyl ether 14 parts, Virahol 8 parts, stir, obtain aqueous alkide resin, wherein the acid number of resin is at about 33mgKOH/g, admittedly containing about 73%.Dilute according to the Dilution ratio propylene glycol monomethyl ether of 1:1, obtain viscosity 50-100cp, the resin obtained 100 parts, add neutralizing agent N, N-dimethylethanolamine 5 parts, be distributed in 100 parts of water, add siccative, auxiliary agent etc., water self-drying type alkyd varnish can be obtained, Air drying 7 days, gained paint film pendulum-rocker hardness 0.22, impacts 50cm, snappiness 1mm, adhesion 1 grade, water-fast, salt spray resistance 48hr is non-foaming, non-corrosive, and the VOC of varnish can be controlled in less than 15%.
Embodiment 3
By TriMethylolPropane(TMP) 21 parts, 7.7 parts, phenylformic acid, organotin catalysts 0.01 part adds reaction flask, heat up, be raised to from 170 DEG C to 230 DEG C with 3hr, column temperature is kept to be less than 105 DEG C, reaction to acid number is less than 3mgKOH/g, add dehydrated castor oleic acid 3 parts, linolenic acid 18 parts, m-phthalic acid 17 parts, organotin catalysts 0.02 part, progressively be warming up to 230 DEG C, control column temperature less than 105 DEG C, reaction to acid number is less than 5mgKOH/g, be cooled to 170 DEG C, add trimellitic acid 1,2-anhydride 5.9 parts, catalyzer 0.01 part, 180 DEG C of reactions are to acid number 45-50mgKOH/g, be cooled to 160 DEG C, add butyl glycol ether 10 parts, 15 parts, butanols, stir, obtain aqueous alkide resin, wherein the acid number of resin is at about 35mgKOH/g, admittedly containing about 75%.Dilute according to the Dilution ratio propylene glycol monomethyl ether of 1:1, obtain viscosity 50-100cp, the resin obtained 100 parts, adds neutralizing agent N, N-dimethylethanolamine 5 parts, be distributed in 100 parts of water, obtain water self-drying type Synolac water dispersion, add siccative in dispersions, auxiliary agent etc., water self-drying type alkyd varnish can be obtained, Air drying 7 days, gained paint film pendulum-rocker hardness 0.22, impacts 50cm, snappiness 1mm, adhesion 1 grade, water-fast, salt spray resistance 48hr is non-foaming, non-corrosive, and the VOC of varnish can be controlled in less than 15%.
Claims (7)
1. a preparation method for aqueous alkide resin, comprises the following steps:
(1) by TriMethylolPropane(TMP) 17-26 part, phenylformic acid 1-8.8 part, in 0-0.055 part catalyzer 25 ~ 50% add reaction vessel, start stirring, with in the middle of material, stirring velocity occurs that whirlpool is advisable, slowly heat up, with 3hr, temperature is risen to 220-240 DEG C, keep column temperature at 98-105 DEG C, react to acid number and be less than 3mgKOH/g;
(2) add unsaturated fatty acids 18-33 part, phthalic anhydride or m-phthalic acid 14-20 part, 25 ~ 50% catalyst levelss, rise to 220-240 DEG C of reaction ester below acid number 5mgKOH/g;
(3) be cooled to less than 170 DEG C, add trimellitic acid 1,2-anhydride and residual catalyst, 170-180 DEG C of reaction is to acid number 40-50mgKOH/g;
(4) be cooled to below added solvent boiling point and add solubility promoter 20-25 part, stirring velocity is advisable there to be whirlpool in the middle part of material, stirs, obtains aqueous alkide resin.
2. the preparation method of a kind of aqueous alkide resin as claimed in claim 1, it is characterized in that, synthesis material is: unsaturated fatty acids 20-30 part, TriMethylolPropane(TMP) 18-23 part, phenylformic acid 1-8 part, catalyzer 0-0.05 part, phthalic anhydride or m-phthalic acid 16-19 part, trimellitic acid 1,2-anhydride 5-7 part, solubility promoter 20-25 part.
3. the preparation method of a kind of aqueous alkide resin as claimed in claim 1, is characterized in that: described unsaturated fatty acids is dehydrated castor oleic acid, linolenic acid, Bristol oleic acid, eleostearic acid, one or more in behenic acid.
4. the preparation method of a kind of aqueous alkide resin as claimed in claim 1, is characterized in that: described solubility promoter is butanols, propylene glycol monomethyl ether, butyl glycol ether, propandiol butyl ether, Virahol, sec-butyl alcohol, ethanol, one or more of ethylene glycol ethyl ether etc.
5. the preparation method of a kind of aqueous alkide resin as claimed in claim 1, it is characterized in that: described catalyzer is 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 the water dispersion of an aqueous alkide resin, it is characterized in that: the Synolac synthesized by claim formula material arbitrary in Claims 1 to 5 gets 100 parts, add 4-6 part neutralizing agent, dispersed with stirring, in 100-150 part water, is uniformly dispersed and obtains aqueous alkide resin water dispersion.
7. the preparation method of the water dispersion of aqueous alkide resin as claimed in claim 6, is characterized in that: described 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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| CN201410736206.0A CN104513385A (en) | 2014-12-04 | 2014-12-04 | Preparation method for waterborne alkyd resin and aqueous dispersion thereof |
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| CN201410736206.0A CN104513385A (en) | 2014-12-04 | 2014-12-04 | Preparation method for waterborne alkyd resin and aqueous dispersion thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774544A (en) * | 2015-04-27 | 2015-07-15 | 西北永新涂料有限公司 | Waterborne alkyd emulsion, waterborne alkyd varnish and waterborne alkyd color lacquer and preparation method of waterborne alkyd emulsion |
| CN105669961A (en) * | 2016-02-02 | 2016-06-15 | 成都杰晟蜀邦新材料科技有限公司 | Highly branched alkyd resin with high solid content and low viscosity and preparation method of alkyd resin |
| CN106832237A (en) * | 2017-01-16 | 2017-06-13 | 南通方鑫化工有限公司 | A kind of castor oil modified polyurethane dull finishing coat alkyd resin composition and preparation method thereof |
| CN106978049A (en) * | 2017-05-17 | 2017-07-25 | 河北晨阳工贸集团有限公司 | It is a kind of for aqueous benzoic acid modified alkyd resin of self-drying paint and preparation method thereof |
| CN107987264A (en) * | 2017-12-26 | 2018-05-04 | 海安常州大学高新技术研发中心 | A kind of preparation method of graphene oxide modified waterborne alkyd anti-corrosion lotion |
| CN108034044A (en) * | 2017-12-29 | 2018-05-15 | 珠海长先新材料科技股份有限公司 | A kind of water-base resin of casing paint and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831061A (en) * | 2010-05-11 | 2010-09-15 | 浙江工业大学 | Benzoic acid modified waterborne alkyd resin and amino plastic baking varnish prepared by same |
-
2014
- 2014-12-04 CN CN201410736206.0A patent/CN104513385A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831061A (en) * | 2010-05-11 | 2010-09-15 | 浙江工业大学 | Benzoic acid modified waterborne alkyd resin and amino plastic baking varnish prepared by same |
Non-Patent Citations (1)
| Title |
|---|
| 吴海霞等: "《精细化工生产技术》", 31 August 2013, 中国石化出版社 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774544A (en) * | 2015-04-27 | 2015-07-15 | 西北永新涂料有限公司 | Waterborne alkyd emulsion, waterborne alkyd varnish and waterborne alkyd color lacquer and preparation method of waterborne alkyd emulsion |
| CN105669961A (en) * | 2016-02-02 | 2016-06-15 | 成都杰晟蜀邦新材料科技有限公司 | Highly branched alkyd resin with high solid content and low viscosity and preparation method of alkyd resin |
| CN106832237A (en) * | 2017-01-16 | 2017-06-13 | 南通方鑫化工有限公司 | A kind of castor oil modified polyurethane dull finishing coat alkyd resin composition and preparation method thereof |
| CN106978049A (en) * | 2017-05-17 | 2017-07-25 | 河北晨阳工贸集团有限公司 | It is a kind of for aqueous benzoic acid modified alkyd resin of self-drying paint and preparation method thereof |
| CN107987264A (en) * | 2017-12-26 | 2018-05-04 | 海安常州大学高新技术研发中心 | A kind of preparation method of graphene oxide modified waterborne alkyd anti-corrosion lotion |
| CN108034044A (en) * | 2017-12-29 | 2018-05-15 | 珠海长先新材料科技股份有限公司 | A kind of water-base resin of casing paint and preparation method thereof |
| CN108034044B (en) * | 2017-12-29 | 2020-09-18 | 珠海长先新材料科技股份有限公司 | Water-based resin for shell paint and preparation method thereof |
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Application publication date: 20150415 |
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