CN101070377A - Water-soluble alcohol-acid resin solution and water-soluble alcohol-acid amino baking paint and preparing method - Google Patents
Water-soluble alcohol-acid resin solution and water-soluble alcohol-acid amino baking paint and preparing method Download PDFInfo
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Abstract
The present invention disclosed a kind of water-soluble alkyd resin solution and a kind of water-soluble alkyd amino baking finish using water-soluble alkyd resin solution as base material and their preparation methods. The water-soluble alkyd resin solution is synthesized firstly, and is used for base material then. After prepared with paints, water, additives and amino resin, and through steps of distribution, grinding, etc., the resin solution will be processed into high gloss water-soluble alkyd amino baking finish. The baking finish used water as diluent, is noncombustible, and has no harm to the health of its users. The baking finish has low levels of volatile organic compounds, which meets the national environment protection requirements for water borne coatings and is secure and easy to use. The baking finish has a high mechanical strength of its painting film, a high corrosion stability, and well weather ability. Its every indicator has achieved or exceeded the indicator of solvent type alkyd amino baking finish.
Description
Technical field
The present invention relates to the paint field, be specifically related to a kind of alkyd resin solution and contain the baking finish of this alkyd resin solution, and the preparation method of alkyd resin solution and baking finish.
Background technology
Aminoresin cooperates the amino oven dry coating made from Synolac, be one of most widely used coating in present industrial coating field.Its forms films and has higher hardness and glossiness, resistance to acids and bases, water tolerance and weathering resistance all obviously are better than alkydpaints, but and pipelining, easy construction.
At present, the amino oven dry of China coating all occupies important position in industries such as light industry, household electrical appliances, automobile and machineries.But traditional amino oven dry coating all is solvent type basically, and the volatilization of a large amount of noxious solvents has not only worsened operating environment in the drying course, has increased disaster hidden-trouble, also atmosphere has been caused serious pollution.Day by day strict along with the big bulge in price of petroleum products in the global range and various countries' environmental regulation, coating material production producer and coating user particularly pay attention to the raw materials cost of coating and organic volatile (VOC) content of finished product coating.Therefore, under the prerequisite that fully satisfies use properties, exploitation water-based oven dry coating substitutes it, and promptly economize on resources and alleviate environmental pollution, secure and non-combustible, be a kind of environmentally friendly coating with wide market development prospect.
Because aqueous alkide resin and aminoresin compatibility are bad, cause gloss of film and clarity far away not as good as the baking finish of solvent-borne type alcohol acid amido.And since the ester bond of aqueous alkide resin molecular chain under weak basic condition than facile hydrolysis, the coating package stability is descended, and defective such as paint film poor water resistance.It uses these two effects limit widely.
Summary of the invention
The objective of the invention is to overcome the shortcoming of the amino oven dry of existing solvent-borne type coating, prescription and synthesis technique by the design water soluble alkyd resin, make full use of the degraded that intermolecular neighboring group effect and steric effect stop resin, the oil content of control Synolac, synthesising stability good water-solubility Synolac.
Another object of the present invention provides a kind of preparation method of above-mentioned water soluble alkyd resin.
The present invention also has a purpose to provide a kind ofly to utilize above-mentioned water soluble alkyd resin solution to make base-material, and selection and water soluble alkyd resin consistency aminoresin preferably, through preparation meticulously, design the water-soluble alcohol acid amine baking varnish of a kind of gloss height, period of storage length, good mechanical property, the performance index of this baking finish paint film can reach traditional solvent-borne type alcohol acid amido oven dry coating standard, and especially gloss of film and clarity surpass the baking finish of common solvent type alcohol acid amido.
Another object of the present invention provides a kind of preparation method of water-soluble alcohol acid amine baking varnish.
Purpose of the present invention can reach by following measure:
A kind of water soluble alkyd resin solution, the prescription of this water soluble alkyd resin solution comprises following raw material:
| Component | Weight (%) |
| Castor oil acid phthalic anhydride pentaerythrite trimellitic anhydride water cosolvent nertralizer | 10～20 10～20 10～15 3～5 30～40 4～8 6～10 |
Wherein neutralizing agent is selected from N-ethylmorpholine, N, one or more in N dimethylethanolamine, triethylamine or 20～30% the ammoniacal liquor (mass percent, preferred 25%).
Wherein solubility promoter is selected from one or more in ethylene glycol monobutyl ether, propylene glycol monobutyl ether or the butanols.
A kind of method for preparing above-mentioned water soluble alkyd resin solution comprises the steps:
(1) ricinolic acid of formula ratio, tetramethylolmethane and phthalic anhydride are mixed, stir and add dimethylbenzene down, and be warming up to 180～210 ℃ and carry out esterification, stopped reaction when acid number is reduced to 30-40mgKOH/g;
(2) after above-mentioned reaction stops, being cooled to 140～160 ℃, adding the trimellitic acid 1,2-anhydride of formula ratio, be warming up to 170～200 ℃ more gradually and carry out esterification, dropping to 60～70mgKOH/g to acid number is reaction end;
(3) step 2 is behind reaction end, and vacuum filtration is removed solvent xylene, is cooled to 50～60 ℃, adds solubility promoter, the neutralizing agent of formula ratio, transfers pH to 7～8, after the water that adds formula ratio again disperses, obtains water soluble alkyd resin solution.
The consumption of solvent xylene is 4～6% of all raw materials quality in the reaction, preferred 5%.
More than one state the water-soluble alcohol acid amine baking varnish that water soluble alkyd resin solution is made base-material, and prescription comprises following raw material:
| Component | Weight (%) |
| Water soluble alkyd resin solution pigments auxiliary agent water aminoresin | 35～55 20～40 1～5 5～20 5～10 |
Wherein aminoresin is water soluble amino resin, 5717 or 5386 of the R717 or 2608 of the special company of preferred cyanogen, three wooden companies, and the consumption between each aminoresin is an arbitrary proportion.
Wherein pigment is selected from one or more in chrome yellow, Tai Dark-red indigo plant, lemon yellow, molybdenum red, titanium dioxide or the toluidine red.
Wherein auxiliary agent is selected from one or more in water-soluble wetting dispersing agent, defoamer or the flow agent.The water-based wetting dispersing agent is preferably 4580 of EFKA company, and defoamer is preferably the AQ3025 of the special company of cyanogen, and flow agent is preferably the special VXW6214 of company of cyanogen.
A kind of method for preparing above-mentioned water-soluble alcohol acid amine baking varnish comprises the steps:
(1) the water soluble alkyd resin solution of the water of formula ratio, auxiliary agent and 30～50% is mixed after, add the pigment of formula ratio, stirring obtains slurry;
(2) with slurry, being ground to fineness is 10～15 microns, gets mill base;
(3) in mill base, add after remainder water dissolubility alkyd resin solution stirs, add the aminoresin of formula ratio, stir, filter the water-soluble alcohol acid amine baking varnish.
Purpose of the present invention specifically can reach by following measure:
Water soluble alkyd resin solution can be synthetic by following prescription:
| Component | Weight (%) |
| Castor oil acid phthalic anhydride pentaerythrite trimellitic anhydride water cosolvent nertralizer | 10～20 10～20 10～15 3～5 30～40 4～8 6～10 |
To achieve the object of the present invention, the preparation method that takes of the present invention is as follows:
1. drop into ricinolic acid, tetramethylolmethane and the phthalic anhydride of prescription metering in reactor, start stirring, add dimethylbenzene, be warmed up to 180-210 ℃ and carry out esterification, dropping to 30-40mgKOH/g to acid number is the first step esterification terminal point.
2. be cooled to 150 ℃, add trimellitic acid 1,2-anhydride, be warmed up to 170-200 ℃ more gradually and carry out esterification, dropping to 60-70mgKOH/g to acid number is reaction end.
3. be cooled to 60 ℃, add solubility promoter, the neutralizing agent of formula ratio, adjust pH=7-8, added water-dispersion 3-5 minute again, both getting solid part is the water soluble alkyd resin solution of 40-60%.
Above-mentioned solubility promoter is chosen one or more in ethylene glycol monobutyl ether, propylene glycol monobutyl ether, the butanols.Neutralizing agent is to be selected from N-ethylmorpholine, N, one or more in N dimethylethanolamine, triethylamine, the ammoniacal liquor.Water is deionized water or distilled water, and the content that requires water-soluble substances wherein is less than 100ppm.
Water soluble alkyd resin solution of the present invention is carboxyl by the hydrophilic radical of introducing in the Synolac molecular chain, by in the amine and after be dispersed in the water and form, make full use of the degraded that intermolecular neighboring group effect and steric effect stop resin, its good stability.
The present invention utilizes the water soluble alkyd resin solution of gained to make base-material to cooperate with pigment, auxiliary agent, water and make the water-soluble alcohol acid amine baking varnish, and its composition comprises:
| Component | Weight (%) |
| Water soluble alkyd resin solution | 35～55 |
| Pigment | 20～40 |
| Auxiliary agent | 1～5 |
| Water | 5～10 |
| Aminoresin | 5～20 |
The preparation method of this water-soluble alcohol acid amine baking varnish is:
1. in joining the slurry container, add water, auxiliary agent, the portion water dissolubility alkyd resin solution of accurately metering, stir with the adjustable high-speed dispersion machine.
2. add the pigment in the above-mentioned prescription, stir.
3. the slurry that (2) step is stirred is transferred in the grinding plant, and being ground to fineness is the 10-15 micron, gets mill base.
4. in joining the lacquer container, add above-mentioned mill base, add remainder water dissolubility alkyd resin solution, stir.
5. add the aminoresin of above-mentioned formula ratio, stir.
6. filter, packing gets finished product water-soluble alcohol acid amine baking varnish.
Described pigment is selected from medium chrome yellow medium yellow, Tai Dark-red indigo plant, lemon yellow, molybdenum red, titanium dioxide, toluidine red, chooses wherein one or more, and the consumption between each pigment is an arbitrary proportion.
The present invention makes full use of the degraded that intermolecular neighboring group effect and steric effect stop resin, synthesising stability good water-solubility Synolac.Because water soluble alkyd resin is wetting good inadequately to pigment, so will add a certain amount of water-soluble wetting dispersing agent, improves the dispersiveness of pigment in water soluble alkyd resin, so that further increase the package stability of this water-soluble alcohol acid amine baking varnish.And selection and water soluble alkyd resin consistency moderate etherified amino resins preferably,, through preparation meticulously, design that a kind of gloss height, period of storage are long, water-soluble alcohol acid amine baking varnish of good mechanical property and preparation method thereof.
The water-soluble alcohol acid amine baking varnish that the present invention relates to has following characteristics:
1. gloss of film substantially exceeds similar water-thinned baking paint with clarity, even surpasses the level of common solvent type amine baking varnish.
2. these baking finish raw material sources are wide, and cost is low, is convenient to large-scale promotion application.
3. safe and convenient to use, this baking finish is dispersion medium with water, and VOC (volatile organic matter) is very low, reaches country fully to the water-miscible paint environmental protection requirement, has improved construction environment, has avoided disaster hidden-trouble.
The every index of this baking finish has met or exceeded solvent-borne type alcohol acid amido baking finish level, can replace the baking finish of solvent-borne type alcohol acid amido fully, and verified this baking finish is applicable to the application of industries such as light industry, household electrical appliances, automobile and machinery.
Embodiment
Only the invention will be further described for following example, summary of the invention do not limited.
The prescription of the water soluble alkyd resin solution of table 1 embodiment 1～5
| Component | Weight (%) | ||||
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Ricinolic acid | 15 | 16 | 18 | 18 | 13 |
| Phthalic anhydride | 16 | 15 | 14 | 18 | 19 |
| Tetramethylolmethane | 15 | 15 | 13 | 13 | 11 |
| Trimellitic acid 1,2-anhydride | 4 | 4 | 5 | 5 | 5 |
| Water | 36 | 36 | 36 | 30 | 40 |
| Solubility promoter | 6 | 6 | 6 | 7 | 5 |
| Neutralizing agent | 8 | 8 | 8 | 9 | 7 |
Embodiment 1
The prescription of water soluble alkyd resin solution sees Table 1, and neutralizing agent is a N-ethylmorpholine, and solubility promoter is a butanols.
The water soluble alkyd resin solution manufacturing method:
1. drop into ricinolic acid, tetramethylolmethane and the phthalic anhydride of prescription metering in reactor, start stirring, add dimethylbenzene, be warmed up to 200 ℃ and carry out esterification, dropping to 30～40mgKOH/g to acid number is the first step esterification terminal point;
2. be cooled to 150 ℃, add trimellitic acid 1,2-anhydride, be warmed up to 180 ℃ more gradually and carry out esterification, dropping to 60～70mgKOH/g to acid number is reaction end;
3. be cooled to 60 ℃, vacuum filtration removes removal xylene, adds co-solvent ethylene gylcol monobutyl ether, the neutralizing agent N-ethylmorpholine of formula ratio, adjusts pH=7～8, adds water-dispersion again 3～5 minutes, obtains water soluble alkyd resin solution.
Embodiment 2
The prescription of water soluble alkyd resin solution sees Table 1, and wherein neutralizing agent is selected N for use, the N dimethylethanolamine, and solubility promoter is selected ethylene glycol monobutyl ether for use.The preparation method is with embodiment 1.
Embodiment 3
The prescription of water soluble alkyd resin solution sees Table 1, and wherein neutralizing agent is selected triethylamine for use, and solubility promoter is selected butanols for use.Except that neutralizing agent was selected ammoniacal liquor for use, other were with the preparation method of embodiment 1 among the preparation method.
Embodiment 4
The prescription of water soluble alkyd resin solution sees Table 1, and wherein neutralizing agent is selected the ammoniacal liquor of 20% mass content for use, and solubility promoter is selected propylene glycol monobutyl ether for use.Remove step 1 temperature of reaction among the preparation method and adopt 185 ℃, step 2 temperature of reaction adopts 195 ℃, and neutralizing agent is selected N for use, and N dimethylethanolamine, solubility promoter are selected for use outside the propylene glycol monobutyl ether, and other are with the preparation method of embodiment 1.
Embodiment 5
The prescription of water soluble alkyd resin solution sees Table 1, and wherein neutralizing agent is selected triethylamine for use, and solubility promoter is selected butanols for use.Remove step 1 temperature of reaction among the preparation method and adopt 205 ℃, step 2 temperature of reaction adopts 175 ℃, and neutralizing agent is selected triethylamine for use, and solubility promoter is selected for use outside the butanols, and other are with the preparation method of embodiment 1.
The present invention utilizes the water soluble alkyd resin solution of embodiment 1 gained to make base-material to cooperate with pigment, auxiliary agent, water and make the water-soluble alcohol acid amine baking varnish, and its composition sees Table 2.
The prescription of the water-soluble alcohol acid amine baking varnish of table 2 embodiment 6～10
| Component | Weight (%) | ||||
| Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | |
| Water soluble alkyd resin solution | 55 | 52 | 55 | 52 | 50 |
| The pigment medium chrome yellow medium yellow | 1 | 18 | 1 | 18 | 21 |
| The pigment molybdenum red | 19 | 0 | 19 | 0 | 0 |
| Pigment Tai Dark-red indigo plant | 0 | 2 | 0 | 2 | 2 |
| The pigment toluidine red | 0 | 0 | 0 | 0 | 3 |
| The amino tree of Ineos water-based | 6.5 | 6.5 | 0 | 0 | 0 |
| Fat R717 | |||||
| Ineos water-compatible amino resin 6208 | 0 | 0 | 6 | 6 | 6 |
| The special aqueous dispersant 2608 of cyanogen | 1.5 | 1.5 | 1.5 | 1.5 | 1 |
| The special water-based defoamer of cyanogen AQ3025 | 1 | 1 | 1 | 1 | 1 |
| The special water-based flow agent 6214 of cyanogen | 1 | 1 | 1 | 1 | 1 |
| Water | 15 | 18 | 15.5 | 18.5 | 15 |
Embodiment 6
The prescription of water-soluble alcohol acid amine baking varnish sees Table 2.
The preparation method of water-soluble alcohol acid amine baking varnish:
1. in joining the slurry container, add the water, auxiliary agent of accurately metering, 40% water soluble alkyd resin solution, stir with the adjustable high-speed dispersion machine.
2. add the pigment in the above-mentioned prescription, stir.
3. the slurry that (2) step is stirred is transferred in the grinding plant, and being ground to fineness is 15 microns, gets mill base.
4. in joining the lacquer container, add above-mentioned mill base, add remainder water dissolubility alkyd resin solution, stir.
5. add the aminoresin of above-mentioned formula ratio, stir.
6. filter, packing gets finished product water-soluble alcohol acid amine baking varnish.
Embodiment 7
The prescription of water-soluble alcohol acid amine baking varnish sees Table 2.
The preparation method of water-soluble alcohol acid amine baking varnish is with embodiment 6.
Embodiment 8
The prescription of water-soluble alcohol acid amine baking varnish sees Table 2.
The preparation method of water-soluble alcohol acid amine baking varnish is with embodiment 6.
Embodiment 9
The prescription of water-soluble alcohol acid amine baking varnish sees Table 2.
The preparation method of water-soluble alcohol acid amine baking varnish is with embodiment 6.
Embodiment 10
The prescription of water-soluble alcohol acid amine baking varnish sees Table 2.
The preparation method of water-soluble alcohol acid amine baking varnish is with embodiment 6.
Claims (9)
1, a kind of water soluble alkyd resin solution, its characteristic is that the prescription of this water soluble alkyd resin solution comprises following raw material:
2, water soluble alkyd resin solution according to claim 1, its characteristic are that described neutralizing agent is selected from N-ethylmorpholine, N, one or more in N dimethylethanolamine, triethylamine or the ammoniacal liquor.
3, according to the described water soluble alkyd resin solution of claim 1, its characteristic is that described solubility promoter is selected from one or more in ethylene glycol monobutyl ether, propylene glycol monobutyl ether or the butanols.
4, a kind of method for preparing each described water soluble alkyd resin solution of claim 1～3 is characterized in that comprising the steps:
(1) ricinolic acid of formula ratio, tetramethylolmethane and phthalic anhydride are mixed, stir and add dimethylbenzene down, and be warming up to 180～210 ℃ and carry out esterification, stopped reaction when acid number is reduced to 30-40 mgKOH/g;
(2) after above-mentioned reaction stops, being cooled to 140～160 ℃, adding the trimellitic acid 1,2-anhydride of formula ratio, be warming up to 170～200 ℃ more gradually and carry out esterification, dropping to 60～70mgKOH/g to acid number is reaction end;
(3) step 2 is behind reaction end, and vacuum filtration is removed solvent xylene, is cooled to 50～60 ℃, adds solubility promoter, the neutralizing agent of formula ratio, transfers pH to 7～8, after the water that adds formula ratio again disperses, obtains water soluble alkyd resin solution.
5, a kind of water soluble alkyd resin solution with claim 1 is made the water-soluble alcohol acid amine baking varnish of base-material, and its characteristic is that the prescription of water-soluble alcohol acid amine baking varnish comprises following raw material:
6, water-soluble alcohol acid amine baking varnish according to claim 5, its characteristic are that described aminoresin is water soluble amino resin.
7, water-soluble alcohol acid amine baking varnish according to claim 5, its characteristic are that described pigment is selected from one or more in chrome yellow, Tai Dark-red indigo plant, lemon yellow, molybdenum red, titanium dioxide or the toluidine red.
8, water-soluble alcohol acid amine baking varnish according to claim 5, its characteristic is that described auxiliary agent is selected from one or more in water-soluble wetting dispersing agent, defoamer or the flow agent.
9, a kind of method for preparing each described water-soluble alcohol acid amine baking varnish of claim 5～8 is characterized in that comprising the steps:
(1) the water soluble alkyd resin solution of the water of formula ratio, auxiliary agent and 30～50% is mixed after, add the pigment of formula ratio, stirring obtains slurry;
(2) with slurry, being ground to fineness is 10～15 microns, gets mill base;
(3) in mill base, add after remainder water dissolubility alkyd resin solution stirs, add the aminoresin of formula ratio, stir, filter the water-soluble alcohol acid amine baking varnish.
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|---|---|---|---|
| CNB2007100223300A CN100526362C (en) | 2007-05-14 | 2007-05-14 | Water-soluble alcohol-acid resin solution and water-soluble alcohol-acid amino baking paint and preparing method |
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| CN106047104A (en) * | 2016-06-30 | 2016-10-26 | 太仓市金新涂料有限公司 | Environment-friendly alcohol acid amino baking paint and preparation method thereof |
| CN106047023A (en) * | 2016-07-01 | 2016-10-26 | 太仓市金新涂料有限公司 | Environment-friendly flame-retardant modified alkyd amino-baking coating and preparation method thereof |
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| CN100526362C (en) | 2009-08-12 |
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