CN1091449A - Low-temperature quick-dry amine baking varnish and preparation thereof - Google Patents
Low-temperature quick-dry amine baking varnish and preparation thereof Download PDFInfo
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- CN1091449A CN1091449A CN 93101411 CN93101411A CN1091449A CN 1091449 A CN1091449 A CN 1091449A CN 93101411 CN93101411 CN 93101411 CN 93101411 A CN93101411 A CN 93101411A CN 1091449 A CN1091449 A CN 1091449A
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- solidifying agent
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- synolac
- baking varnish
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Abstract
A kind of low-temperature quick-dry amine baking varnish with Synolac and aminoresin and solidifying agent preparation, it is characterized in that aminoresin is with the alcohols modified melamine-formaldehyde resin time, be modified as the best with isopropylcarbinol, Synolac: isopropylcarbinol modified melamine-formaldehyde resin: the weight ratio of solidifying agent=1: 3.8-4.2: 0.04-0.12, especially with 1: 3.8-4.2: 0.08 is the best.This lacquer is under GB1727-79 defined terms, and paint film only needs to toast complete drying within 10 minutes at 100 ℃, and gloss can reach more than 95%, and paint film is plentiful level and smooth, and light is hard, and this product has good physicochemical performance, decorate properties and stability in storage.
Description
Low-temperature quick-dry amine baking varnish of the present invention belongs to a kind of coating composition, is after being added the isopropylcarbinol modified melamine-formaldehyde resin and added an amount of solidifying agent after disperseing by Synolac and pigment, forms through the thinner allotment.
Aminoresin is since entering coating industry; the amino-alkyd baking finiss that makes via the Synolac modification, no matter from decorative effect, barrier propterty; still on use cost, all have other lacquer kind of incomparable superiority, do to decorate protection so be widely used in the mechanicals of higher class.But traditional amino-alkyd baking finiss need be at higher temperature condition (120-130 ℃) and long time (90-120 minute) ability crosslinking curing.Chinese patent CN1031097A discloses a kind of super quick-setting amino baking finish, by changing Synolac structure in the amine baking varnish, makes that reactive group increases in the Synolac molecule, and more functional group reactions increased activity has shortened time of drying.But very easily become glue in manufacturing processed, stability in storage and paint film brightness are all not ideal enough.In addition, invent desired compound method and step according to this, those skilled in the art do not go out the paint of this invention, because the method for this technology is impracticable.
The purpose of this invention is to provide a kind of amine baking varnish, under cold condition, paint film can be dry rapidly, do not become glue in the manufacturing processed, improves the stability in storage of lacquer and the brightness of paint film.
The object of the present invention is achieved like this: a kind of low-temperature quick-dry amine baking varnish with Synolac and aminoresin and solidifying agent preparation, pigment (or filler) is mixed with Synolac and stir, add aminoresin and solidifying agent through grinding, use dimethylbenzene at last, butanol mixed liquid adjustment lacquer fluid viscosity (is coated with 4 flow cups to 55-65 second, survey in the time of 25 ℃), it is characterized in that aminoresin is with the alcohols modified melamine-formaldehyde resin time, be modified as the best with isopropylcarbinol, Synolac: isobutyl modified melamine-formaldehyde resin: the weight ratio of solidifying agent=1: 3.8-4.2: 0.04-0.12, especially with 1: 3.8-4.2: 0.08 is the best.The Synolac of the present invention preparation is a kind of hyperergy Synolac, and the molecular weight in this molecular resin, acid number, hydroxyl value are controlled, and active group increases, and activation energy reduces, and can lure that the rapid open chain of aminoresin is crosslinked into; The aminoresin of preparation is a kind of hyperergy isopropylcarbinol modified melamine-formaldehyde resin, makes it to obtain optimum matching with the active group of hyperergy Synolac; Preparing a kind of solidifying agent simultaneously can make above-mentioned two kinds of hyperergy resins further reduce the required energy of curing cross-linking reaction, promptly by amino-alkyd baking finiss is carried out the structural modification of three aspects, make it to obtain minimum energy and can make maximum active groups participate in crosslinking curing from the external world.Macro manifestations is, under cold condition, drying varniss is rapid, guarantees and improves the quality level that former lacquer has.
One, preparation hyperergy isopropylcarbinol modified melamine-formaldehyde resin
1, formaldehyde, isopropylcarbinol, trimeric cyanamide, magnesiumcarbonate are thrown in the reactor, be warming up to 90-92 ℃, postcooling cooling in 3 hours refluxes;
2, add phthalic anhydride, treat that phthalic anhydride all dissolves, survey pH value and be advisable at 4.4-4.8;
3, heat up, continue to reflux 2 hours, add dimethylbenzene, leave standstill branch water, emit water;
4, controlled temperature is 55 ℃, and vacuum tightness is below the 600mmHg, decompression dehydration;
5, after water takes off to the greatest extent, add isopropylcarbinol, tolerance 3.5-6 is surveyed in sampling, and benzene is clear, is terminal point to reaching requirement, steams excessive isopropylcarbinol, adjusts viscosity 70-90 second, solid composition 58-62%.
Embodiment 1
Material name specification weight percent
Trimeric cyanamide is more than 99.5% 10.55
Formaldehyde 37% 42.36
Isopropylcarbinol industry 42.70
Magnesiumcarbonate analytical pure 0.05
Phthalate anhydride is more than 99.2% 0.07
Dimethylbenzene industry 4.27
When tolerance reaches 3.5-6, viscosity 70-90 second, when containing solid and reaching 58-62%, the isopropylcarbinol modified melamine-formaldehyde resin contains a large amount of active groups
NH ,-CH
2OH can be complementary with a large amount of active group-OH in the hyperergy Synolac.
Two, preparation hyperergy Synolac
1, soya-bean oil and glycerine are added in the still, stir, be warmed up to 120 ℃, stop to stir, the yellow lead powder evenly is sprinkling upon liquid level, continue to heat up and stir, about 1 hour, be warmed up to 230 ± 2 ℃, the insulation alcoholysis;
2, after 45 minutes, it is qualified that sampling survey alcoholysis (sample: 95% ethanol=1: 9, volume ratio, 25 ℃) is when transparent, cooling;
3, add three kinds of acid 210 ℃ the time in still; Add the back temperature and be not less than 180 ℃;
4,180 ℃ feed backflow dimethylbenzene, keep esterification after 1 hour, delay to be warmed up to 190 ± 2 ℃;
5, keep after 2 hours, sampling viscosimetric (portions of resin dimethylbenzene=1: 1 weight ratio, the Ge Shi pipe is surveyed in the time of 25 ℃) treats that viscosity reaches 3-3.5 second, is the resin reaction terminal point.
Embodiment 2
Material name specification weight percent
Soya-bean oil refining 32.62
Glycerine 100% 22.42
Silicone oil 100% 0.0004
Yellow lead 98% 0.013
Phenylformic acid 100% 3.970
Phthalic anhydride is more than 99.2% 38.91
Trimellitic anhydride 100% 2.080
Embodiment 3
Material name specification weight percent
Soya-bean oil refining 30.27
Glycerine 100% 23.66
Silicone oil 100% 0.0004
Yellow lead 98% 0.013
Phenylformic acid 100% 4.087
Phthalic anhydride is more than 99.2% 39.84
Trimellitic anhydride 100% 2.143
Embodiment 4
Material name specification weight percent
Soya-bean oil refining 33.92
Glycerine 100% 22.42
Silicone oil 100% 0.0004
Yellow lead 98% 0.013
Phenylformic acid 100% 3.505
Phthalic anhydride is more than 99.2% 38.87
Trimellitic anhydride 100% 1.285
When oil content controls to 32.8-34.5%, pure excess is 20.3-22.6%, and acid number is not more than 15mgKOH/g, when viscosity is 3-3.5 second (the Ge Shi pipe is surveyed in the time of 25 ℃), an optimum matching can be arranged with the active group of isopropylcarbinol modified melamine-formaldehyde resin.
Three, preparation acid curing agent
1, solidifying agent is prepared by isobutyl ester, ethylene glycol, tosic acid, pyridine, and it consists of isobutyl ester 46-56%, ethylene glycol 15-19%, tosic acid 18-22%, pyridine 8-10%;
2, isobutyl ester and ethylene glycol solvent (by proportioning) are thrown into reactor, heat up, stir;
When 3, temperature was raised to 30 ℃, (by proportioning) added tosic acid, is warmed up to 40 ± 2 ℃ then, insulation esterification, dissolving;
4, after dissolving finishes, slowly add pyridine, controlled temperature is no more than 60 ℃, stirs 30 minutes;
5, cooling when sampling survey acid content reaches 22-25% in the time of 30 ℃, is terminal point.
Embodiment 5
Material name specification weight percent
Isobutyl ester industry 52.24
Ethylene glycol industry 17.71
Tosic acid industry 20.60
Pyridine analytical pure 9.45
Use solidifying agent, can impel the crosslinking curing of amino-alkyd baking finiss, if improper but solidifying agent is selected, add-on is improper, will make solidified nature poor, the low or quick solidifying of hardness, hardness height, but paint film embrittlement, also can make the object corrosion in addition, water tolerance reduces, and is difficult for storing.When than the 0.96g/cm that weighs
3, acid content reaches at 22% o'clock, best results.
Four, the preparation of low-temperature quick-dry amine baking varnish
Add Synolac, isopropylcarbinol modified melamine-formaldehyde resin and solidifying agent during the preparation amine baking varnish, form with the thinner allotment, Synolac: hyperergy isopropylcarbinol modified melamine-formaldehyde resin: the weight ratio of solidifying agent=1: 3.8-4.2: 0.04-0.12, especially with 1: 3.8-4.2: 0.08 is the best.
During preparation, pigment (or filler) mixed with the Synolac of hyperergy and stir be ground to the fineness of regulation after, add hyperergy isopropylcarbinol modified melamine-formaldehyde resin and solidifying agent, become amino-alkyd baking finiss with dimethylbenzene, butanol mixed liquid adjustment lacquer fluid viscosity to 55-65 second (be coated with 4 flow cups, survey in the time of 25 ℃) at last with low-temperature quick-dry characteristic.
Amino-alkyd baking finiss of the present invention has adopted through the hyperergy Synolac of adjusting the intramolecule structure and the hyperergy isopropylcarbinol modified melamine-formaldehyde resin that adapts with it, and snugly has used solidifying agent, this combination amino-alkyd baking finiss is being obtained under the more low-energy condition, a large amount of unsaturated link(age)s in two kinds of hyperergy resins are under the katalysis of solidifying agent, very participate in cross-linking and curing reaction effectively, show characteristic fast dried, energy-conservation and the raising work efficiency.Under the GB1727-79 defined terms, paint film only needs to toast complete drying within 10 minutes at 100 ℃, and gloss can reach more than 95%, hardness (double pendulum instrument) is more than 0.55, and paint film is plentiful level and smooth, lovely luster, light is hard, has good physicochemical performance, decorate properties and stability in storage.
Colored paint embodiment
Embodiment 6 Mitsubishi's whites
Material name specification weight percent
Hyperergy Synolac 50% 61.94
Hyperergy aminoresin 60% 16.30
Titanium dioxide R-930 19.50
Deep chrome yellow qualified 0.16
Carbon black soft 0.02
Red iron oxide qualified 0.02
Anti-tangerine peel agent F400 0.22
Solidifying agent 22% 1.0
Thinner X-4 0.84
Embodiment 7 black
Material name specification weight percent
Hyperergy Synolac 50% 76.8
Hyperergy aminoresin 60% 18.3
Carbon black Fw-200 2.7
Solidifying agent 22% 1.5
Thinner X-4 0.7
Claims (6)
1, a kind of low-temperature quick-dry amine baking varnish with Synolac and aminoresin and solidifying agent preparation, pigment (or filler) is mixed with Synolac and stir, add aminoresin and solidifying agent through grinding, use dimethylbenzene at last, butanol mixed liquid adjustment lacquer fluid viscosity (is coated with 4 flow cups to 55-65 second, survey in the time of 25 ℃), it is characterized in that aminoresin is when selecting the alcohols modified melamine-formaldehyde resin for use, be modified as the best with isopropylcarbinol, Synolac: isopropylcarbinol modified melamine-formaldehyde resin: the weight ratio of solidifying agent=1: 3.8-4.2: 0.04-0.12, especially with 1: 3.8-4.2: 0.08 is the best.
2, low-temperature quick-dry amine baking varnish according to claim 1, the preferred values that it is characterized in that the isopropylcarbinol modified melamine-formaldehyde resin is tolerance 3.5-6, viscosity 70-90 second, contains solid 58-62%.
3, low-temperature quick-dry amine baking varnish according to claim 1 and 2, the oil content that it is characterized in that Synolac is 32.8-34.5%, and pure excess is 20.3-22.6%, and acid number is not more than 15mgKOH/g, and viscosity is 3-3.5 second (the Ge Shi pipe is surveyed in the time of 25 ℃).
4, low-temperature quick-dry amine baking varnish according to claim 1 and 2, it is characterized in that solidifying agent is prepared by isobutyl ester, ethylene glycol, tosic acid and pyridine, it consists of (weight content): isobutyl ester 46-56%, ethylene glycol 15-19%, tosic acid 18-22%, pyridine 8-10%.
5, low-temperature quick-dry amine baking varnish according to claim 4, the optimum value that it is characterized in that solidifying agent is proportion 0.96g/cm
3, acid content 22%.
6, low-temperature quick-dry amine baking varnish according to claim 4 is characterized in that the preparation process of solidifying agent is as follows:
A. isobutyl ester and ethylene glycol solvent are thrown in the reactor, heated up, stir;
When b. temperature is raised to 30 ℃, add tosic acid, when being warmed up to 40 ± 2 ℃ then, insulation esterification, dissolving;
C. after dissolving finishes, slowly add pyridine, controlled temperature is no more than 60 ℃, stirs 30 minutes;
D. cooling when sampling survey acid content reaches 22-25% in the time of 30 ℃, is terminal point.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93101411 CN1091449A (en) | 1993-02-15 | 1993-02-15 | Low-temperature quick-dry amine baking varnish and preparation thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93101411 CN1091449A (en) | 1993-02-15 | 1993-02-15 | Low-temperature quick-dry amine baking varnish and preparation thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1091449A true CN1091449A (en) | 1994-08-31 |
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ID=4983571
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93101411 Pending CN1091449A (en) | 1993-02-15 | 1993-02-15 | Low-temperature quick-dry amine baking varnish and preparation thereof |
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| CN (1) | CN1091449A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343501B (en) * | 2008-08-12 | 2010-06-23 | 无锡市虎皇漆业有限公司 | Quick-drying amino-stoving varnish and preparation thereof |
| CN102388108A (en) * | 2009-03-31 | 2012-03-21 | Ppg工业俄亥俄公司 | Electrocoating composition comprising a crater control additive |
| CN105440878A (en) * | 2015-12-22 | 2016-03-30 | 芜湖恒坤汽车部件有限公司 | Rapid-drying coating material composition and rapid-drying coating material preparation method |
-
1993
- 1993-02-15 CN CN 93101411 patent/CN1091449A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343501B (en) * | 2008-08-12 | 2010-06-23 | 无锡市虎皇漆业有限公司 | Quick-drying amino-stoving varnish and preparation thereof |
| CN102388108A (en) * | 2009-03-31 | 2012-03-21 | Ppg工业俄亥俄公司 | Electrocoating composition comprising a crater control additive |
| CN105440878A (en) * | 2015-12-22 | 2016-03-30 | 芜湖恒坤汽车部件有限公司 | Rapid-drying coating material composition and rapid-drying coating material preparation method |
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| PB01 | Publication | ||
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |