CN107603431B - A kind of amino-stoving varnish multi-functional promotor and preparation method thereof - Google Patents
A kind of amino-stoving varnish multi-functional promotor and preparation method thereof Download PDFInfo
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- CN107603431B CN107603431B CN201710854360.1A CN201710854360A CN107603431B CN 107603431 B CN107603431 B CN 107603431B CN 201710854360 A CN201710854360 A CN 201710854360A CN 107603431 B CN107603431 B CN 107603431B
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Abstract
The invention discloses a kind of multi-functional promotors of amino-stoving varnish, are mainly prepared from the following raw materials: epoxy resin, phosphate compound, glycidol aliphatic compound and organic solvent.The promotor good water solubility, it is compatible with resin good, coating wetability can be promoted, it can accelerate resin and amino resins curing reaction, it can also be with amino resin crosslinked, coating solvent resistance, adhesive force are improved, which can also form one layer of fine and close phosphating coat with metal base, enhance water-resistant coating and anti-sudden strain of a muscle erosion ability.The invention also discloses the above-mentioned amino-stoving varnish preparation methods of multi-functional promotor.
Description
Technical field
The invention belongs to technical field of coatings, and in particular to a kind of amino-stoving varnish multi-functional promotor and its preparation side
Method.
Background technique
Baking vanish used additives function is mostly single on the market at present, and a complete paint is up to standard in order to comprehensive performance, usually
Multiple functions auxiliary agent can be introduced such as in formula: agent, these auxiliary agents are lost in adhesion promoter, acid catalyst, adhesive agent, anti-sudden strain of a muscle
Type uses more, and coating cost is higher, and the stability of coating can also decline therewith, and increases the complexity of formula, makes
It is cumbersome easy because human factor leads to leakage plus miss to add raw material to obtain coating producing process.
In view of the above problems, certain commercial value will be had by developing a kind of auxiliary agent of multi-functional a few unification effects, simplifies and apply
Expect preparation process, reduces coating preparation cost.
Summary of the invention
The purpose of the present invention is to provide a kind of multi-functional promotor of amino-stoving varnish, the promotor good water solubilities, with tree
Lipid phase is held, and coating wetability can be promoted, and can accelerate resin and amino resins curing reaction, moreover it is possible to amino resin crosslinked, mention
High coating solvent resistance, adhesive force, the auxiliary agent can also form one layer of fine and close phosphating coat with metal base, make water-resistant coating
Enhance with anti-sudden strain of a muscle erosion ability.
The object of the invention is also to provide the above-mentioned amino-stoving varnish preparation method of multi-functional promotor, the preparation methods
Simple process, it is cheap.
The first purpose of this invention is achieved through the following technical solutions: a kind of multi-functional promotion of amino-stoving varnish
Agent is mainly prepared from the following raw materials: epoxy resin, phosphate compound, glycidol aliphatic compound and organic solvent.
Phosphoric acid modification epoxy resin has many documents and materials reports in last century, mostly uses as matrix resin, benefit
It is used in the painting of the tank Room with the high-hardness corrosion-resistant characteristic of epoxy resin to load onto, however there is no such products applications seen in market.It is existing
Epoxy phosphate ester is carried out acrylic resin modified or polyurethane mostly, corrosion-resistant field is used in, is directly used as auxiliary agent and is rarely reported.
Because epoxy phosphate ester be used in water paint in stabilizations be not very well, it is bad with matrix resin compatibility, easily lead to coating be layered,
So being not very extensively as auxiliary agent application.
And the present invention introduces ethylene oxidic ester class aliphatic compound in the technology of preparing of existing epoxy phosphate ester, to change
The steady dissolution of kind epoxy phosphate ester, reduces molecular structure surface tension, enhances formulation for coating material wetability.
Further, amino-stoving varnish of the present invention is in multi-functional promotor: the epoxy resin, phosphate compound and
The proportion by weight of glycidol aliphatic compound are as follows: epoxy resin 140~160, phosphate compound 20~70, shrink are sweet
Oil and fat compounds of group 20~70.
The wherein dosage energy dissolved epoxy of the organic solvent, it is excellent with the proportion by weight of epoxy resin
It is selected as epoxy resin 140~160, organic solvent 90~125.
In each raw material of the above-mentioned amino-stoving varnish with multi-functional promotor:
It is 0.2~0.6mol/100g epoxy resin that epoxy resin of the present invention, which is preferably epoxide number,.
More preferably, epoxy resin of the present invention is E-20 epoxy resin, E44 epoxy resin or E-55 epoxy resin.
Phosphate compound of the present invention preferably includes phosphoric acid and polyphosphoric acid, pyrophosphoric acid or phosphorus pentoxide hydrolysis
The chemicals of phosphoric acid can be generated afterwards.
Glycidol aliphatic compound of the present invention can be with sour reactive grafting preferably with epoxy-functional
Aliphatic compound.
More preferably, the epoxy-functional of the present invention that has can be versatic acid with the aliphatic compound of sour reactive grafting
Ethylene oxidic ester (E10P), ethylene oxidic ester stearic acid or lauryl diglycidyl ether.
Organic solvent of the present invention is preferably anti-plain boiled water, propylene glycol monomethyl ether or propylene glycol methyl ether acetate.
Second object of the present invention is achieved through the following technical solutions: the multi-functional rush of above-mentioned amino-stoving varnish
Into the preparation method of agent, comprising the following steps:
(1) it chooses epoxy resin and organic solvent is placed in container, stirring is complete to epoxy resin dissolution, then in ice water
Stirring is cooled to temperature of charge lower than 5 DEG C in bath；
(2) addition phosphate compound, which continues stirring, mixes material；
(3) bath temperature is adjusted to 20~25 DEG C of heat preservations, and material in container starts reaction and releases a large amount of tropical animal material temperatures
Degree rises；
(4) 70~90 DEG C are gradually warming up to after temperature of charge is stablized, faint yellow clear shape is presented in material；
(5) glycidol aliphatic compound is added, keeps the temperature 50~70min, reactant is taken to test acid value, controls product acid
Value is that 60~120mgKOH/g discharges to get the multi-functional promotor of amino-stoving varnish.
The principle of the present invention is: the present invention is to use phosphoric acid modification epoxy resin, and be aided with glycidol aliphatic compound.
P-OH group in phosphoric acid molecules structure can be formed with metal base and, phosphatization substrate, increase adhesive force, acid catalysis accelerate resin
With the curing reaction of amino resins, epoxy resin can promote the solvent resistance of film, and the hydroxyl in strand can also be with
Amino resins reaction increase film crosslink density, ethylene oxidic ester class formation enhance the auxiliary agent steady dissolution and with resin
Compatibility, to the wetability of substrate.
Compared with prior art, the invention has the following advantages:
(1) the multi-functional promotor of amino-stoving varnish in the present invention, raw material is cheap and easy to get, synthesis technology handy and safe；
(2) the multi-functional promotor of amino-stoving varnish in the present invention, product, applies in addition to having to be promoted compared with the existing technology
The characteristics of layer adhesive force, also have the characteristics that resin compatible is good；
(3) the multi-functional promotor of amino-stoving varnish in the present invention, compared with the existing technology product, moreover it is possible to further increase
Coating wetability improves coating crosslink density, is obviously improved coating organic solvent-resistant wiping properties, can accelerate resin and amino tree
Rouge curing reaction, moreover it is possible to which, with amino resin crosslinked, raising coating solvent resistance, adhesive force, are a kind of suitable for amino-stoving varnish
Multi-functional promotor has the effect of multi-functional a few unifications；
(4) amino-stoving varnish in the present invention can also form one layer of fine and close phosphatization with metal base with multi-functional promotor
Film enhances water-resistant coating and anti-sudden strain of a muscle erosion ability, the particularly suitable amino-stoving varnish for making substrate with metal；
(5) amino-stoving varnish in the present invention can be neutralized into alkalescent with amine with multi-functional promotor and be dissolved in water, be used in water
In property coating.
Specific embodiment
For a further understanding of the present invention, illustrate below in conjunction with specific embodiment, following each embodiments are merely to illustrate
Of the invention rather than limitation of the present invention.
In following embodiment, the raw material of use is marketable material unless otherwise specified.
Embodiment 1
The multi-functional promotor of amino-stoving varnish provided in this embodiment, is mainly made of the raw material of following proportion by weight:
Epoxy resin 150, phosphate compound 25.9, glycidol aliphatic compound 57.6, consumption of organic solvent are can dissolve ring
Oxygen resin is advisable, and is herein 98.
It is 0.2~0.6mol/100g epoxy resin, specially E-20 epoxy resin that wherein epoxy resin, which is epoxide number,.
Phosphate compound is the phosphoric acid that mass percentage is 85%.
Glycidol aliphatic compound is can be with the aliphatic compound of sour reactive grafting, specifically with epoxy-functional
For tertiary carbonic acid glycidyl ester.
Organic solvent is anti-plain boiled water.
The preparation method of the multi-functional promotor of the amino-stoving varnish, comprising the following steps:
(1) 150 parts of E-20 epoxy resin are taken, 98 parts of anti-plain boiled water is added in four-hole bottle, and starting stirring fills epoxy resin
Divide dissolution in a solvent, four-hole bottle is placed in stirring in ice-water bath and is cooled to temperature of charge lower than 5 DEG C；
(2) when temperature of charge be lower than 5 DEG C when be added 25.9 parts of 85% phosphoric acid continue stir half an hour mix material；
(3) bath temperature is slowly increased to keep the temperature to 20 DEG C, in bottle material start reaction release heat drive temperature of charge after
It is continuous to rise；
(4) bath temperature is stepped up to 90 DEG C after temperature stabilization in bottle, material is faint yellow in clear shape in bottle
Liquid；
(5) 57.6 parts of tertiary carbonic acid glycidyl ester monomer are added, stirring keeps the temperature 1 hour, sampling and testing acid value, and acid value is
70mgKOH/g, discharging, obtains amino-stoving varnish with multi-functional promotor.
Embodiment 2
The multi-functional promotor of amino-stoving varnish provided in this embodiment, is mainly made of the raw material of following proportion by weight:
Epoxy resin 150, phosphate compound 50.7, glycidol aliphatic compound 26.4, consumption of organic solvent are can dissolve ring
Oxygen resin is advisable, and is herein 110.
It is 0.2~0.6mol/100g epoxy resin, specially E-44 epoxy resin that wherein epoxy resin, which is epoxide number,.
Phosphate compound is the phosphoric acid that mass percentage is 85%.
Glycidol aliphatic compound is can be with the aliphatic compound of sour reactive grafting, specifically with epoxy-functional
For tertiary carbonic acid glycidyl ester.
Organic solvent is anti-plain boiled water.
The preparation method of the multi-functional promotor of the amino-stoving varnish, comprising the following steps:
(1) 150 parts of E-44 epoxy resin are taken, 110 parts of anti-plain boiled water is added in four-hole bottle, and starting stirring fills epoxy resin
Divide dissolution in a solvent, four-hole bottle is placed in stirring in ice-water bath and is cooled to temperature of charge lower than 5 DEG C；
(2) when temperature of charge be lower than 5 DEG C when be added 50.7 parts of 85% phosphoric acid continue stir half an hour mix material；
(3) bath temperature is slowly increased to keep the temperature to 20 DEG C, in bottle material start reaction release heat drive temperature of charge after
It is continuous to rise；
(4) bath temperature is stepped up to 90 DEG C after temperature stabilization in bottle, material is faint yellow in clear shape in bottle
Liquid；
(5) 26.4 parts of tertiary carbonic acid glycidyl ester monomer are added, stirring keeps the temperature 1 hour, sampling and testing acid value, and acid value is
100mgKOH/g, discharging, obtains amino-stoving varnish with multi-functional promotor.
Embodiment 3
The multi-functional promotor of amino-stoving varnish provided in this embodiment, is mainly made of the raw material of following proportion by weight:
Epoxy resin 150, phosphate compound 63.4, glycidol aliphatic compound 33, consumption of organic solvent are can dissolve epoxy
Resin is advisable, and is herein 118.
It is 0.2~0.6mol/100g epoxy resin, specially E-55 epoxy resin that wherein epoxy resin, which is epoxide number,.
Phosphate compound is the phosphoric acid that mass percentage is 85%.
Glycidol aliphatic compound is can be with the aliphatic compound of sour reactive grafting, specifically with epoxy-functional
For tertiary carbonic acid glycidyl ester.
Organic solvent is anti-plain boiled water.
The preparation method of the multi-functional promotor of the amino-stoving varnish, comprising the following steps:
(1) 150 parts of E-55 epoxy resin are taken, 118 parts of anti-plain boiled water is added in four-hole bottle, and starting stirring fills epoxy resin
Divide dissolution in a solvent, four-hole bottle is placed in stirring in ice-water bath and is cooled to temperature of charge lower than 5 DEG C；
(2) when temperature of charge be lower than 5 DEG C when be added 63.4 parts of 85% phosphoric acid continue stir half an hour mix material；
(3) bath temperature is slowly increased to keep the temperature to 20 DEG C, in bottle material start reaction release heat drive temperature of charge after
It is continuous to rise；
(4) bath temperature is stepped up to 90 DEG C after temperature stabilization in bottle, material is faint yellow in clear shape in bottle
Liquid；
(5) 33 parts of tertiary carbonic acid glycidyl ester monomer are added, stirring keeps the temperature 1 hour, sampling and testing acid value, and acid value is
110mgKOH/g, discharging, obtains amino-stoving varnish with multi-functional promotor.
Embodiment 4
The multi-functional promotor of amino-stoving varnish provided in this embodiment, is mainly made of the raw material of following proportion by weight:
Epoxy resin 140, phosphate compound 70, glycidol aliphatic compound 20, consumption of organic solvent is can dissolve asphalt mixtures modified by epoxy resin
Rouge is advisable.
It is 0.2~0.6mol/100g epoxy resin, specially E-55 epoxy resin that wherein epoxy resin, which is epoxide number,.
Phosphate compound is polyphosphoric acid.
Glycidol aliphatic compound is can be with the aliphatic compound of sour reactive grafting, specifically with epoxy-functional
For ethylene oxidic ester stearic acid.
Organic solvent is propylene glycol monomethyl ether.
The amino-stoving varnish with the preparation method of multi-functional promotor other than raw material and raw material dosage are slightly different, it is more
Phosphoric acid is first dissolved in advance in the water of part, the other the same as in Example 1.
Embodiment 5
The multi-functional promotor of amino-stoving varnish provided in this embodiment, is mainly made of the raw material of following proportion by weight:
Epoxy resin 160, phosphate compound 20, glycidol aliphatic compound 70, organic solvent dosage epoxy can be dissolved
Resin is advisable.
It is 0.2~0.6mol/100g epoxy resin, specially E-44 epoxy resin that wherein epoxy resin, which is epoxide number,.
Phosphate compound is pyrophosphoric acid.
Glycidol aliphatic compound is can be with the aliphatic compound of sour reactive grafting, specifically with epoxy-functional
For lauryl diglycidyl ether.
Organic solvent is propylene glycol methyl ether acetate.
The amino-stoving varnish with the preparation method of multi-functional promotor other than raw material and raw material dosage are slightly different, it is burnt
Phosphoric acid is first dissolved in advance in the water of part, the other the same as in Example 1.
Application of the amino-stoving varnish of the present invention of table 1 with multi-functional promotor in painting formula
Remarks: the promotor in painting formula 2~6 is respectively the multi-functional promotor that Examples 1 to 5 obtains.
Paint sample 1~6 is coated on sheet metal, baking oven high temperature is put into and bakes, obtain solidify coating.To solidify coating according to
Standard testing performance.The test method of adhesive force is: GB/T 6739-2006, adhesion test method are: GB/T1720-
1979, boiling test method is: GB/T5237-2004.
Test result is as follows table 2:
Table 2 adds the properties of the paint sample of promotor of the present invention
If the basic performance for not adding accelerant coatings is very poor it can be seen from upper table 2, it is difficult to meet the standard of using.
Properties of coating can be obviously improved by being added to 1.5% promotor of the present invention, be primarily due to promotor of the present invention first
It has been catalyzed the curing reaction of resin Yu full etherified amino, has kept the solidification of coating more abundant；Followed by epoxy phosphate structure and gold
Belong to substrate and forms and enhance coating adhesion；Hydroxyl in last promotor molecular structure takes part in curing reaction and improves coating crosslinking
Density, further strengthened coat various aspects of performance.
Due to ethylene oxidic ester class formation can enhance multi-functional promotor steady dissolution and with the compatibility of resin, with
And the wetability to substrate.So the amino-stoving varnish in the present invention stored for a long time with multi-functional promotor it is Clear & Transparent, it is constant
Muddiness, it is as clear as crystal to prepare varnish sample, and storage is not muddy not stratified for a long time.
Each component cited by the present invention, and bound, the section value of each component of the present invention can realize the present invention,
Embodiment numerous to list herein.A part of specific embodiment is enumerated above, and the present invention will be described, it is necessary to it is pointed out here that
Be that specific embodiment is served only for that the present invention is further illustrated up and down, do not represent limiting the scope of the invention.
The some nonessential modifications and adjustment that other people make according to the present invention still fall within protection scope of the present invention.
Claims (7)
1. the multi-functional promotor of a kind of amino-stoving varnish, it is characterized in that being mainly prepared from the following raw materials: epoxy resin, phosphoric acid class
Close object, glycidol aliphatic compound and organic solvent；
The proportion by weight of the epoxy resin, phosphate compound and glycidol aliphatic compound are as follows: epoxy resin
140 ~ 160, phosphate compound 20 ~ 70, glycidol aliphatic compound 20 ~ 70；
The phosphate compound includes that can generate phosphoric acid after phosphoric acid and polyphosphoric acid, pyrophosphoric acid or phosphorus pentoxide hydrolysis
Compound；
The glycidol aliphatic compound is can be with the aliphatic compound of sour reactive grafting with epoxy-functional；
The acid value of the multi-functional promotor of the amino-stoving varnish is 60~120mgKOH/g.
2. the multi-functional promotor of amino-stoving varnish according to claim 1, it is characterized in that: the dosage energy of the organic solvent
Dissolved epoxy.
3. the multi-functional promotor of amino-stoving varnish according to claim 1 or 2, it is characterized in that: the epoxy resin is
Epoxide number is 0.2 ~ 0.6mol/100g epoxy resin.
4. the multi-functional promotor of amino-stoving varnish according to claim 3, it is characterized in that: the epoxy resin is E-20
Epoxy resin, E44 epoxy resin or E-55 epoxy resin.
5. the multi-functional promotor of amino-stoving varnish according to claim 1, it is characterized in that: described has epoxy-functional
It can be that tertiary carbonic acid glycidyl ester, ethylene oxidic ester stearic acid or dodecyl shrink with the aliphatic compound of sour reactive grafting
Glycerin ether.
6. the multi-functional promotor of amino-stoving varnish according to claim 1 or 2, it is characterized in that: the organic solvent is
Anti- plain boiled water, propylene glycol monomethyl ether or propylene glycol methyl ether acetate.
7. the amino-stoving varnish of any of claims 1 or 2 preparation method of multi-functional promotor, it is characterized in that including following step
It is rapid:
(1) it chooses epoxy resin and organic solvent is placed in container, stirring is complete to epoxy resin dissolution, then in ice-water bath
Stirring is cooled to temperature of charge lower than 5 DEG C；
(2) addition phosphate compound, which continues stirring, mixes material；
(3) bath temperature is adjusted to 20 ~ 25 DEG C of heat preservations, and material in container starts reaction and releases big calorimetric, drives on temperature of charge
It rises；
(4) 70 ~ 90 DEG C are gradually warming up to after temperature of charge is stablized, faint yellow clear shape is presented in material；
(5) glycidol aliphatic compound is added, keeps the temperature 50 ~ 70min, reactant is taken to test acid value, control product acid value is
60~120mgKOH/g discharges to get the multi-functional promotor of amino-stoving varnish.
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| CN113025109A (en) * | 2021-04-12 | 2021-06-25 | 广东科鼎功能材料有限公司 | Water-oil universal adhesion promoter and preparation method thereof |
| CN113174158B (en) * | 2021-04-16 | 2023-04-07 | 虎皇新材料科技集团有限公司 | Modified epoxy phosphonate accelerant for coating and preparation method and application thereof |
| CN116218279B (en) * | 2023-03-31 | 2023-09-19 | 佛山市普加化工有限公司 | Silane modified acrylic ester phosphate adhesion promoter and application thereof |
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| JP2003292731A (en) * | 2002-03-29 | 2003-10-15 | Sumitomo Bakelite Co Ltd | Epoxy resin composition and semiconductor device |
| CN101429356A (en) * | 2008-12-18 | 2009-05-13 | 济南华临化工有限公司 | General adhesion promoter for paint and method of producing the same |
| CN105688743A (en) * | 2016-03-02 | 2016-06-22 | 济南华临化工有限公司 | Fluorine-silicon modified epoxy phosphate surfactant and preparation method thereof |
| CN106566363A (en) * | 2016-10-21 | 2017-04-19 | 广州擎天材料科技有限公司 | Disc-type electrostatic coating process for vehicle transmission shaft aqueous anticorrosion coating material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003292731A (en) * | 2002-03-29 | 2003-10-15 | Sumitomo Bakelite Co Ltd | Epoxy resin composition and semiconductor device |
| CN101429356A (en) * | 2008-12-18 | 2009-05-13 | 济南华临化工有限公司 | General adhesion promoter for paint and method of producing the same |
| CN105688743A (en) * | 2016-03-02 | 2016-06-22 | 济南华临化工有限公司 | Fluorine-silicon modified epoxy phosphate surfactant and preparation method thereof |
| CN106566363A (en) * | 2016-10-21 | 2017-04-19 | 广州擎天材料科技有限公司 | Disc-type electrostatic coating process for vehicle transmission shaft aqueous anticorrosion coating material |
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Address after: No.5 Lisha East Road, Shatian Town, Dongguan City, Guangdong Province 523000 Patentee after: Qingtian Material Technology Co., Ltd Address before: 510860, Yucai Road, Furong Town, Huadu District, Guangdong, Guangzhou 8, China Patentee before: GUANGZHOU KINTE INDUSTRIAL Co.,Ltd. |