CN110358412A - Oily cathode electrophoresis dope of a kind of contracting and preparation method thereof - Google Patents
Oily cathode electrophoresis dope of a kind of contracting and preparation method thereof Download PDFInfo
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- CN110358412A CN110358412A CN201910772031.1A CN201910772031A CN110358412A CN 110358412 A CN110358412 A CN 110358412A CN 201910772031 A CN201910772031 A CN 201910772031A CN 110358412 A CN110358412 A CN 110358412A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4473—Mixture of polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4488—Cathodic paints
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Paints Or Removers (AREA)
Abstract
This application discloses oily cathode electrophoresis dopes of a kind of contracting and preparation method thereof, and isocyanates, methyl iso-butyl ketone (MIBK) are added in reaction vessel, leads to nitrogen, stirs simultaneously, is heated；The end-sealed type dimethyl silicone polymer of the H containing activity is added dropwise into reaction vessel, is heated after being added dropwise, to first set reaction after, then cool down；Continue that butyl glycol ether, heating, to after reaction, cool down spare for the second time is added dropwise into reaction vessel；Epoxy resin is added into another reaction vessel, the above-mentioned material prepared is added in this reaction vessel, stirs, then heating is added acetic acid, neutralizes resin；Stop heating, pure water is added, is uniformly dispersed and prepares finished product.The oily electrophoretic coating of contracting of the invention has many advantages, such as the excellent oily effect of multiple lasting contracting and hardness, is provided simultaneously with good former paint stability and easily application.
Description
Technical field
The invention belongs to cathode electrophoresis dopes and preparation method technical field, and in particular to a kind of oily cathode electrophoresis dope of contracting
And preparation method thereof.
Background technique
Electrophoretic coating be the 1970s mid-term grow up and obtain a kind of new coating of industrial applications, it has
Have the advantages that environmental protection, throwing power are high, coating efficiency is high, coating quality is good and apply high degree of automation, as society is to energy conservation
The consciousness of environmental protection is increasingly enhanced, and related environmental regulation implements stringent limitation to volatile organic content, electrophoretic coating
Using also increasingly wider.
Epoxy type cathode electrophoresis dope has adhesiveness strong, high temperature resistant, and chemicals-resistant etc. a little, and is applied to kitchen ventilator
Flabellum has repeatedly the electrophoretic paint of lasting contracting oil fewer and fewer, and the oily electrophoretic paint of traditional contracting is the side by additional contracting oil assistant
Formula, makes conventional electrophoretic paint have the effect of contracting oil, and such contracting oil assistant is generally organic silicone oil and fluorinated low surface tension
Substance.But after this outer add mode electrophoresis paint film after the drying, auxiliary agent levelling to surface of the paint film, although having the oily effect that contracts,
It is not achieved repeatedly lasting effect, and with the extension of time, the characteristics of contracting oil assistant in former paint is due to its low surface tension,
Former paint surface can be floated on, cause the disadvantages such as paint film shrinkage cavity.It is limited in the development and application in kitchen ventilator field.Therefore, cathode
The modified contracting oil of epoxy electrophoretic coating has important research significance.
Summary of the invention
The purpose of the invention is to provide oily cathode electrophoresis dopes of a kind of contracting and preparation method thereof, solve above-mentioned existing skill
One or more in art problem.
A kind of contracting oil cathode electrophoresis dope of the invention includes: in parts by weight
30-100 parts of isocyanates；
5-35 parts of methyl iso-butyl ketone (MIBK)；
5-20 parts of the end-sealed type dimethyl silicone polymer of the H containing activity；
40-800 parts of butyl glycol ether；
200-450 parts of epoxy resin；
10-400 parts of acetic acid；
900-1500 parts of pure water.
In one embodiment: including: in parts by weight
65-70 parts of isocyanates；
10-15 parts of methyl iso-butyl ketone (MIBK)；
8-10 parts of the end-sealed type dimethyl silicone polymer of the H containing activity；
55-60 parts of butyl glycol ether；
300-350 parts of epoxy resin；
15-20 parts of acetic acid；
900-1000 parts of pure water.
In one embodiment: the end-sealed type dimethyl silicone polymer of the H containing activity includes that amino-terminated type is poly-
Dimethyl siloxane, carboxy blocking type dimethyl silicone polymer or alcoholic extract hydroxyl group end-sealed type dimethyl silicone polymer.
In one embodiment: the isocyanates is diisocyanate.
In one embodiment: the diisocyanate include toluene di-isocyanate(TDI), isophorone diisocyanate,
Methyl diphenylene diisocyanate, two isocyanide of dicyclohexyl methyl hydride diisocyanate, hexamethylene diisocyanate or lysine
Acid esters.
Further, it would be desirable to provide a kind of preparation methods for preparing above-mentioned contracting oil cathode electrophoresis dope: include the following steps,
Isocyanates, methyl iso-butyl ketone (MIBK) are added in reaction vessel, leads to nitrogen, stirs simultaneously, is heated；
The end-sealed type dimethyl silicone polymer of the H containing activity is added dropwise into reaction vessel, is heated after being added dropwise, to first
After secondary response, then cool down；
Continue that butyl glycol ether, heating, to after reaction, cool down spare for the second time is added dropwise into reaction vessel；
Epoxy resin is added into another reaction vessel, the above-mentioned material prepared is added in this reaction vessel, stirs,
Heating, is then added acetic acid, neutralizes resin；
Stop heating, pure water is added, is uniformly dispersed and prepares finished product.
In some embodiments, it is 255-275 ‰ that first set reaction, which is reaction to nco value,.
In some embodiments, it is < 1.5 ‰ that the second secondary response, which is reaction to nco value,.
The present invention, which provides a kind of oily cathode electrophoresis dope that contracts, to be changed using the end-sealed type dimethyl silicone polymer of the H containing activity
Property, the electrophoretic coating of the bulk cured dose of dimethyl silicone polymer comprising a kind of main chain bonding low surface tension.The H's containing activity
End-sealed type dimethyl silicone polymer not only has the advantages that the had low surface tension of silicone oil, easy to clean, with high hardness, while end
Also with the group of activity H, these structures impart the excellent oil rub resistance of end-sealed type dimethyl silicone polymer of the H containing activity
Performance and reactivity.The end-sealed type polydimethylsiloxane--modified isocyanate curing agent of the H containing activity, dimethyl silicone polymer
The activity group at both ends is reacted with NCO group, is connected in isocyanates, and then spent glycol butyl ether seals remaining NCO group entirely,
Epoxy resin and isocyanate-modified curing agent is sealed entirely sufficiently wrap up uniformly, after electrophoresis, the solidification of polydimethylsiloxane--modified
Agent is evenly affixed to coated article surface, after solidification, since dimethyl silicone polymer molecular weight is big, does not unseal under solidification temperature, institute
Can uniformly be present in paint film.Simultaneously because the low surface tension and lubricity of siloxanes, so that the paint film after solidifying has
There is the multiple oily effect of duration contracting.Also it solves the problems, such as siloxanes facile hydrolysis in aqueous electrophoretic paint, avoids paint film appearance
Shrinkage cavity and original paint unstable problem, to substantially increase the easy application in application end.
Specific embodiment
Embodiment 1
A kind of oily cathode electrophoresis dope of contracting includes: in parts by weight
30 parts of toluene di-isocyanate(TDI)；
5 parts of methyl iso-butyl ketone (MIBK)；
5 parts of carboxy blocking type dimethyl silicone polymer；
40 parts of butyl glycol ether；
200 parts of epoxy resin；
10 parts of acetic acid；
900 parts of pure water.
Further, it would be desirable to provide a kind of preparation methods for preparing above-mentioned contracting oil cathode electrophoresis dope: include the following steps,
Toluene di-isocyanate(TDI), methyl iso-butyl ketone (MIBK) are added in the reaction vessel with stirring and condensation, nitrogen, heating are led to
To 60 ± 2 DEG C, it is then slowly added dropwise carboxy blocking type dimethyl silicone polymer into reaction vessel, time for adding 30 ± 5 minutes,
Dropwise addition process maintains 60 ± 2 DEG C of temperature, and 80 ± 2 DEG C are warming up to after being added dropwise, and reacts ± 5 minutes 2 hours, until nco value is
255-275 ‰, is cooled to 60 ± 2 DEG C, continues that 55-60 parts by weight butyl glycol ether is added dropwise into reaction vessel, is warming up to 85 ± 2
DEG C, react ± 5 minutes 3 hours, until nco value < 1.5 ‰, be cooled to 55 ± 2 DEG C it is spare；
Epoxy resin is added into another reaction vessel, the above-mentioned material prepared is all added in this reaction vessel,
Stirring is warming up to 70 ± 2 DEG C, stirs 15 ± 2 minutes at this temperature, stirs two kinds of materials, vinegar is then added
Acid maintains 65 ± 2 DEG C to keep the temperature 15 ± 2 minutes, makes in resin and abundant；Heating system is closed, pure water is added, is uniformly dispersed and makes
Standby contracting oil cathode electrophoresis dope above-mentioned out.
Embodiment 2
A kind of oily cathode electrophoresis dope of contracting includes: in parts by weight
65-70 parts of isophorone diisocyanate；
10-15 parts of methyl iso-butyl ketone (MIBK)；
8-10 parts of amino-terminated type dimethyl silicone polymer；
55-60 parts of butyl glycol ether；
300-350 parts of epoxy resin；
15-20 parts of acetic acid；
900-1000 parts of pure water.
Preparation method is identical with preceding method.
Embodiment 3
A kind of oily cathode electrophoresis dope of contracting, includes: 68 parts of methyl diphenylene diisocyanate in parts by weight；
13 parts of methyl iso-butyl ketone (MIBK)；
9 parts of amino-terminated type dimethyl silicone polymer；
58 parts of butyl glycol ether；
325 parts of epoxy resin；
18 parts of acetic acid；
950 parts of pure water.
Preparation method is identical with preceding method.
Embodiment 4
A kind of oily cathode electrophoresis dope of contracting includes: in parts by weight
70 parts of dicyclohexyl methyl hydride diisocyanate；
15 parts of methyl iso-butyl ketone (MIBK)；
10 parts of carboxy blocking type dimethyl silicone polymer；
60 parts of butyl glycol ether；
350 parts of epoxy resin；
20 parts of acetic acid；
1000 parts of pure water.
Preparation method is identical with preceding method.
Embodiment 5
A kind of oily cathode electrophoresis dope of contracting includes: in parts by weight
100 parts of hexamethylene diisocyanate；
35 parts of methyl iso-butyl ketone (MIBK)；
20 parts of alcoholic extract hydroxyl group end-sealed type dimethyl silicone polymer；
800 parts of butyl glycol ether；
450 parts of epoxy resin；
400 parts of acetic acid；
1500 parts of pure water.
Preparation method is identical with preceding method.
The electrophoretic coating that above-described embodiment 1,3,5 obtains is mixed colored paint to help with unmodified electrophoretic coating and additional contracting oil
The identical colored paint of electrophoretic coating collocation of agent (BYK-3720), does circulation electrophoresis making sheet in 1 day and circulation rear electrophoresis making sheet in 5 days, film
Thickness is 18-22um, and 190 DEG C/15min-20min baking cools down, and test sample plate index, template indication range is as follows:
The oily test method of surface of the paint film contracting
1, instrument
Test sample plate, paper handkerchief have certain roughness paper, protective gloves.
2, reagent
Used edible oil (soybean oil)
3, checking procedure
3.1 edible oil test methods:
3.1.1 primary contracting is oily: an oil dripping of similar soya bean size is dripped in product surface of the paint film, and Product Level is placed, and is used
Finger pushes down surface of the paint film and rapidly scratches oil, and the phenomenon that building up is collapsed in observation, occurs shrinkage phenomenon, 10S contract in 2S
It is dotted at multiple light rain.
3.1.2 two contractings oil: after paper handkerchief wiped clean surface of the paint film oil, with there is certain roughness paper to be wiped repeatedly 10
Secondary, an oil dripping of similar soya bean size is dripped in product surface of the paint film, Product Level is placed, it is rapid to push down surface of the paint film with finger
Oil is scratched, the phenomenon that building up is collapsed in observation, occurs shrinkage phenomenon in 2S, 15S contract is dotted at multiple light rain.
3.1.3 contracting oil three times: after paper handkerchief wiped clean surface of the paint film oil, with there is certain roughness paper to be wiped repeatedly 10
Secondary, an oil dripping of similar soya bean size is dripped in product surface of the paint film, Product Level is placed, it is rapid to push down surface of the paint film with finger
Oil is scratched, the phenomenon that building up is collapsed in observation, occurs shrinkage phenomenon in 2S, 20S contract is dotted at multiple light rain.
4, points for attention
4.1 have certain roughness paper wiping surface firmly when guarantee wiping pressure is maintained between 500g-1000g.
To sum up, it is the end-sealed type poly dimethyl silicon using the H containing activity that the present invention, which provides a kind of oily cathode electrophoresis dope that contracts,
It is siloxane modified, the electrophoretic coating of the bulk cured dose of dimethyl silicone polymer comprising a kind of main chain bonding low surface tension.Containing work
The end-sealed type dimethyl silicone polymer for sprinkling property H not only has the advantages that the had low surface tension of silicone oil, easy to clean, with high hardness,
End also has the group of activity H simultaneously, and the end-sealed type dimethyl silicone polymer that these structures impart the H containing activity is excellent
Resistance to oily stain energy and reactivity.The end-sealed type polydimethylsiloxane--modified isocyanate curing agent of the H containing activity, poly- diformazan
The activity group at radical siloxane both ends is reacted with NCO group, is connected in isocyanates, and then spent glycol butyl ether seals residue entirely
NCO group, epoxy resin and seals isocyanate-modified curing agent entirely and sufficiently wraps up uniformly, and after electrophoresis, dimethyl silicone polymer changes
The curing agent of property is evenly affixed to coated article surface, after solidification, since dimethyl silicone polymer molecular weight is big, under solidification temperature not
Deblocking, so can uniformly be present in paint film.Simultaneously because the low surface tension and lubricity of siloxanes, so that after solidification
Paint film has the oily effect of multiple duration contracting.Also it solves the problems, such as siloxanes facile hydrolysis in aqueous electrophoretic paint, avoids paint
There is shrinkage cavity in film and original paints unstable problem, to substantially increase the easy application in application end.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of oily cathode electrophoresis dope of contracting, wherein include: in parts by weight
30-100 parts of isocyanates；
5-35 parts of methyl iso-butyl ketone (MIBK)；
5-20 parts of the end-sealed type dimethyl silicone polymer of the H containing activity；
40-800 parts of butyl glycol ether；
200-450 parts of epoxy resin；
10-400 parts of acetic acid；
900-1500 parts of pure water.
2. the oily cathode electrophoresis dope of a kind of contracting according to claim 1, wherein include: in parts by weight
65-70 parts of isocyanates；
10-15 parts of methyl iso-butyl ketone (MIBK)；
8-10 parts of the end-sealed type dimethyl silicone polymer of the H containing activity；
55-60 parts of butyl glycol ether；
300-350 parts of epoxy resin；
15-20 parts of acetic acid；
900-1000 parts of pure water.
3. according to claim 1 or a kind of oily cathode electrophoresis dopes of 2 described in any item contractings, wherein the envelope of the H containing activity
End type dimethyl silicone polymer is amino-terminated type dimethyl silicone polymer, carboxy blocking type dimethyl silicone polymer, alcoholic extract hydroxyl group
One of end-sealed type dimethyl silicone polymer is a variety of.
4. according to claim 1 or a kind of oily cathode electrophoresis dopes of 2 described in any item contractings, wherein the isocyanates is two
Isocyanates.
5. the oily cathode electrophoresis dope of a kind of contracting according to claim 4, wherein the diisocyanate includes that toluene two is different
Cyanate, isophorone diisocyanate, methyl diphenylene diisocyanate, dicyclohexyl methyl hydride diisocyanate, six methylenes
Group diisocyanate or lysine diisocyanate.
6. preparing a kind of preparation method of contracting oil cathode electrophoresis dope described in claim 1-5, wherein include the following steps,
Isocyanates, methyl iso-butyl ketone (MIBK) are added in reaction vessel, leads to nitrogen, stirs simultaneously, is heated；
The end-sealed type dimethyl silicone polymer of the H containing activity is added dropwise into reaction vessel, is heated after being added dropwise, to anti-for the first time
After answering, then cool down；
Continue that butyl glycol ether, heating, to after reaction, cool down spare for the second time is added dropwise into reaction vessel；
Epoxy resin is added into another reaction vessel, the above-mentioned material prepared is added in this reaction vessel, stirs, adds
Then acetic acid is added in heat, neutralize resin；
Stop heating, pure water is added, is uniformly dispersed and prepares finished product.
7. a kind of preparation method of oily cathode electrophoresis dope that contracts as claimed in claim 6, wherein first set reaction is to react extremely
Nco value is 255-275 ‰.
8. a kind of preparation method of oily cathode electrophoresis dope that contracts as claimed in claim 6, wherein the second secondary response is to react extremely
Nco value is < 1.5 ‰.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910772031.1A CN110358412B (en) | 2019-08-21 | 2019-08-21 | Oil-shrinking cathode electrophoretic coating and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910772031.1A CN110358412B (en) | 2019-08-21 | 2019-08-21 | Oil-shrinking cathode electrophoretic coating and preparation method thereof |
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| Publication Number | Publication Date |
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| CN110358412A true CN110358412A (en) | 2019-10-22 |
| CN110358412B CN110358412B (en) | 2021-12-28 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319689A (en) * | 2013-06-24 | 2013-09-25 | 浩力森涂料（上海）有限公司 | Emulsion resin for high-throwing-power cathode electrophoretic paint and preparation method thereof |
| CN108753245A (en) * | 2018-06-29 | 2018-11-06 | 合肥帧讯低温科技有限公司 | Low-temperature-resistant environment-friendly sealant and preparation method thereof |
| CN108976884A (en) * | 2018-07-29 | 2018-12-11 | 立邦工业涂料(上海)有限公司 | A kind of electrophoretic coating and preparation method thereof |
| CN109111563A (en) * | 2018-07-19 | 2019-01-01 | 浩力森化学科技（江苏）有限公司 | Pigment dispersing resin and preparation method thereof for bottom surface unification cathode electrophoresis dope |
-
2019
- 2019-08-21 CN CN201910772031.1A patent/CN110358412B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319689A (en) * | 2013-06-24 | 2013-09-25 | 浩力森涂料（上海）有限公司 | Emulsion resin for high-throwing-power cathode electrophoretic paint and preparation method thereof |
| CN108753245A (en) * | 2018-06-29 | 2018-11-06 | 合肥帧讯低温科技有限公司 | Low-temperature-resistant environment-friendly sealant and preparation method thereof |
| CN109111563A (en) * | 2018-07-19 | 2019-01-01 | 浩力森化学科技（江苏）有限公司 | Pigment dispersing resin and preparation method thereof for bottom surface unification cathode electrophoresis dope |
| CN108976884A (en) * | 2018-07-29 | 2018-12-11 | 立邦工业涂料(上海)有限公司 | A kind of electrophoretic coating and preparation method thereof |
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| CN110358412B (en) | 2021-12-28 |
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