CN105504252B - The preparation method of watersoluble baking paint polyester resin - Google Patents
The preparation method of watersoluble baking paint polyester resin Download PDFInfo
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- CN105504252B CN105504252B CN201610017374.3A CN201610017374A CN105504252B CN 105504252 B CN105504252 B CN 105504252B CN 201610017374 A CN201610017374 A CN 201610017374A CN 105504252 B CN105504252 B CN 105504252B
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- polyester resin
- baking paint
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- watersoluble baking
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/695—Polyesters containing atoms other than carbon, hydrogen and oxygen containing silicon
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention relates to watersoluble baking paint technical fields,More particularly to a kind of preparation method of watersoluble baking paint polyester resin,By mass fraction by 28~36 parts of M-phthalic acid,20~26 parts of polyalcohol,24~32 parts of phthalic anhydride,9~12 parts of dihydromethyl propionic acid,0.2 part of antioxidant,3~5 parts of dimethylbenzene,19~26 parts of butyl glycol ether,5~9 parts of dimethylethanolamines,3~6 parts of epoxy silicones oxygen alkane monomer mixing,1h is kept the temperature at 150 DEG C~170 DEG C,Then heat to 170 DEG C~180 DEG C heat preservation 2h 3h,It is warming up to 210 DEG C~230 DEG C progress esterifications again,Polyorganosiloxane segment is introduced into aqueous polyester resin system,The organic siloxane modified polyester resin of water-base epoxy base is synthesized,It produces water resistance after being mixed with amino resins,The excellent watersoluble baking paint of weatherability.
Description
Technical field
The present invention relates to technical field of aqueous paint, more particularly to a kind of preparation side of watersoluble baking paint polyester resin
Method.
Background technology
As coatings industry and coating process develop to low stainization, water paint increasingly rises.Water paint subtracts
Organic solvent is lacked to be endangered caused by environment with polluting, has ensured the health of operating personnel, reduced the production of coating
Cost takes safety measures and is transported convenient for factory, while is convenient for the cleaning of tool again.Safe and environment-friendly, nuisanceless, volatility
Organic matter（VOC）Few green environmental friendly coatings are discharged, there is the necessity developed very much, be also with a wide range of applications.
The common water-base resin of water paint has：It is aqueous epoxy resins, aqueous polyurethane, water-based acrylic resin, aqueous
Alkyd resin, aqueous polyester resin etc..Wherein, aqueous alkide resin, aqueous polyester resin can be used for production watersoluble baking paint.Water
Property Baking Paint be generally used for metal works surfaces externally and internally application, after workpiece surface sprays paint, shape through high-temperature baking, show
Color is good, but also higher to paint requirements simultaneously.Compared with solvent type Baking Paint, the ageing-resistant performance of water-soluble Baking Paint
Well, the characteristics of nontoxic, pollution-free, non-ignitable not quick-fried, is more outstanding.
In the prior art, a kind of method for producing watersoluble baking paint is to mix polyester resin with amino resins, polyester
Resin does not react at normal temperatures with amino resins, reacts by high-temperature baking, so as to crosslinking curing.To obtain preferable oil
Performance is painted, some other structures can be introduced by chemical modification in synthesizing polyester resin, polyester resin can be made to have originally
The performance not having reaches improvement and certain prominent performance purpose, to reach special application performance requirement.It is existing by changing
The Baking Paint of property polyester resin production is the problem is that water resistance, weatherability, adhesive force are poor.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to by the way that epoxy silicones oxygen alkane segment is introduced into water
Property polyester resin system in, synthesized water resistance, good weatherability, adhesive force it is excellent for producing the polyester tree of watersoluble baking paint
Fat.
The technical solution adopted by the present invention to solve the technical problems is：A kind of preparation of watersoluble baking paint polyester resin
Method is, by mass fraction by 28~36 parts of M-phthalic acid, 20~26 parts of polyalcohol, 24~32 parts of phthalic acid
Acid anhydride, 9~12 parts of dihydromethyl propionic acid, 0.2 part of antioxidant, 3~5 parts of dimethylbenzene, 19~26 parts of butyl glycol ether, 5
~9 parts of dimethylethanolamines, the mixing of 3~6 parts of epoxy silicones oxygen alkane monomer, keep the temperature 1h, then at 150 DEG C~170 DEG C
170 DEG C~180 DEG C heat preservation 2h-3h are warming up to, then are warming up to 210 DEG C~230 DEG C progress esterifications.
The antioxidant is triphenyl phosphite.
Preferably, preparation method of the invention is：By mass fraction by 30~35 parts of M-phthalic acid, 25 parts of three hydroxyls
Methylpropane, 25~30 parts of phthalic anhydride, 10~12 parts of dihydromethyl propionic acid, 0.2 part of antioxidant, 3~5 parts
Dimethylbenzene, 20~25 parts of butyl glycol ether, 5~8 parts of dimethylethanolamines, the mixing of 3~5 parts of organosiloxane monomer,
160 DEG C of heat preservation 1h then heat to 180 DEG C of heat preservation 2h-3h, then are warming up to 220 DEG C of progress esterifications.
The polyalcohol is pentaerythrite, trimethylolpropane or glycerine.
The epoxy silicones oxygen alkane monomer is 2- (3,4- 7-oxa-bicyclo[4.1.0s) ethyl trimethoxy silane, γ-shrink
Glycerin ether oxygroup propyl trimethoxy silicane or γ-glycydoxy triethoxysilane.
The beneficial effects of the invention are as follows：By in the epoxy group in epoxy silicones oxygen alkane and polyester resin strand
Alcoholic extract hydroxyl group, carboxyl are reacted, and so as to which polyorganosiloxane segment is introduced into aqueous polyester resin system, have synthesized aqueous ring
It is excellent to produce water resistance, weatherability, adhesive force for the organic siloxane modified polyester resin of oxygroup after being mixed with amino resins
Good watersoluble baking paint.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, is not the practical range the present invention
Limited to this.
Embodiment one.
The preparation method of a kind of watersoluble baking paint polyester resin of the present embodiment, by mass fraction by 28~36 parts
M-phthalic acid, 20~26 parts of polyalcohol, 24~32 parts of phthalic anhydride, 9~12 parts of dihydromethyl propionic acid, 0.2
The antioxidant, 3~5 parts of dimethylbenzene, 19~26 parts of butyl glycol ether, 5~9 parts of dimethylethanolamines, 3~6 parts of ring of part
Oxygroup organosiloxane monomer mixes, and 1h is kept the temperature at 150 DEG C~170 DEG C, then heats to 170 DEG C~180 DEG C heat preservation 2h-3h,
It is warming up to 210 DEG C~230 DEG C progress esterifications again.The polyester resin obtained after reaction is mixed with amino resins, at normal temperatures
It does not react, reacts and crosslinking curing by high-temperature baking.
Further, the antioxidant is triphenyl phosphite, and the dimethylbenzene of addition can promote esterification to positive and negative
Direction is answered to carry out, dihydromethyl propionic acid is aqueous monomers, and butyl glycol ether is cosolvent, and dimethylethanolamine is neutralizer.
The epoxy silicones oxygen alkane monomer is 2- (3,4- 7-oxa-bicyclo[4.1.0s) ethyl trimethoxy silane, γ-shrink
Glycerin ether oxygroup propyl trimethoxy silicane or γ-glycydoxy triethoxysilane.
In the process of watersoluble baking paint polyester resin, alcohol carries out esterification generation polyester resin with carboxylic acid,
Meanwhile epoxy silicones oxygen alkane monomer is reacted with alcoholic extract hydroxyl group, the carboxyl in polyester resin strand.
The molecular formula of epoxy silicones oxygen alkane monomer is。
Epoxy silicones oxygen alkane monomer is a kind of containing there are one epoxy organic active base and a methoxy silane are inorganic
The bifunctional silane of active group.Epoxy group has the activity reacted with alcoholic extract hydroxyl group, the carboxyl of polyester resin, reacts machine
It manages and is：
It is reacted with carboxyl：
It is reacted with alcoholic extract hydroxyl group：。
By reaction, so that polyorganosiloxane segment is introduced into aqueous polyester resin system, water resistance, resistance to has been synthesized
The excellent organic siloxane modified polyester resin of water-base epoxy base of time property, epoxy silicones oxygen alkane monomer contain methoxyl group silicon
Alkane inorganic active base functional group, it is anti-that condensation occurs for the silicone hydroxyl and the hydroxyl of inorganic material surface formed after functional group hydrolysis
Should, so as to improve adhesive force of the aqueous polyester resin to ground, simultaneously as polyester resin branched fraction polyorganosiloxane segment
Introducing, substantially increase drying property, weatherability, durability, heat resistance and the water resistance of the aqueous polyester resin.
Embodiment two.
The preparation method of the present embodiment is：By mass fraction by 30~35 parts of M-phthalic acid, 25 parts of trihydroxy methyl
Propane, 25~30 parts of phthalic anhydride, 10~12 parts of dihydromethyl propionic acid, 0.2 part of antioxidant, 3~5 parts of diformazan
Benzene, 20~25 parts of butyl glycol ether, 5~8 parts of dimethylethanolamines, the mixing of 3~5 parts of organosiloxane monomer, at 160 DEG C
1h is kept the temperature, then heats to 180 DEG C of heat preservation 2h-3h, then is warming up to 220 DEG C of progress esterifications.Other are identical with embodiment one,
It repeats no more.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected
The limitation of range is protected, although being explained in detail with reference to preferred embodiment to the present invention, those of ordinary skill in the art should
Work as understanding, technical scheme of the present invention can be modified or replaced equivalently, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (4)
1. a kind of preparation method of watersoluble baking paint polyester resin, it is characterised in that：It will be between 28~36 parts by mass fraction
Phthalic acid, 20~26 parts of polyalcohol, 24~32 parts of phthalic anhydride, 9~12 parts of dihydromethyl propionic acid, 0 .2 parts
Antioxidant, 3~5 parts of dimethylbenzene, 19~26 parts of butyl glycol ether, 5~9 parts of dimethylethanolamines, 3~6 parts of epoxy
Base organosiloxane monomer mixes, and 1h is kept the temperature at 150 DEG C~170 DEG C, then heats to 170 DEG C~180 DEG C heat preservation 2h-3h, then
It is warming up to 210 DEG C~230 DEG C progress esterifications；The epoxy silicones oxygen alkane monomer is 2- (3,4- 7-oxa-bicyclo[4.1.0)
Three second of ethyl trimethoxy silane, γ-glycydoxy trimethoxy silane or γ-glycydoxy
Oxysilane.
2. the preparation method of watersoluble baking paint polyester resin according to claim 1, it is characterised in that：The antioxidant
For triphenyl phosphite.
3. the preparation method of watersoluble baking paint polyester resin according to claim 1, it is characterised in that：By mass fraction
By 30~35 parts of M-phthalic acid, 25 parts of trimethylolpropane, 25~30 parts of phthalic anhydride, the two of 10~12 parts
Hydroxymethyl propionic acid, 0.2 part of antioxidant, 3~5 parts of dimethylbenzene, 20~25 parts of butyl glycol ether, 5~8 parts of dimethyl ethanols
Amine, the mixing of 3~5 parts of epoxy silicones oxygen alkane monomer, 1h is kept the temperature at 160 DEG C, then heats to 180 DEG C of heat preservation 2h-3h, then
It is warming up to 220 DEG C of progress esterifications.
4. the preparation method of watersoluble baking paint polyester resin according to claim 1, it is characterised in that：The polyalcohol
For pentaerythrite, trimethylolpropane or glycerine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610017374.3A CN105504252B (en) | 2016-01-12 | 2016-01-12 | The preparation method of watersoluble baking paint polyester resin |
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|---|---|---|---|
| CN201610017374.3A CN105504252B (en) | 2016-01-12 | 2016-01-12 | The preparation method of watersoluble baking paint polyester resin |
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| CN105504252A CN105504252A (en) | 2016-04-20 |
| CN105504252B true CN105504252B (en) | 2018-06-26 |
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| CN107099024A (en) * | 2017-06-21 | 2017-08-29 | 珠海市金团化学品有限公司 | A kind of waterborne polyester of water boiling resistance excellent performance and preparation method thereof |
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| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Ruilian Inventor before: He Chunquan Inventor before: Wang Ruilian Inventor before: Wang Ruiqi Inventor before: Yu Guo Inventor before: Liao Luquan Inventor before: Wang Jicheng |
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Effective date of registration: 20180508 Address after: 441400 Song Yu four Road Economic Development Zone, Yicheng, Xiangyang, Hubei Applicant after: Wang Ruilian Address before: 441400 Song Yu four road Hubei Xingxing Chemical Industry Co., Ltd., Yicheng Economic Development Zone, Xiangfan, Hubei Applicant before: Hubei Qianxing Chemical Co., Ltd. |
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Effective date of registration: 20190122 Address after: 518107 Guangming Street Sightseeing Road 3009 Guangming New Area Overseas Students Pioneer Park 708, Guangming New Area, Shenzhen City, Guangdong Province Patentee after: Shenzhen Hyde New Materials Technology Co., Ltd. Address before: 441400 Song Yu four Road Economic Development Zone, Yicheng, Xiangyang, Hubei Patentee before: Wang Ruilian |