CN104788652A - Anti-aging super-weatherability saturated polyester resin and preparation method thereof - Google Patents
Anti-aging super-weatherability saturated polyester resin and preparation method thereof Download PDFInfo
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- CN104788652A CN104788652A CN201510117777.0A CN201510117777A CN104788652A CN 104788652 A CN104788652 A CN 104788652A CN 201510117777 A CN201510117777 A CN 201510117777A CN 104788652 A CN104788652 A CN 104788652A
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Abstract
The invention discloses an anti-aging super-weatherability saturated polyester resin comprising the components in parts by weight: 100 parts by weight of neopentyl glycol; 12-28 parts by weight of pentaerythritol; 10-30 parts by weight of 1,4-cyclohexanedimethanol; 20-35 parts by weight of titanium dioxide; 60-70 parts by weight of m-phthalic acid; 20-45 parts by weight of beta-hydroxyalkylamide; 8-15 parts by weight of an antioxidant; and 4-12 parts by weight of decabromodiphenyl ether. The invention also discloses a preparation method of the anti-aging super-weatherability saturated polyester resin. While ensuring good weatherability, the anti-aging super-weatherability saturated polyester resin has good mechanical properties, and has friendly environmental performance and excellent flame retardant property.
Description
Technical field
The invention belongs to outdoor powder coating technical field, relate to a kind of anti-aging super weather-proof saturated polyester resin, also relate to the preparation method of this kind of anti-aging super weather-proof saturated polyester resin.
Background technology
Powder coating is a kind of green coating of non-volatile solvent, has solvent-free, low stain, the advantages such as material use efficiency is high, energy expenditure is low.At present, powder coating application is out of doors increasingly extensive, and as traffic facilities, vehicle, exterior wall decorating coating etc., this just requires that it has stronger weathering resistance.Generally speaking, for the consideration to mechanical property and cost, weather resistant vibrin many employings terephthalic acid and m-phthalic acid copolycondensation obtain, and super-weatherable polyether resin many employings m-phthalic acid of routine obtains, cause the mechanical property of resin poor like this, have impact on the use of resin.
The weathering resistance of recent domestic to powder coating has more research, and successfully develop and be a series ofly applicable to outdoor powder coating systems, as polyester/triglycidyl group isocyanuric acid ester (TGIC) system, polyester/esters of acrylic acid system, polyurethane system and fluorine-containing, silicon system etc.Polyester/TGIC type powder coating is that in current polyester series, weathering resistance is a kind of preferably.When polyester and solidifying agent TGIC are cross-linked, paint having no volatile substances produces, and can obtain the film of free of pinholes, and system is homogeneous, stable, adjustable, has good heat-resisting and weather resistance, substantially can meet the requirement in market.But its strong skin irritation and potential carinogenicity, make its production and selling all be greatly affected, become inevitable by market.Wherein, the use of TGIC in powder coating is expressly forbidden in Europe.How while guarantee good weatherability properties, also there is good mechanical property, and there is friendly environmental performance will become new problem.
Summary of the invention
The object of this invention is to provide a kind of anti-aging super weather-proof saturated polyester resin, while guarantee good weatherability properties, can also have good mechanical property, and there is friendly environmental performance and excellent flame retardant properties.
Another object of the present invention is to provide the preparation method of this kind of anti-aging super weather-proof saturated polyester resin.
For technical solution problem, the present invention adopts following technical scheme:
A kind of anti-aging super weather-proof saturated polyester resin, comprise following component, each component is respectively according to weight part:
The preparation method of this kind of anti-aging super weather-proof saturated polyester resin, its preparation process comprises: reactor is heated to 95 ~ 100 DEG C, add neopentyl glycol, tetramethylolmethane, 1, 4-cyclohexanedimethanol and titanium dioxide, slowly heat up while stirring, pass into nitrogen protection simultaneously, constant temperature is kept after within 20 ~ 30 minutes, being warming up to 245 DEG C, react 3 ~ 5 hours, until reactant clarification and acid number at 6 ~ 8mgKOH/g, continue to stir, then 230 ~ 235 DEG C are slow cooling to, add m-phthalic acid and beta-hydroxy alkylamide, constant temperature is kept after being slowly warming up to 245 DEG C, react 3 ~ 5 hours, until reactant clarification and acid number at 42 ~ 48mgKOH/g, then vacuumize, vacuum tightness is 0.06 ~ 0.08Mpa, until reactant viscosity is at 4500 ~ 5500mPas, acid number is at 32 ~ 34mgKOH/g, stopping vacuumizes, cool to 200 ~ 210 DEG C, add oxidation inhibitor and decabromodiphynly oxide, stir 0.5 hour, obtain anti-aging super weather-proof saturated polyester resin product.
Present invention employs the tetramethylolmethane of four functionality, modified monomer 1,4 cyclohexane dimethanol, low toxic and environment-friendly type compound beta-hydroxy alkylamide and pollution-free interpolation sex flame retardant decabromodiphynly oxide to react.Tetramethylolmethane can make the collateralization degree of polyester greatly improve, thus improves the weathering resistance of product; 1,4 cyclohexane dimethanol effectively can improve the mechanical property of polyester; Beta-hydroxy alkylamide as the solidifying agent of vibrin, has the advantages such as reactive behavior is strong, solidification value is low, stability in storage is good in art of powder coatings; Decabromodiphynly oxide, except itself is pollution-free, environmentally friendly, can also increase the flame retardant resistance of polyester, makes powder coating in use can be more effectively fire-retardant, is specially adapted to outdoor powder coating.
Preferably, anti-aging super weather-proof saturated polyester resin comprises following component, and each component is respectively according to weight part:
Preferably, anti-aging super weather-proof saturated polyester resin comprises following component, and each component is respectively according to weight part:
Preferably, anti-aging super weather-proof saturated polyester resin comprises following component, and each component is respectively according to weight part:
Preferably, anti-aging super weather-proof saturated polyester resin comprises following component, and each component is respectively according to weight part:
Compared with prior art, the present invention has following beneficial effect:
Present invention employs the tetramethylolmethane of four functionality, modified monomer 1,4 cyclohexane dimethanol, low toxic and environment-friendly type compound beta-hydroxy alkylamide and pollution-free interpolation sex flame retardant decabromodiphynly oxide to react.Make the anti-aging super weather-proof saturated polyester resin product obtained while guarantee good weatherability properties, can also have good mechanical property, and there is friendly environmental performance and excellent flame retardant properties, be specially adapted to outdoor powder coating.
Below in conjunction with embodiment, the invention will be further described:
Embodiment
A kind of anti-aging super weather-proof saturated polyester resin embodiment 1 of the present invention, comprise following component, each component is respectively according to weight part:
The preparation method of this kind of anti-aging super weather-proof saturated polyester resin is as follows: reactor is heated to 95 ~ 100 DEG C, add neopentyl glycol, tetramethylolmethane, 1, 4-cyclohexanedimethanol and titanium dioxide, slowly heat up while stirring, pass into nitrogen protection simultaneously, constant temperature is kept after within 20 ~ 30 minutes, being warming up to 245 DEG C, react 3 ~ 5 hours, until reactant clarification and acid number at 6 ~ 8mgKOH/g, continue to stir, then 230 ~ 235 DEG C are slow cooling to, add m-phthalic acid and beta-hydroxy alkylamide, constant temperature is kept after being slowly warming up to 245 DEG C, react 3 ~ 5 hours, until reactant clarification and acid number at 42 ~ 48mgKOH/g, then vacuumize, vacuum tightness is 0.06 ~ 0.08Mpa, until reactant viscosity is at 4500 ~ 5500mPas, acid number is at 32 ~ 34mgKOH/g, stopping vacuumizes, cool to 200 ~ 210 DEG C, add oxidation inhibitor and decabromodiphynly oxide, stir 0.5 hour, obtain anti-aging super weather-proof saturated polyester resin product.
A kind of anti-aging super weather-proof saturated polyester resin embodiment 2 of the present invention, comprise following component, each component is respectively according to weight part:
The preparation method of this kind of anti-aging super weather-proof saturated polyester resin is identical with embodiment 1.
A kind of anti-aging super weather-proof saturated polyester resin embodiment 3 of the present invention, comprise following component, each component is respectively according to weight part:
The preparation method of this kind of anti-aging super weather-proof saturated polyester resin is identical with embodiment 1.
A kind of anti-aging super weather-proof saturated polyester resin embodiment 4 of the present invention, comprise following component, each component is respectively according to weight part:
The preparation method of this kind of anti-aging super weather-proof saturated polyester resin is identical with embodiment 1.
Saturated polyester resin comparative example of the prior art, comprises following component, and each component is respectively according to weight part:
The preparation method of this kind of saturated polyester resin is as follows: reactor is heated to 95 ~ 100 DEG C, add neopentyl glycol, m-phthalic acid and titanium dioxide, slowly heat up while stirring, pass into nitrogen protection simultaneously, constant temperature is kept after being warming up to 245 DEG C, react 12 ~ 15 hours, until reactant clarification and acid number at 42 ~ 48mgKOH/g, then vacuumize, vacuum tightness is 0.06 ~ 0.08Mpa, until reactant viscosity is at 4500 ~ 5500mPas, acid number is at 32 ~ 34mgKOH/g, stopping vacuumizes, cool to 200 ~ 210 DEG C, add oxidation inhibitor, stir 0.5 hour, obtain saturated polyester resin product.
The acid number of the anti-aging super weather-proof saturated polyester resin product that embodiment 1 ~ 4 obtains, viscosity, second-order transition temperature, softening temperature, set time and limiting oxygen index(LOI) etc. at 200 DEG C are detected, be compared with the prior art example to compare, detected result is as shown in table 1 simultaneously.
Table 1
Test result shows, the acid number of the anti-aging super weather-proof saturated polyester resin product that the embodiment of the present invention 1 ~ 4 obtains is at 30 ± 2mgKOH/g, viscosity is at 5500 ± 600mPas, second-order transition temperature is at 64 ± 2 DEG C, softening temperature is at 110 ± 10 DEG C, set time at 200 DEG C at 10 ± 2min, limiting oxygen index(LOI) >=35%.Compared with comparative example, second-order transition temperature, the softening temperature of embodiment 1 ~ 4 are significantly improved, and illustrate that weather resistance increases to some extent, and viscosity also increases and is evenly distributed, and are conducive to the quality control to finished product.The acid number of embodiment 1 ~ 4 and but greatly declining than comparative example the set time at 200 DEG C, 10 ~ 20min can be accomplished preferably in prior art, the present invention but can drop to 10 ± 2min, illustrate that the time required for solidification is shorter, obviously be better than comparative example, and limiting oxygen index(LOI) is obviously large than comparative example, illustrates that flame retardant properties significantly improves than comparative example, limiting oxygen index(LOI) refers to the statement of sample combustion requisite oxygen tolerance, therefore can judge the flame retardant properties of fabric by measuring oxygen index.Oxygen index is higher then illustrates that the oxygen concentration maintained needed for burning is higher, namely represent more difficult to burn, be divided into inflammable (LOI<20%), flammable (LOI=20% ~ 26%), difficult combustion (LOI=26% ~ 34%) and do not fire (LOI>35%) four grades.The over-all properties of visible product is all significantly improved than prior art.
The foregoing is only specific embodiments of the invention, but technical characteristic of the present invention is not limited thereto, any those skilled in the art is in the field of the invention, and the change done or modification are all encompassed among the scope of the claims of the present invention.
Claims (6)
1. an anti-aging super weather-proof saturated polyester resin, it is characterized in that: comprise following component, each component is respectively according to weight part:
2. a kind of anti-aging super weather-proof saturated polyester resin as claimed in claim 1, it is characterized in that: comprise following component, each component is respectively according to weight part:
3. a kind of anti-aging super weather-proof saturated polyester resin as claimed in claim 1, it is characterized in that: comprise following component, each component is respectively according to weight part:
4. a kind of anti-aging super weather-proof saturated polyester resin as claimed in claim 1, it is characterized in that: comprise following component, each component is respectively according to weight part:
5. a kind of anti-aging super weather-proof saturated polyester resin as claimed in claim 1, it is characterized in that: comprise following component, each component is respectively according to weight part:
6. the preparation method of a kind of anti-aging super weather-proof saturated polyester resin as claimed in claim 1, it is characterized in that: its preparation process comprises: reactor is heated to 95 ~ 100 DEG C, add neopentyl glycol, tetramethylolmethane, 1, 4-cyclohexanedimethanol and titanium dioxide, slowly heat up while stirring, pass into nitrogen protection simultaneously, constant temperature is kept after within 20 ~ 30 minutes, being warming up to 245 DEG C, react 3 ~ 5 hours, until reactant clarification and acid number at 6 ~ 8mgKOH/g, continue to stir, then 230 ~ 235 DEG C are slow cooling to, add m-phthalic acid and beta-hydroxy alkylamide, constant temperature is kept after being slowly warming up to 245 DEG C, react 3 ~ 5 hours, until reactant clarification and acid number at 42 ~ 48mgKOH/g, then vacuumize, vacuum tightness is 0.06 ~ 0.08Mpa, until reactant viscosity is at 4500 ~ 5500mPas, acid number is at 32 ~ 34mgKOH/g, stopping vacuumizes, cool to 200 ~ 210 DEG C, add oxidation inhibitor and decabromodiphynly oxide, stir 0.5 hour, obtain anti-aging super weather-proof saturated polyester resin product.
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| CN201510117777.0A CN104788652A (en) | 2015-03-18 | 2015-03-18 | Anti-aging super-weatherability saturated polyester resin and preparation method thereof |
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| CN201510117777.0A CN104788652A (en) | 2015-03-18 | 2015-03-18 | Anti-aging super-weatherability saturated polyester resin and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633665A (en) * | 2012-04-14 | 2012-08-15 | 修建东 | Preparation method of hydroxyalkyl amide type hard water softening agent |
| CN107964093A (en) * | 2017-09-29 | 2018-04-27 | 广东依斯特新材料有限公司 | Powdery paints hydroxyl telechelic polyester resin, preparation method and obtained powdery paints |
| CN112321808A (en) * | 2020-10-11 | 2021-02-05 | 芜湖市森沐知识产权科技服务有限公司 | Saturated polyester resin |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010501A (en) * | 2010-10-27 | 2011-04-13 | 中国电器科学研究院 | Polyester resin for beta-hydroxyalkylamide low temperature curing weather-resistant powder paint and preparation method thereof |
-
2015
- 2015-03-18 CN CN201510117777.0A patent/CN104788652A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010501A (en) * | 2010-10-27 | 2011-04-13 | 中国电器科学研究院 | Polyester resin for beta-hydroxyalkylamide low temperature curing weather-resistant powder paint and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633665A (en) * | 2012-04-14 | 2012-08-15 | 修建东 | Preparation method of hydroxyalkyl amide type hard water softening agent |
| CN107964093A (en) * | 2017-09-29 | 2018-04-27 | 广东依斯特新材料有限公司 | Powdery paints hydroxyl telechelic polyester resin, preparation method and obtained powdery paints |
| CN112321808A (en) * | 2020-10-11 | 2021-02-05 | 芜湖市森沐知识产权科技服务有限公司 | Saturated polyester resin |
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Effective date of registration: 20150929 Address after: Jiaxing City, Zhejiang province 314412 Haining Yanguan Central Garden Road No. 3 Applicant after: ZHEJIANG GUANGHUA MATERIAL TECHNOLOGY CO., LTD. Address before: Jiaxing City, Zhejiang province 314412 Haining Yanguan Central Garden Road No. 3 Applicant before: ZHEJIANG GUANGHUA NEW MATERIALS CO., LTD. |
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Application publication date: 20150722 |