CN104448273A - Indoor physical-matting-type saturated polyester resin as well as preparation method thereof and coating - Google Patents
Indoor physical-matting-type saturated polyester resin as well as preparation method thereof and coating Download PDFInfo
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Abstract
The invention discloses indoor physical-matting-type saturated polyester resin as well as a preparation method thereof and a coating. The indoor physical-matting-type saturated polyester resin is prepared from the following components in parts by weight: 30-45 parts of polyol, 55-70 parts of polyacid, 0-5 parts of dimethylolpropionic acid, 0.1-0.3 part of a catalyst, 0.1-0.5 part of an antioxidant, 5-10 parts of trimellitic anhydride, 3-8 parts of polyacid prepolymer, and 0.1-1 part of a curing accelerator. The indoor physical-matting-type saturated polyester resin can be used in combination with epoxy resin and an indoor physical matting agent, after the saturated polyester resin is cured, the 60-degree gloss of the film is between 5% and 30%, the saturated polyester resin has the advantages of good leveling property, impact resistance, bending resistance, no pollution and low cost, can meet the physical matting requirement of indoor metal profiles and is an environment-friendly product.
Description
Technical field
The present invention relates to technical field of surface coating, particularly relate to a kind of regulatable type indoor physics extinction type saturated polyester resin and preparation method thereof and coating.
Background technology
The shares of feature shared by Coating Market such as powder coating is pollution-free because of it, the high and convenient transport of availability are increasing, and the paint film of saturated polyester resin is full, excellent property, purposes are different, are China's most active kinds of development & production voluntarily in recent years.Along with the raising of living standard, the transformation of the aesthetic standards of people, extinction type coating is accepted by users, especially indoor application part, the environment worked long hours as car and boat wheel house, office etc. more needs peace and quiet comfortable low gloss, therefore, the focus that low gloss saturated polyester resin also becomes research staff's concern is developed.But traditional low gloss saturated polyester resin is generally use chemical quenching agent to carry out delustring, it is high to there is cost in chemical quenching, easily produces the shortcomings such as pollution; If use more environmental protection, the physics matting agent that cost performance is higher carries out delustring, then need to propose higher requirement to saturated polyester resin.Present saturated polyester resin is on the market difficult to reach desired effect.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of indoor physics extinction type saturated polyester resin and preparation method thereof and coating, be intended to solve existing saturated polyester resin and use physics matting agent to be difficult to reach the problem of high comprehensive performance.
Technical scheme of the present invention is as follows:
A kind of indoor physics extinction type saturated polyester resin, wherein, count composed of the following components by weight:
Polyvalent alcohol 30-45 part;
Polyprotonic acid 55-70 part;
Dimethylol propionic acid 0-5 part;
Catalyzer 0.1-0.3 part;
Antioxidant 0.1-0.5 part;
Trimellitic acid 1,2-anhydride 5-10 part;
Polyprotonic acid performed polymer 3-8 part;
Curing catalyst 0.1-1 part.
Described indoor physics extinction type saturated polyester resin, wherein, described polyvalent alcohol is one or more in neopentyl glycol, TriMethylolPropane(TMP), ethylene glycol, Diethylene Glycol.
Described indoor physics extinction type saturated polyester resin, wherein, described polyprotonic acid is one or more in terephthalic acid, m-phthalic acid, hexanodioic acid.
Described indoor physics extinction type saturated polyester resin, wherein, described polyprotonic acid performed polymer is ethylene glycol and pyromellitic dianhydride performed polymer.
Described indoor physics extinction type saturated polyester resin, wherein, described catalyzer is one or more in Mono-n-butyltin, dibutyl tin dilaurate, dibutyl tin acetate.
Described indoor physics extinction type saturated polyester resin, wherein, described antioxidant is Hypophosporous Acid, 50 or triphenylphosphate.
Described indoor physics extinction type saturated polyester resin, wherein, described curing catalyst is one or more in triphenylphosphine, anilino formyl imidazoles, benzylimidazoline.
A preparation method for indoor physics extinction type saturated polyester resin as above, wherein, comprises the following steps:
Add polyvalent alcohol 30 ~ 45 parts in advance, polyprotonic acid 55 ~ 70 parts, dimethylol propionic acid 0 ~ 5 part; Catalyzer 0.1 ~ 0.3 part and antioxidant 0.1 ~ 0.5 part, be warming up to 240 ~ 250 DEG C, reacts 5 ~ 10 hours; Testing product acid number, after 15 ~ 25mgKOH/g, is cooled to 200 ~ 230 DEG C, is evacuated to vacuum tightness-0.1MPa, reacts 2 ~ 6 hours; Testing product acid number, at 5 ~ 10mgKOH/g, adds trimellitic acid 1,2-anhydride 5 ~ 10 parts; Polyprotonic acid performed polymer 3 ~ 8 parts, reacts 1 ~ 2 hour at 180 ~ 200 DEG C; Testing product acid number, at 65 ~ 80mgKOH/g, adds curing catalyst 0.1 ~ 1 part, reacts 0.5 ~ 1 hour; Discharging, obtained indoor physics extinction type saturated polyester resin.
A kind of coating, wherein, comprises indoor physics extinction type saturated polyester resin as above in the raw material of described coating.
Described coating, wherein, also comprises epoxy resin and indoor physics matting agent in the raw material of described coating.
Described coating, wherein, described coating comprises following component by weight:
Indoor physics extinction type saturated polyester resin 50 parts;
Epoxy resin 50 parts;
Indoor physics matting agent 5 parts;
Titanium dioxide 50 parts;
15 parts, barium sulfate;
St-yrax 0.8 part;
Flow agent 1 part.
Beneficial effect: the invention provides a kind of regulatable type indoor physics extinction type saturated polyester resin and preparation method thereof and coating, described indoor physics extinction type saturated polyester resin can with epoxy resin and indoor physics matting agent with the use of, after solidification, paint film 60 ° of glossiness are between 5% ~ 30%, good leveling property, shock-resistance and resistance to bend(ing) well, can meet the physics delustring demand of indoor shape, pollution-free, cost is low, is Green Product.
Embodiment
The invention provides a kind of regulatable type indoor physics extinction type saturated polyester resin and preparation method thereof and coating, for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
A kind of regulatable type provided by the present invention indoor physics extinction type saturated polyester resin, its be by polyvalent alcohol and polyprotonic acid after polycondensation, obtained with trimellitic acid 1,2-anhydride and polyprotonic acid prepolymer reaction again, its participate in the monomer of reaction and consumption (calculating by weight) as follows:
Polyvalent alcohol 30 ~ 45 parts; Polyprotonic acid 55 ~ 70 parts; Dimethylol propionic acid 0 ~ 5 part; Catalyzer 0.1 ~ 0.3 part; Antioxidant 0.1 ~ 0.5 part; Trimellitic acid 1,2-anhydride 5 ~ 10 parts; Polyprotonic acid performed polymer 3 ~ 8 parts; Curing catalyst 0.1 ~ 1 part.
In preferred embodiment, in described indoor physics extinction type saturated polyester resin, the consumption (counting by weight) of each component is: neopentyl glycol 30 parts; Ethylene glycol 4 parts; Diethylene Glycol 6 parts; Terephthalic acid 65 parts; Catalyzer (Mono-n-butyltin) 0.1 part, antioxidant (triphenyl phosphite) 0.3 part; Trimellitic acid 1,2-anhydride 8 parts; Polyprotonic acid performed polymer 5 parts; Curing catalyst (triphenylphosphine, anilino formyl imidazoles and benzylimidazoline) 1 part.
Further, described polyvalent alcohol is one or more in neopentyl glycol, TriMethylolPropane(TMP), ethylene glycol, Diethylene Glycol.
Described polyprotonic acid is one or more in terephthalic acid, m-phthalic acid, hexanodioic acid.
Described polyprotonic acid performed polymer is ethylene glycol and pyromellitic dianhydride performed polymer, and ethylene glycol and pyromellitic dianhydride form polyprotonic acid performed polymer according to the ratio of the amount of substance of 0.7-1.4.
Described catalyzer is one or more in Mono-n-butyltin, dibutyl tin dilaurate, dibutyl tin acetate.
Described antioxidant is Hypophosporous Acid, 50 or triphenylphosphate.
Described curing catalyst is one or more in triphenylphosphine, anilino formyl imidazoles, benzylimidazoline.
The preparation method of described indoor physics extinction type saturated polyester resin is also provided in the present invention, specifically comprises the following steps:
Add polyvalent alcohol 30 ~ 45 parts in advance, polyprotonic acid 55 ~ 70 parts, dimethylol propionic acid 0 ~ 5 part, catalyzer 0.1 ~ 0.3 part, antioxidant 0.1 ~ 0.5 part, is warming up to 240 ~ 250 DEG C, and react 5 ~ 10 hours, testing product acid number is at 15 ~ 25mgKOH/g; Be cooled to 200 ~ 230 DEG C, be evacuated to vacuum tightness-0.1MPa, react 2 ~ 6 hours, testing product acid number is at 5 ~ 10mgKOH/g; Add trimellitic acid 1,2-anhydride 5 ~ 10 parts; Polyprotonic acid performed polymer 3 ~ 8 parts; React 1 ~ 2 hour at 180 ~ 200 DEG C, testing product acid number is at 65 ~ 80mgKOH/g; Add curing catalyst 0.1 ~ 1 part, react 0.5 ~ 1 hour; Discharging, obtained indoor physics extinction type saturated polyester resin.
In its preparation process, first carry out esterifying polycondensation reaction, increase to until molecule and to a certain degree afterwards add trimellitic acid 1,2-anhydride and polyprotonic acid performed polymer reacts, contribute to the active reactive group that molecule forming position is different; In addition, one or more curing catalysts are finally added in reaction, the unfairness formed on paint film microcosmic because different active reactive group causes speed of response inconsistent during resin solidification can be made, thus be more conducive to physics matting agent and be attached to coating surface, finally reach more good extinction effect.Therefore, described indoor physics extinction type saturated polyester resin can with physics matting agent with the use of, after solidification, paint film 60 ° of glossiness are between 5% ~ 30%, good leveling property, shock-resistance and resistance to bend(ing) well, can meet the physics delustring demand of indoor shape, pollution-free, cost is low, is Green Product.
In order to more detailed description preparation method of the present invention, below enumerate several embodiment further description.
Embodiment 1
A kind of production formula of indoor physics extinction type saturated polyester resin: TriMethylolPropane(TMP) 1 part; Neopentyl glycol 25 parts; Ethylene glycol 7 parts; Diethylene Glycol 3 parts; Dimethylol propionic acid 1 part; Terephthalic acid 55 parts; M-phthalic acid 5 parts; Catalyzer (Mono-n-butyltin) 0.1 part, antioxidant (Hypophosporous Acid, 50) 0.3 part; Trimellitic acid 1,2-anhydride 7 parts; Polyprotonic acid performed polymer 4 parts; Curing catalyst (triphenylphosphine) 0.3 part.
Preparation technology: in reactor, in advance TriMethylolPropane(TMP) 1 part; Neopentyl glycol 25 parts; Ethylene glycol 7 parts; Diethylene Glycol 3 parts; Dimethylol propionic acid 1 part; Terephthalic acid 55 parts; M-phthalic acid 5 parts; Catalyzer (Mono-n-butyltin) 0.1 part, antioxidant (Hypophosporous Acid, 50) 0.3 part; Be warming up to 250 DEG C of reactions 6 hours; Detection acid number is 17.5mgKOH/g; Be cooled to 220 DEG C; Be evacuated to-0.1MPa, react 2 hours; Detection acid number is 9.2mgKOH/g; Add trimellitic acid 1,2-anhydride 7 parts; Polyprotonic acid performed polymer 4 parts; Be cooled to 195 DEG C of reactions 1.5 hours; Detecting acid number is 73.6mg KOH/g; Add curing catalyst (triphenylphosphine) 0.3 part, react 1 hour; Discharging, obtained indoor physics extinction type saturated polyester resin.Carry out performance test to obtained indoor physics extinction type saturated polyester resin, the main performance index drawn is as shown in table 1.
The main performance index of table 1 indoor physics extinction type saturated polyester resin
Embodiment 2
A kind of production formula of indoor physics extinction type saturated polyester resin: TriMethylolPropane(TMP) 1 part; Neopentyl glycol 30 parts; Ethylene glycol 6 parts; Diethylene Glycol 4 parts; Terephthalic acid 60 parts; Hexanodioic acid 3 parts; Catalyzer (dibutyl tin acetate) 0.2 part, antioxidant (triphenylphosphate) 0.2 part; Trimellitic acid 1,2-anhydride 6 parts; Polyprotonic acid performed polymer 5 parts; Curing catalyst (anilino formyl imidazoles and benzylimidazoline) 0.8 part.
Preparation technology: in reactor, in advance TriMethylolPropane(TMP) 1 part; Neopentyl glycol 30 parts; Ethylene glycol 6 parts; Diethylene Glycol 4 parts; Terephthalic acid 60 parts; Hexanodioic acid 3 parts; Catalyzer (dibutyl tin acetate) 0.2 part, antioxidant (triphenylphosphate) 0.2 part; Be warming up to 245 DEG C of reactions 8 hours; Detection acid number is 16.7mgKOH/g; Be cooled to 210 DEG C; Be evacuated to-0.1MPa, react 4 hours; Detection acid number is 10.5mgKOH/g; Add trimellitic acid 1,2-anhydride 6 parts; Polyprotonic acid performed polymer 5 parts; Be cooled to 190 DEG C of reactions 1 hour; Detecting acid number is 75.5mg KOH/g; Add curing catalyst (anilino formyl imidazoles and benzylimidazoline) 0.8 part, react 1 hour; Discharging, obtained indoor physics extinction type saturated polyester resin.Carry out performance test to obtained indoor physics extinction type saturated polyester resin, main performance index is as shown in table 2.
The main performance index of table 2 indoor physics extinction type saturated polyester resin
Embodiment 3
A kind of production formula of indoor physics extinction type saturated polyester resin: neopentyl glycol 30 parts; Ethylene glycol 4 parts; Diethylene Glycol 6 parts; Terephthalic acid 65 parts; Catalyzer (dibutyl tin dilaurate) 0.3 part, antioxidant (triphenyl phosphite) 0.4 part; Trimellitic acid 1,2-anhydride 8 parts; Polyprotonic acid performed polymer 5 parts; Curing catalyst (triphenylphosphine, anilino formyl imidazoles and benzylimidazoline) 1 part.
Preparation technology: in reactor, adds neopentyl glycol 30 parts in advance; Ethylene glycol 4 parts; Diethylene Glycol 6 parts; Terephthalic acid 65 parts; Catalyzer (dibutyl tin dilaurate) 0.3 part, antioxidant (triphenyl phosphite) 0.4 part; Be warming up to 240 DEG C of reactions 10 hours; Detection acid number is 20.1mgKOH/g; Be cooled to 230 DEG C; Be evacuated to-0.1MPa, react 5 hours; Detection acid number is 7.8mgKOH/g; Add trimellitic acid 1,2-anhydride 8 parts; Polyprotonic acid performed polymer 5 parts; Be cooled to 185 DEG C of reactions 2 hours; Detecting acid number is 69.7mg KOH/g; Add curing catalyst (triphenylphosphine, anilino formyl imidazoles and benzylimidazoline) 1 part, react 1 hour; Discharging, obtained indoor physics extinction type saturated polyester resin.Carry out performance test to obtained indoor physics extinction type saturated polyester resin, main performance index is as shown in table 3.
The main performance index of table 3 indoor physics extinction type saturated polyester resin
Embodiment 4
The present invention also provides a kind of coating, comprises indoor physics extinction type saturated polyester resin as above in the raw material of described coating.What coordinate indoor physics extinction type saturated polyester resin to use in addition also has epoxy resin and indoor physics matting agent.
In preferred version, described coating specifically comprises following component by weight:
Indoor physics extinction type saturated polyester resin 50 parts;
Epoxy resin 50 parts;
Indoor physics matting agent 5 parts;
Titanium dioxide 50 parts;
15 parts, barium sulfate;
St-yrax 0.8 part;
Flow agent 1 part.
Particularly, the indoor physics extinction type saturated polyester resin of embodiment 1 ~ 3 gained is used for epoxy resin and physics matting agent with the use of, be prepared into powder coating, shown in concrete formula table 4.Wherein, coating 1,2, the saturated polyester resin used in 3 corresponds to embodiment 1 respectively, the indoor physics extinction type saturated polyester resin of 2,3.In form, each ingredient units of coating is parts by weight.
Table 4 indoor physics extinction type saturated polyester resin makes the formula of coating
| Coating 1 | Coating 2 | Coating 3 | |
| Saturated polyester resin | 50 | 50 | 50 |
| Epoxy resin | 50 | 50 | 50 |
| Physics matting agent SA2065 | 5 | 5 | 5 |
| Titanium dioxide | 50 | 50 | 50 |
| Barium sulfate | 15 | 15 | 15 |
| St-yrax | 0.8 | 0.8 | 0.8 |
| Flow agent | 1 | 1 | 1 |
Carry out performance test to the coating by proportioning preparation in table 4, its result is as shown in table 5.
Table 5 coating property detected result
| Test item | Index | Coating 1 | Coating 2 | Coating 3 |
| Pencil hardness | ≥1H | 1H | 1H | 1H |
| Sticking power | ≤1 | 0 | 0 | 0 |
| Resistance to bend(ing) | ≤2 | 2 | 2 | 2 |
| Shock-resistant/cmkg | 50 | 50 | 50 | 50 |
| 60 ° of glossiness/% | Nothing | 22 | 16 | 7 |
From in the detected result of table 5, the coating adopting indoor physics extinction type saturated polyester resin of the present invention to join is after 180 DEG C of baking 15min, 60 ° of glossiness are low, glossiness can adjust between 5% ~ 30%, strong adhesion, have good shock-resistance and resistance to bend(ing), its over-all properties is better, has higher cost performance.And the present invention is physics extinction type product, has environment-friendly advantage.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (10)
1. an indoor physics extinction type saturated polyester resin, is characterized in that, count composed of the following components by weight:
Polyvalent alcohol 30-45 part;
Polyprotonic acid 55-70 part;
Dimethylol propionic acid 0-5 part;
Catalyzer 0.1-0.3 part;
Antioxidant 0.1-0.5 part;
Trimellitic acid 1,2-anhydride 5-10 part;
Polyprotonic acid performed polymer 3-8 part;
Curing catalyst 0.1-1 part.
2. indoor physics extinction type saturated polyester resin according to claim 1, is characterized in that, described polyvalent alcohol is one or more in neopentyl glycol, TriMethylolPropane(TMP), ethylene glycol, Diethylene Glycol;
Described polyprotonic acid is one or more in terephthalic acid, m-phthalic acid, hexanodioic acid.
3. indoor physics extinction type saturated polyester resin according to claim 1, is characterized in that, described catalyzer is one or more in Mono-n-butyltin, dibutyl tin dilaurate, dibutyl tin acetate.
4. indoor physics extinction type saturated polyester resin according to claim 1, it is characterized in that, described antioxidant is Hypophosporous Acid, 50 or triphenylphosphate.
5. indoor physics extinction type saturated polyester resin according to claim 1, is characterized in that, described curing catalyst is one or more in triphenylphosphine, anilino formyl imidazoles, benzylimidazoline.
6. indoor physics extinction type saturated polyester resin according to claim 1, is characterized in that, described polyprotonic acid performed polymer is ethylene glycol and pyromellitic dianhydride performed polymer.
7. a preparation method for the indoor physics extinction type saturated polyester resin as described in as arbitrary in claim 1 ~ 6, is characterized in that, comprise the following steps:
Add polyvalent alcohol 30 ~ 45 parts in advance, polyprotonic acid 55 ~ 70 parts, dimethylol propionic acid 0 ~ 5 part; Catalyzer 0.1 ~ 0.3 part and antioxidant 0.1 ~ 0.5 part, be warming up to 240 ~ 250 DEG C, reacts 5 ~ 10 hours; Testing product acid number, after 15 ~ 25mgKOH/g, is cooled to 200 ~ 230 DEG C, is evacuated to vacuum tightness-0.1MPa, reacts 2 ~ 6 hours; Testing product acid number, at 5 ~ 10mgKOH/g, adds trimellitic acid 1,2-anhydride 5 ~ 10 parts; Polyprotonic acid performed polymer 3 ~ 8 parts, reacts 1 ~ 2 hour at 180 ~ 200 DEG C; Testing product acid number, at 65 ~ 80mgKOH/g, adds curing catalyst 0.1 ~ 1 part, reacts 0.5 ~ 1 hour; Discharging, obtained indoor physics extinction type saturated polyester resin.
8. a coating, is characterized in that, comprise in the raw material of described coating as arbitrary in claim 1 ~ 6 as described in indoor physics extinction type saturated polyester resin.
9. coating according to claim 8, is characterized in that, also comprises epoxy resin and indoor physics matting agent in the raw material of described coating.
10. coating according to claim 9, is characterized in that, described coating comprises following component by weight:
Indoor physics extinction type saturated polyester resin 50 parts;
Epoxy resin 50 parts;
Indoor physics matting agent 5 parts;
Titanium dioxide 50 parts;
15 parts, barium sulfate;
St-yrax 0.8 part;
Flow agent 1 part.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105860047A (en) * | 2016-06-14 | 2016-08-17 | 黄山市徽州康佳化工有限责任公司 | Polyester resin for matte powdery coating and preparation method and application thereof |
| CN110563936A (en) * | 2019-09-01 | 2019-12-13 | 合众（佛山）化工有限公司 | Self-flame-retardant antibacterial water-based polyester resin and preparation method thereof |
| CN111995894A (en) * | 2020-09-01 | 2020-11-27 | 梧州市泽和高分子材料有限公司 | Extinction paper-removing additive for thermal transfer powder coating |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101056938A (en) * | 2004-11-12 | 2007-10-17 | 伊斯曼化学公司 | Polyester blends with improved stress whitening for film and sheet applications |
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2014
- 2014-12-10 CN CN201410750694.0A patent/CN104448273B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101056938A (en) * | 2004-11-12 | 2007-10-17 | 伊斯曼化学公司 | Polyester blends with improved stress whitening for film and sheet applications |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105860047A (en) * | 2016-06-14 | 2016-08-17 | 黄山市徽州康佳化工有限责任公司 | Polyester resin for matte powdery coating and preparation method and application thereof |
| CN110563936A (en) * | 2019-09-01 | 2019-12-13 | 合众（佛山）化工有限公司 | Self-flame-retardant antibacterial water-based polyester resin and preparation method thereof |
| CN111995894A (en) * | 2020-09-01 | 2020-11-27 | 梧州市泽和高分子材料有限公司 | Extinction paper-removing additive for thermal transfer powder coating |
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