CN107619471A - High levelling polyester resin of high acid value of HAA solidifications and preparation method thereof - Google Patents
High levelling polyester resin of high acid value of HAA solidifications and preparation method thereof Download PDFInfo
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- CN107619471A CN107619471A CN201710857480.7A CN201710857480A CN107619471A CN 107619471 A CN107619471 A CN 107619471A CN 201710857480 A CN201710857480 A CN 201710857480A CN 107619471 A CN107619471 A CN 107619471A
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Abstract
The present invention provides a kind of high levelling polyester resin of high acid value of HAA solidifications and preparation method thereof, and the polyester resin includes the raw material of following parts by weight：Wherein polyester resin includes the raw material of following parts by weight：30 50 parts of neopentyl glycol；0 10 parts of ethylene glycol；0.5 3 parts of 2 butyl, 2 ethyl, 1,3 propane diols；0 10 parts of trimethylolpropane；30 65 parts of terephthalic acid (TPA)；1,4 0 15 parts of cyclohexane cyclohexanedimethanodibasics；5 30 parts of M-phthalic acid；1 20 parts of adipic acid.Polyester adjusts the rational proportion of each raw material, and using the 55mgKOH/g of high acid value 45, low-viscosity, 160 DEG C of solidifications of low temperature, reaction speed is fast, and film crosslink density is big, and impact strength is good, and weatherability is more preferable, and hydrolytic resistance is good, and high levelling.
Description
Technical field
The invention belongs to polymeric material field, is related to a kind of polyester resin, more particularly to a kind of high acid value of HAA solidifications
High levelling polyester resin and preparation method thereof.
Background technology
Powdery paints has solvent-free, pollution-free, recyclable, environmentally friendly, the saving energy and resource, reduces labor intensity and apply
The features such as film high mechanical strength, thus be rapidly developed, it is widely used in household electrical appliances, car paint, aluminum alloy doors and windows and gold
Category and nonmetallic external decoration coating protection.
At present because environmental requirement, TGIC are disabled in developed countries such as America and Europes as curing agent.And replaced as it
For product, HAA (hydroxyalkyl amide) does not have genetoxic, and reaction is fast, does not reduce the glass transition temperature of powdery paints, improves
Storage stability, and low-temperature curable.
But HAA/ polyester powder coatings there is also it is certain the defects of, had during solidification hydrone spilling, applying
Film surface can produce pin hole, not only influenceed outward appearance but also can cause hydrolytic resistance, the decline of chemical resistance.
Most of patent of existing HAA curing types uses acid number 28~37 to obtain high levelling, so required
Curing dose is few, and crosslink density is low, and moisture caused by reaction is also few, and curing rate is slow, but can influence impact strength and resistance to
Hou Xing, hydrolytic resistance.
The content of the invention
The present invention is in order to solve the above problems, there is provided a kind of high levelling polyester resin of high acid value of HAA solidifications, reaches preparation
The purpose of high acid value but levelling is excellent, hydrolytic resistance is good polyester resin.
For achieving the above object, the present invention uses following technical scheme：
A kind of preparation method of the high levelling polyester resin of high acid value of HAA solidifications, comprises the following steps：
Wherein polyester resin includes the raw material of following parts by weight：
Reactor is warming up to 70-100 DEG C, by the parts by weight weigh RAW MATERIALS Neopentyl glycol, ethylene glycol, 2- butyl-
2- ethyls -1,3-PD, Isosorbide-5-Nitrae-cyclohexane cyclohexanedimethanodibasic, trimethylolpropane, p-phthalic acid, esterification catalyst, in nitrogen
It is gradually heated up being warming up to 235-245 DEG C of maintenance under the protection of gas, until the acid number measured is 5-10mgKOH/g, is then cooled to
210-220 DEG C, end-capping reagent M-phthalic acid or/and adipic acid are put into, is warming up to 238-245 DEG C of maintenance, until reactant acid number
For 62-66mgKOH/g, vacuumizing is carried out, until reactant acid number is 48-55mgKOH/g, is cooled to 205-210 DEG C, input
Antioxidant, 15-30 minutes are maintained to discharge.
Further, the polyester resin includes the raw material of following parts by weight：
Further, reactor is warming up to 85 DEG C.
Further, esterification catalyst is one in monobutyltin oxide, dibutyltin oxide, stannous oxalate, stannous octoate
Kind is several.
The present invention also provides a kind of high levelling polyester tree of high acid value of the HAA solidifications obtained according to above-mentioned preparation method
Fat.
Further, wherein polyester resin includes the raw material of following parts by weight：
Further, wherein polyester resin includes the raw material of following parts by weight：
Compared with prior art, the technical program has advantages below：
The polyester of the present invention adjusts the rational proportion of each raw material, and using high acid value 45-55mgKOH/g, 160 DEG C of low temperature is solid
Change, low-viscosity, reaction speed are fast, and crosslink density is big, and impact strength is good, and weatherability is more preferable, and levelling is excellent, hydrolytic resistance is good.
Although acid number is high, caused moisture is slightly more, does not interfere with film coated surface, still light, levelling are fine on surface.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1：
Raw material is weighed by following mass fraction, prepares polyester resin
Reactor is warming up to 85 DEG C, adds neopentyl glycol, ethylene glycol, the 2- butyl -2- ethyls -1,3- of said ratio amount
Propane diols, Isosorbide-5-Nitrae-cyclohexane cyclohexanedimethanodibasic, trimethylolpropane, p-phthalic acid, esterification catalyst, under the protection of nitrogen by
235-245 DEG C of maintenance is gradually heated to, until the acid number measured is 5-10mgKOH/g, 210-220 DEG C is then cooled to, throws
Enter end-capping reagent M-phthalic acid or/and adipic acid, be warming up to 238-245 DEG C of maintenance, until reactant acid number is 62-66mgKOH/
G, vacuumizing is carried out, until reactant acid number is 48-55mgKOH/g, be cooled to 205-210 DEG C, put into antioxidant, maintain
It can discharge within 20 minutes.
Embodiment 2-4 preparation method and embodiment 1 are basically identical, and only proportioning is different.Specific embodiment 1-4 polyester
Match as shown in the table：
The embodiment 1-4 of table 1 proportioning table
Its major parameter of polyester resin is as shown in table 2 as made from upper table 1.
Obtained polyester resin adds filler, levelling agent, optical brightener, curing agent, is extruded after well mixed through extruder, uses
Flour mill is milled, and is then screened into powdery paints.The condition of cure of the powdery paints prepared through such a method is 160 DEG C/10-
15min, it is easy for construction, it is easy to reclaim, energy-conserving and environment-protective.
Polyester resin made from the embodiment 1-4 of table 2 and its performance parameter after powder processed
As shown in upper table 2, embodiment 1-4 various performance parameters are all preferable, and wherein embodiment 4 is rushed by 1kg x 50cm
Hit, Tg is also higher, and levelling is excellent, and surface does not have pin hole, has taken into account hydrolytic resistance and weatherability.
Although the present invention is disclosed as above with preferred embodiment, it is not for limiting the present invention, any this area
Technical staff without departing from the spirit and scope of the present invention, may be by the methods and technical content of the disclosure above to this hair
Bright technical scheme makes possible variation and modification, therefore, every content without departing from technical solution of the present invention, according to the present invention
Any simple modifications, equivalents, and modifications made to above example of technical spirit, belong to technical solution of the present invention
Protection domain.
Claims (7)
1. a kind of preparation method of the high levelling polyester resin of high acid value of HAA solidifications, it is characterised in that the preparation method includes
Following steps：
Wherein polyester resin includes the raw material of following parts by weight：
Reactor is warming up to 70-100 DEG C, RAW MATERIALS Neopentyl glycol, ethylene glycol, 2- butyl -2- second are weighed by the parts by weight
Base -1,3-PD, Isosorbide-5-Nitrae-cyclohexane cyclohexanedimethanodibasic, trimethylolpropane, p-phthalic acid, esterification catalyst, in nitrogen
It is gradually heated up being warming up to 235-245 DEG C of maintenance under protection, until the acid number measured is 5-10mgKOH/g, is then cooled to 210-
220 DEG C, end-capping reagent M-phthalic acid or/and adipic acid are put into, is warming up to 238-245 DEG C of maintenance, until reactant acid number is 62-
66mgKOH/g, vacuumizing is carried out, until reactant acid number is 48-55mgKOH/g, be cooled to 205-210 DEG C, put into antioxygen
Agent, 15-30 minutes are maintained to discharge.
2. the preparation method of the high levelling polyester resin of high acid value of HAA solidifications according to claim 1, it is characterised in that
The polyester resin includes the raw material of following parts by weight：
3. the preparation method of the high levelling polyester resin of high acid value of HAA solidifications according to claim 1, it is characterised in that
Reactor is warming up to 85 DEG C.
4. the preparation method of the high levelling polyester resin of high acid value of HAA solidifications according to claim 1, it is characterised in that
Esterification catalyst is the one or more in monobutyltin oxide, dibutyltin oxide, stannous oxalate, stannous octoate.
5. a kind of high levelling of high acid value for the HAA solidifications that preparation method according to described in claim 1-4 any one obtains gathers
Ester resin.
6. the high levelling polyester resin of high acid value of HAA solidifications as claimed in claim 5, it is characterised in that wherein polyester resin bag
Include the raw material of following parts by weight：
7. the high levelling polyester resin of high acid value of HAA solidifications as claimed in claim 6, it is characterised in that wherein polyester resin bag
Include the raw material of following parts by weight：
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710857480.7A CN107619471A (en) | 2017-09-21 | 2017-09-21 | High levelling polyester resin of high acid value of HAA solidifications and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710857480.7A CN107619471A (en) | 2017-09-21 | 2017-09-21 | High levelling polyester resin of high acid value of HAA solidifications and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107619471A true CN107619471A (en) | 2018-01-23 |
Family
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710857480.7A Pending CN107619471A (en) | 2017-09-21 | 2017-09-21 | High levelling polyester resin of high acid value of HAA solidifications and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108409948A (en) * | 2018-04-25 | 2018-08-17 | 黄山市向荣新材料有限公司 | A kind of HAA systems low temperature curing polyester resin and the preparation method and application thereof |
| CN109503820A (en) * | 2018-12-03 | 2019-03-22 | 安徽恒明工程技术有限公司 | A kind of fast low temperature cure type polyester resin and preparation method thereof |
| CN109762145A (en) * | 2018-11-30 | 2019-05-17 | 安徽神剑新材料股份有限公司 | A kind of hydroxyalkyl amide solidification thermal transfer powdery paints carboxyl end group saturated polyester resin and its synthetic method |
| CN110128640A (en) * | 2019-05-15 | 2019-08-16 | 江苏达美瑞新材料有限公司 | A kind of HAA solidifies indoor polyester resin for powder coating and preparation method thereof, the powdery paints containing the polyester resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516511A (en) * | 2011-11-14 | 2012-06-27 | 中国电器科学研究院有限公司 | Polyester resin for high-performance aqueous coating and preparation method thereof |
| CN103304790A (en) * | 2013-06-06 | 2013-09-18 | 广东伊诗德新材料科技有限公司 | Polyester resin for outdoor aluminum profile heat transfer printing powder coating and preparation method thereof |
| CN104448265A (en) * | 2014-11-19 | 2015-03-25 | 广州擎天材料科技有限公司 | Polyester resin for low-temperature-cured and energy-saving thermal-transfer-printing powdery coating material and preparation method thereof |
-
2017
- 2017-09-21 CN CN201710857480.7A patent/CN107619471A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516511A (en) * | 2011-11-14 | 2012-06-27 | 中国电器科学研究院有限公司 | Polyester resin for high-performance aqueous coating and preparation method thereof |
| CN103304790A (en) * | 2013-06-06 | 2013-09-18 | 广东伊诗德新材料科技有限公司 | Polyester resin for outdoor aluminum profile heat transfer printing powder coating and preparation method thereof |
| CN104448265A (en) * | 2014-11-19 | 2015-03-25 | 广州擎天材料科技有限公司 | Polyester resin for low-temperature-cured and energy-saving thermal-transfer-printing powdery coating material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108409948A (en) * | 2018-04-25 | 2018-08-17 | 黄山市向荣新材料有限公司 | A kind of HAA systems low temperature curing polyester resin and the preparation method and application thereof |
| CN109762145A (en) * | 2018-11-30 | 2019-05-17 | 安徽神剑新材料股份有限公司 | A kind of hydroxyalkyl amide solidification thermal transfer powdery paints carboxyl end group saturated polyester resin and its synthetic method |
| CN109503820A (en) * | 2018-12-03 | 2019-03-22 | 安徽恒明工程技术有限公司 | A kind of fast low temperature cure type polyester resin and preparation method thereof |
| CN110128640A (en) * | 2019-05-15 | 2019-08-16 | 江苏达美瑞新材料有限公司 | A kind of HAA solidifies indoor polyester resin for powder coating and preparation method thereof, the powdery paints containing the polyester resin |
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