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Hyperbranched hydroxyl polyester resin, and preparation method and application of hyperbranched hydroxyl polyester resin

A technology of hydroxypolyester resin and hydroxypolyester, which is applied in the field of fine chemical synthesis, can solve the problems of difficult control of the reaction end point, high acid value of hyperbranched polyester, and easy formation of gelled products, so as to reduce construction VOC emissions , high solubility and easy reaction end point

Active Publication Date: 2017-04-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the hyperbranched polyester prepared by this method has a high acid value, the reaction end point is difficult to control, and gelation products are easily formed; exploring the preparation method of high-solid and low-viscosity hyperbranched polyester is still a research hotspot and difficulty in this field

Method used

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  • Hyperbranched hydroxyl polyester resin, and preparation method and application of hyperbranched hydroxyl polyester resin
  • Hyperbranched hydroxyl polyester resin, and preparation method and application of hyperbranched hydroxyl polyester resin
  • Hyperbranched hydroxyl polyester resin, and preparation method and application of hyperbranched hydroxyl polyester resin

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A kind of hyperbranched hydroxyl polyester resin (HBP-1), raw material formula mass percent composition is as table 1 (excluding catalyzer):

[0036] Table 1

[0037]

[0038] (2) The preparation technology of this hyperbranched hydroxyl polyester resin (HBP-1), comprises the following steps:

[0039] Mix pyromellitic dianhydride, pentaerythritol, and ethyl acetate uniformly in the reactor according to a given mass, and add catalyst p-toluenesulfonic acid (0.5% of the mass of the anhydride) to react for 2 hours at 120°C under nitrogen protection; Fixed mass of phthalic anhydride, reacted for 3h; added epichlorohydrin, and added catalyst tetraethylammonium bromide (1.0% of epoxy compound mass fraction) and butanone, reacted under nitrogen protection at 110°C for 4h until the acid value was less than 10mgKOH / g, cooling and discharging to obtain hyperbranched hydroxyl polyester resin (HBP-1). attachedfigure 1 It shows that the HBP-1 is the ideal structure of the firs...

Embodiment 2

[0050] (1) A kind of hyperbranched hydroxyl polyester resin (HBP-2), the mass percentage composition of raw material formula is as shown in Table 4 (excluding catalyst):

[0051] Table 4

[0052]

[0053] (2) The preparation technology of this hyperbranched hydroxyl polyester resin (HBP-2), comprises the following steps:

[0054] Mix pyromellitic anhydride, trimethylolpropane, and ethyl acetate uniformly in the reaction kettle according to the given mass, and add the catalyst p-toluenesulfonic acid (0.4% of the mass of the anhydride) to react for 3 hours at 115°C under nitrogen protection; continue Add a given mass of phthalic anhydride and react for 2 hours; add epichlorohydrin, and add catalyst cetyl ammonium bromide (0.5% of the epoxy compound mass fraction) and ethyl acetate to react for 5 hours at 130°C under nitrogen protection to acid The value is less than 10mgKOH / g, the temperature is lowered and the material is discharged to obtain a hyperbranched hydroxyl polyes...

Embodiment 3

[0065] (1) A kind of hyperbranched hydroxyl polyester resin (HBP-3), the mass percentage composition of raw material formula is as shown in Table 7 (excluding catalyst):

[0066] Table 7

[0067]

[0068] (2) The preparation technology of this hyperbranched hydroxyl polyester resin (HBP-3), comprises the following steps:

[0069] Mix 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride, ditrimethylolpropane, and propylene glycol methyl ether acetate in a given mass evenly in the reactor, and add the catalyst p-toluenesulfonic acid ( 0.1% of acid anhydride quality) reacted 3h under 105 ℃ of nitrogen protection; Continue to add the phthalic anhydride of given quality, react 2h; Add E10P, and add catalyst tetraethylammonium bromide (1.2% of epoxide mass fraction) and propylene glycol Methyl ether acetate was reacted at 120°C under nitrogen protection for 5 hours until the acid value was less than 10mgKOH / g, and the temperature was lowered to discharge to obtain hyperbranched ...

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Abstract

The invention discloses hyperbranched hydroxyl polyester resin, and a preparation method and an application of the hyperbranched hydroxyl polyester resin.The preparation method of the hyperbranched hydroxyl polyester resin comprises the following steps: 1) according to molar fraction, 1 part of dicarboxylic anhydride and 2-4 parts of polyhydric alcohol are mixed in a reaction kettle, paratoluenesulfonic acid and an organic solvent are added for reaction at 105-125 degrees under nitrogen protection, then 4-10 parts of phthalic anhydride are added, and reaction for 2-3h is carried out; and 2) according to molar fraction, 6-10 parts of epoxy compounds are added to a matrix prepared in the step 1), a catalyst and an organic solvent are added for reaction for 4-6h at 105-1130 degrees under the nitrogen protection till an acid value is less than 10mgKOH / g, and cooling and discharging are carried out. The solid content of the hyperbranched hydroxyl polyester resin reaches above 70%, and the viscosity is 3000-12000mPa.s. High solid-content bi-component polyurethane dope prepared with the adoption of the hyperbranched hydroxyl polyester resin has high construction solid content, low VOC content, high film hardness, good heat resistance and outstanding anti-corrosion property.

Description

technical field [0001] The invention relates to a polyester resin, in particular to a hyperbranched hydroxyl polyester resin and its preparation method and application, belonging to the field of fine chemical synthesis. Background technique [0002] The development trend of coatings is to develop environmentally friendly coatings, including high solids coatings, water-based coatings, powder coatings and UV curing coatings. Hyperbranched polyester has a highly branched, compact three-dimensional spherical shape, less entanglement between molecular chains, and a lower viscosity than linear polymers of the same molecular weight in solution or molten state. The use of hyperbranched polyester in coatings can reduce the viscosity of coatings, increase the solid content of coatings, and reduce the content of volatile organic compounds (VOC) in coatings. In addition, hyperbranched hydroxyl polyester resin contains multiple hydroxyl groups, which can prepare high-performance two-com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09D175/04C09D5/08
Inventor 瞿金清刘晚秋张凯旋
Owner SOUTH CHINA UNIV OF TECH
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