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Star-shaped hydroxyl polyester adopting polyhydric alcohol as nucleus and preparation method and application of star-shaped hydroxyl polyester

A technology of hydroxyl polyester and polyol, applied in polyurea/polyurethane coatings, coatings, etc., can solve the needs of shortening the activation period of two-component polyurethane coatings, environmental and human health hazards, and the difficulty of applying star-shaped hydroxyl polyesters to environmental protection And other issues

Active Publication Date: 2017-01-04
SOUTH CHINA UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this invention uses heavy metal catalysts to catalyze caprolactone-modified DMPA, which can efficiently catalyze the reaction between hydroxyl groups and NCO groups, and shorten the activation period of the prepared two-component polyurethane coating; Strong hazard, the star-shaped hydroxyl polyester prepared by the method disclosed in the invention is difficult to be applied to the coating field with higher environmental protection requirements such as toys and food filling containers

Method used

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  • Star-shaped hydroxyl polyester adopting polyhydric alcohol as nucleus and preparation method and application of star-shaped hydroxyl polyester
  • Star-shaped hydroxyl polyester adopting polyhydric alcohol as nucleus and preparation method and application of star-shaped hydroxyl polyester
  • Star-shaped hydroxyl polyester adopting polyhydric alcohol as nucleus and preparation method and application of star-shaped hydroxyl polyester

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Raw material composition

[0040] See Table 1 for the raw materials and proportions used in the preparation of the star-shaped hydroxyl polyester SHP-1.

[0041] Table 1

[0042]

[0043] 2. Preparation

[0044] The preparation of star-shaped hydroxyl polyester SHP-1 specifically comprises the steps:

[0045] (1) Add 250.3g of ditrimethylolpropane, 228.3g of caprolactone, and 308.3g of hexahydrophthalic anhydride to a four-necked flask equipped with a mechanical stirrer, a thermometer, a spherical condenser, and a nitrogen port. After reacting for 7 hours under the protection of nitrogen, the infrared characteristic peak of caprolactone in the infrared spectrum detection reaction system disappeared, and the acid value of the detection reaction system dropped to 50% (mass percentage) of its initial value, and the matrix star polyester was obtained by cooling.

[0046] (2) Add 185.0g epichlorohydrin and 1.5g tetraethylammonium bromide to the matrix star polyester...

Embodiment 2

[0063] 1. Raw material composition

[0064] See Table 5 for the raw materials and proportions used in the preparation of the star-shaped hydroxyl polyester SHP-2.

[0065] table 5

[0066]

[0067]

[0068] 2. Preparation

[0069] The preparation of star-shaped hydroxyl polyester SHP-2 specifically comprises the following steps:

[0070] (1) In a four-necked flask equipped with a mechanical stirrer, a thermometer, a spherical condenser, and a nitrogen port, add 250.3g of ditrimethylolpropane, 228.3g of caprolactone, and 296.2g of phthalic anhydride at 110 ℃, reaction under nitrogen protection for 8h, the infrared characteristic peak of caprolactone in the infrared spectrum detection reaction system disappeared, the acid value of the detection reaction system dropped to 50% (mass percentage) of its initial value, and the matrix star polyester was obtained by cooling.

[0071] (2) Add 436g of benzyl glycidyl ether and 2.5g of tetraethylammonium bromide to the matrix star ...

Embodiment 3

[0085] 1. Raw material composition

[0086] See Table 9 for the raw materials and proportions used in the preparation of the star-shaped hydroxyl polyester SHP-3.

[0087] Table 9

[0088]

[0089] 2. Preparation

[0090] The preparation of star-shaped hydroxyl polyester SHP-3 specifically comprises the steps:

[0091] (1) Add 134.2g trimethylolpropane, 114.1g caprolactone, and 308.3g hexahydrophthalic anhydride to a four-necked flask equipped with a mechanical stirrer, a thermometer, a spherical condenser, and a nitrogen port. After reacting for 8 hours under protection, the infrared characteristic peak of caprolactone in the reaction system detected by infrared spectroscopy disappeared, and the acid value of the detected reaction system dropped to 50% (mass percentage) of its initial value, and the matrix star polyester was obtained by cooling down.

[0092] (2) Add 185.0g epichlorohydrin and 1.5g tetrabutylammonium chloride to the matrix star polyester prepared in ste...

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Abstract

The invention discloses star-shaped hydroxyl polyester adopting polyhydric alcoho as a nucleus and a preparation method and an application of the star-shaped hydroxyl polyester. The preparation method comprises the following steps: enabling 1 to 8 molar caprolactone and 1 to 4 molar anhydride to react for 6 to 10 h at 80 to 140 DEG C by adopting 1 molar small molecular polylasic alcohol as a core molecule to obtain a matrix star-shaped polyester, then reacting with 1 to 4 molar monoglycidyl ether at 90 to 150 DEG C to obtain star-shaped hydroxyl polyester. The prepared star-shaped hydroxyl polyester has the advantages of simple synthesis process, high solid content and low viscosity, a hydroxyl value is 140 to 250 mg KOH / g (80 percent of solid content), the viscosity at 25 DEG C when the solid content is 80 percent is 300 to 3000cp, the star-shaped hydroxyl polyester can be cross-linked with a polyurethane curing agent containing an isocyanate group and can be used for preparing a coating with a high solid content, the VOC content at the construction viscosity is smaller than 380 g / L, and the film performance can satisfy the national standard of the solvent-type dual-component polyurethane wood coatings.

Description

technical field [0001] The invention relates to a star-shaped hydroxyl polyester with polyol as the core, in particular to a method for preparing star-shaped hydroxyl polyester by reacting caprolactone, acid anhydride, monoglycidyl ether and small molecular polyol core molecules , and its application in high solids content two-component polyurethane coatings. [0002] technical background [0003] Environmental pollution caused by volatile organic compounds (VOC) and its harm to human health have been paid more and more attention. Paint, as one of the main sources of VOC, has become a social consensus to limit its VOC emissions. Since February 1, 2015, my country has imposed a 4% consumption tax on solvent-based coatings with a VOC content exceeding 420g / L; at the same time, cities including Beijing, Shanghai, and Shenzhen have begun to restrict and eliminate high-pollution, high-VOC solvent-based coatings. This has caused great research and development pressure on paint com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91C08G63/60C08G18/42C09D175/06
CPCC09D175/06C08G18/4286C08G63/60C08G63/914
Inventor 瞿金清黄山朱延安陈荣华
Owner SOUTH CHINA UNIV OF TECH
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