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Low-viscosity heteroarm star-shaped hydroxyl resin with multiple epoxy compounds as the core and its preparation method and application

A technology of epoxy compounds and hydroxyl resins, which is applied in the preparation of organic compounds, the preparation of ester groups and hydroxyl groups, chemical instruments and methods, etc. It can solve the problems of high viscosity of hyperbranched polyester, difficulty in controlling the synthesis process, and difficulty in construction and use, etc. problems, to achieve the effect of reducing the overall viscosity, light product color, and adjusting the pot life

Active Publication Date: 2020-05-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese invention patent CN101583650A discloses a method of synthesizing hyperbranched polyesters by reacting polycarboxylic acids and their derivatives with polyols, but the hyperbranched polyesters synthesized by them have extremely high viscosity at room temperature, making it difficult to carry out construction and use, and the synthesis process is not easy controlled, prone to gelation

Method used

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  • Low-viscosity heteroarm star-shaped hydroxyl resin with multiple epoxy compounds as the core and its preparation method and application
  • Low-viscosity heteroarm star-shaped hydroxyl resin with multiple epoxy compounds as the core and its preparation method and application
  • Low-viscosity heteroarm star-shaped hydroxyl resin with multiple epoxy compounds as the core and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0050] 1) The low-viscosity heteroarm star-shaped hydroxyl resin (SHP-1) with multiple epoxy compounds as the core, the composition of raw materials is shown in Table 1:

[0051] Table 1

[0052]

[0053] 2) if figure 1 Shown, polyvalent epoxy compound is the preparation technology of the low-viscosity heteroarm star-shaped hydroxyl resin (SHP-1) of nucleus, comprises the following steps:

[0054] Mix the given amount of 1,2-propanediol, caprolactone, and anhydrous zinc acetate in the reaction kettle evenly, raise the temperature to 100°C, and react under the protection of nitrogen. The infrared spectrum of caprolactone in the reaction system is detected by infrared spectroscopy. The characteristic peak disappears, and when the solid content of the detection reaction system is >99%, the reaction reaches the end point to obtain a star-shaped resin branch (arm); Methyl triglycidyl ether, drop it within 2 hours, raise the temperature to 60°C, react for 4 hours until the epox...

Embodiment 2

[0069] 1) The low-viscosity heteroarm star-shaped hydroxyl resin (SHP-2) with multiple epoxy compounds as the core, the raw material composition is shown in Table 4:

[0070] Table 4

[0071]

[0072] 2) The multi-component epoxy compound is the preparation process of the low-viscosity heteroarm star-shaped hydroxyl resin (SHP-2) of the core, comprising the following steps:

[0073] Mix a given amount of 1,2-propanediol, caprolactone, and anhydrous zinc acetate evenly in the reaction kettle, raise the temperature to 120°C, and react under the protection of nitrogen, and detect the disappearance of the infrared characteristic peak of caprolactone in the reaction system by infrared spectroscopy , when detecting the solid content of the reaction system > 99%, the reaction reaches the end point to obtain a star-shaped resin branch (arm); add n-hexanol, cationic ring-opening catalyst boron trifluoride ether, and drop a given mass of trimethylol at 30°C Triglycidyl ether, drop i...

Embodiment 3

[0084] 1) The low-viscosity heteroarm star-shaped hydroxyl resin (SHP-3) with multiple epoxy compounds as the core, the raw material composition is shown in Table 7:

[0085] Table 7

[0086]

[0087] 2) The multi-component epoxy compound is the preparation process of the low-viscosity heteroarm star-shaped hydroxyl resin (SHP-3) of the core, comprising the following steps:

[0088] Mix a given amount of 1,2-butanediol, caprolactone, and dibutyltin dilaurate evenly in a reaction kettle, raise the temperature to 130°C, and react under nitrogen protection, and detect the infrared spectrum of caprolactone in the reaction system by infrared spectroscopy. The characteristic peak disappears, and when the solid content of the detection reaction system is >99%, the reaction reaches the end point to obtain a star-shaped resin branch (arm); add n-hexanol, cationic ring-opening catalyst boron trifluoride ethanol, and drop a given mass of pentaerythritol at 30°C The tetraglycidyl ethe...

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Abstract

The invention discloses low viscosity miktoarm star hydroxyl resin taking a polynary epoxy compound as a nucleus as well as a preparation method and an application of the low viscosity miktoarm star hydroxyl resin. The preparation method comprises the steps of uniformly mixing 1-4 parts of dihydric alcohol and 1-4 parts of caprolactone in a reaction kettle, adding a ring opening catalyst for reaction at 100-130 DEG C till an infrared characteristic peak disappears, finishing the reaction when a system solid content is greater than 99%, adding unitary primary alcohol, dropwise adding the polynary epoxy compound, performing reaction under the action of a cation ring opening catalyst till an epoxy value reaches a theoretical value, finishing the reaction, and performing cooling and discharging. The resin has the advantages of simple synthesis technology, high solid content, low viscosity, long shelf life and the like; the solid content reaches 100%; the viscosity is as low as 1000-5000 mpa.s; the shelf life is as long as 4-8 hours; the resin can be cross-linked with an isocyanate curing agent for curing to prepare high solid content paint; a VOC content of the resin is less than 340 g / L at the construction viscosity.

Description

technical field [0001] The invention relates to a low-viscosity hydroxyl resin, in particular to a low-viscosity heteroarm star-shaped hydroxyl resin with multiple epoxy compounds as the core, its preparation method and application. Background technique [0002] Polyurethane resin refers to a polymer resin containing carbamate, urea, allophanate and other groups in its molecular chain. Polyurethane coatings have excellent physical and chemical properties-high gloss, good flexibility, and UV stability. Good, chemical resistance, etc., and are widely used in wood, plastics, automobiles, aerospace, ink and other fields. However, most of the products currently on the market are traditional solvent-based polyurethane coatings. With the establishment of environmental protection regulations in various countries and the enhancement of people's environmental awareness, it is imminent to reduce VOC emissions, which greatly promotes the development of high-solid content polyurethane co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/675C07C67/03C07C67/29C08G18/32C09D175/04
Inventor 瞿金清刘晚秋
Owner SOUTH CHINA UNIV OF TECH