A kind of synthetic method for uv-led cured terminal vinyl water-based flame-retardant polyester

A UV-LED and flame-retardant polyester technology, which is applied in the direction of polyester coatings, coatings, fire-resistant coatings, etc., can solve the problems of hydrolysis resistance, coating film performance and poor flame-retardant performance, and achieve low cost and weaken hydrogen Bonding effect, effect of high grafting rate

Active Publication Date: 2021-08-10
CHINA THREE GORGES UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the defects of poor hydrolysis resistance, coating film performance and flame retardancy of the existing water-based polyester resin, the present invention provides a method of introducing phosphate ester and vinyl structure into the water-based polyester structure and applying it to UV-LED curing In the field of water-based flame-retardant coatings, a method for preparing UV-LED cured water-based vinyl-terminated water-based flame-retardant polyester with improved medium resistance, coating film performance and flame-retardant properties of the coating film

Method used

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  • A kind of synthetic method for uv-led cured terminal vinyl water-based flame-retardant polyester
  • A kind of synthetic method for uv-led cured terminal vinyl water-based flame-retardant polyester
  • A kind of synthetic method for uv-led cured terminal vinyl water-based flame-retardant polyester

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A kind of synthesis that is used for UV-LED curing terminal vinyl water-based flame retardant polyester, the raw material type and consumption of each component are shown in Table 1 (xylene is used as water-carrying agent):

[0032] Table 1:

[0033]

[0034] Preparation process: in parts by mass, add 50.9g phthalic acid, 35g trimethylolpropane, 5g castor oil and 5g phosphoric acid into the reaction kettle, add xylene as water-carrying agent, and raise the temperature under the protection of nitrogen to 190°C, reflux reaction until the acid value is 9mgKOH / g, extract xylene under reduced pressure; cool down to 130°C, extract water-carrying agent xylene under reduced pressure at a vacuum degree of 0.04-0.1MPa, add 2g maleic anhydride, React for 3 to 5 hours; keep the temperature of the system constant, add 2g of hydroxyethyl acrylate and 0.1g of p-methoxyphenol, react for 4 hours, and obtain an adduct containing a hydrophilic group and a vinyl group; cool down to 50°C...

Embodiment 2

[0045] A kind of synthesis that is used for UV-LED curing terminal vinyl water-based flame-retardant polyester, the raw material type and consumption of each component are shown in Table 4 (xylene is used as water-carrying agent):

[0046] Table 4:

[0047]

[0048]

[0049] Preparation process: in parts by mass, add 50.9g phthalic acid, 5g phosphoric acid, 35g trimethylolpropane and 5g hydroxylated tung oil with multiple double bonds into the reactor, add xylene as water-carrying agent, Under protection, raise the temperature to 190°C, reflux to react to an acid value of 8 mgKOH / g, cool down to 130°C, extract the water-carrying agent xylene under reduced pressure at a vacuum degree of 0.04-0.1 MPa; add 2g of maleic anhydride, and react for 3 hours; Keep the temperature of the system constant, add 2g hydroxyethyl acrylate and 0.1g p-methoxyphenol, react for 4 hours, and obtain an adduct containing hydrophilic groups and vinyl groups; cool down to 50°C, add 0.8g triethyla...

Embodiment 3

[0059] A kind of synthesis that is used for UV-LED curing terminal vinyl water-based flame-retardant polyester, the raw material type and consumption of each component are shown in Table 7 (xylene is used as water-carrying agent):

[0060] Table 7:

[0061]

[0062] Preparation process: In parts by mass, 51.8g of phthalic acid, 6g of phosphoric acid, 30g of pentaerythritol and 6g of castor oil were added to the reaction kettle, xylene was added as a water-carrying agent, and the temperature was raised to 190°C under the protection of nitrogen. Reflux reaction until the acid value is lower than 10mgKOH / g, extract the xylene under reduced pressure; cool down to 130°C, extract the water-carrying agent xylene under reduced pressure at a vacuum degree of 0.04-0.1MPa, add 3g of maleic anhydride, and react for 3- 5h; keep the temperature of the system constant, add 3g hydroxypropyl acrylate and 0.2g p-methoxyphenol, react for 3~5h, and get the adduct containing hydrophilic group a...

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Abstract

The invention discloses a water-based flame-retardant polyester used for UV-LED curing terminal vinyl and a synthesis method thereof. The synthesis method is as follows: add polybasic acid, polyol, functional flame-retardant polyhydroxy compound and functional multi-double bond hydroxylated vegetable oil into the reaction kettle, add organic solvent as water-carrying agent, and heat up to 180~210 o C, reflux reaction until the acid value is lower than 10 mgKOH / g, extract the organic solvent under reduced pressure; cool down to 120~150 o C, add maleic anhydride to react; keep the temperature of the system constant, add metered vinyl functional monomers and polymerization inhibitors containing hydroxyl structures, react for 3 to 5 h, and obtain a mixture containing hydrophilic groups and vinyl groups adducts; cooling to 40~60 o C. Add a neutralizing agent to obtain a carboxylate polyester containing vinyl groups; add deionized water to emulsify and disperse to obtain a UV‑LED curable vinyl-terminated water-based polyester. The vinyl water-based polyester obtained in the present invention has excellent medium resistance, coating film hardness and flexibility, and is very suitable for UV-LED curing water-based coatings.

Description

technical field [0001] The invention relates to the field of UV-LED curing water-based flame-retardant coatings, in particular to a preparation method for UV-LED curing terminal vinyl water-based flame-retardant polyester. Background technique [0002] Polyester resin systems are widely used in the field of coatings because of their excellent gloss, fullness, impact resistance, flexibility, weather resistance and adhesion. However, polyester is still mainly solvent-based at present. With the improvement of people's awareness of environmental protection, environmental protection laws and regulations on the content of volatile organic compounds (VOC) in coatings are becoming more and more stringent, and coating products with low VOC or even zero VOC are increasingly favored by the market. On the other hand, polyester resins are extremely flammable. With the increasing safety requirements, halogen-free flame-retardant polyester resins are particularly urgent. Therefore, it is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/91C08G63/692C09D167/07C09D5/18
CPCC08G63/6928C08G63/918C09D5/18C09D167/07
Inventor 汪磊李德江周昌林
Owner CHINA THREE GORGES UNIV
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