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Ultraviolet-cured transparent halogen-free flame-retardant unsaturated polyester and preparation method thereof

An unsaturated and ultraviolet light technology, applied in the field of halogen-free flame retardant unsaturated polyester resin, can solve the problems of volatilization and loss, and achieve the effect of enhanced oxidation resistance and heat resistance.

Active Publication Date: 2012-12-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention focuses on solving the problems existing in the volatilization loss and halogen-free flame retardancy of the existing unsaturated polyester resin, and provides a UV-curable transparent halogen-free flame-retardant unsaturated polyester;

Method used

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  • Ultraviolet-cured transparent halogen-free flame-retardant unsaturated polyester and preparation method thereof
  • Ultraviolet-cured transparent halogen-free flame-retardant unsaturated polyester and preparation method thereof
  • Ultraviolet-cured transparent halogen-free flame-retardant unsaturated polyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 1.2mol 1,3-propanediol, 0.55mol maleic anhydride, 0.2mol maleic anhydride and 9,10-dihydro-9-oxa-10- The addition product of phosphaphenanthrene-10-oxide (DOPO) and 0.25mol boric acid are heated up to 150-160°C, kept at a constant temperature for 2 hours, then heated up to 180-205°C for reaction, and the outlet temperature of the distillation is controlled to be lower than 100°C. Measure the acid value every 1 hour, stop heating when the acid value is lower than 40mg KOH / g, and cool to 100°C to obtain a phosphorus-boron flame-retardant unsaturated polyester prepolymer; add hydroxyethyl acrylate, cool to room temperature, and add After hydroquinone and benzoin butyl ether, stir at room temperature for 30 minutes to obtain UV-curable transparent halogen-free flame-retardant unsaturated polyester; 1 part of hydroxyethyl acrylate, 0.1 part of hydroquinone and 0.4 part of benzoin butyl ether. The general structural formula of the obtained phosphorus-boron flame-retardan...

Embodiment 2

[0032]Add 0.5mol ethylene glycol, 0.6mol 1,2-propanediol, 0.55mol maleic anhydride, 0.15mol maleic acid, 0.15mol itaconic anhydride and DOPO to a 500ml three-necked flask equipped with a thermometer, a stirrer, and a distillation branch pipe. Addition product and 0.15mol boric acid, heat up to 150-160°C, hold constant temperature for about 2 hours, then heat up to 180-205°C to react, control the distillation outlet temperature below 100°C, measure the acid value every 1 hour, when the acid value Stop heating when it is lower than 40mg KOH / g, cool to 120°C to obtain phosphorus boron flame retardant unsaturated polyester prepolymer; add hydroxyethyl acrylate and triethylene glycol diacrylate, cool to room temperature, add p-tert-butyl o- After hydroquinone and benzoin dimethyl ether (Irgacure 651), stir at room temperature for 60 minutes to obtain UV-curable transparent halogen-free flame-retardant unsaturated polyester; polymer, 32 parts hydroxyethyl acrylate, 13 parts triethyl...

Embodiment 3

[0036] Add 0.65 mol of diethylene glycol, 0.6 mol of 1,3-propanediol, 0.4 mol of maleic anhydride, 0.2 mol of fumaric anhydride, 0.2 mol of itaconic anhydride into a 500ml three-necked flask equipped with a thermometer, a stirrer, and a distillation branch pipe With the addition product of DOPO and 0.2mol boric acid, heat up to 150-160°C, keep the temperature for about 2 hours, then raise the temperature to 180-205°C to react, control the distillation outlet temperature to be lower than 100°C, and measure the acid value every 1 hour. Stop heating when the acid value is lower than 40mg KOH / g, and cool to 110°C to obtain a phosphorus-boron flame-retardant unsaturated polyester prepolymer; add hydroxyethyl acrylate, propoxylated neopentyl glycol diacrylate and three Methylol propane triacrylate, cooled to room temperature, after adding methyl hydroquinone and 4,4-dimethylaminobenzophenone (Michler's ketone), stirred at room temperature for 40 minutes to obtain UV-curable transpare...

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Abstract

The invention discloses an ultraviolet-cured transparent halogen-free flame-retardant unsaturated polyester and preparation method thereof. A raw material formula comprises the following raw materials in percentage by mass: 49.5-65 percent of a phosphorus-boron flame-retardant unsaturated polyester prepolymer, 50-30 percent of an active diluent, 0.4-4.5 percent of a photoinitiator and 0.1-0.5 percent of a polymerization inhibitor, wherein the phosphorus-boron flame-retardant unsaturated polyester prepolymer is prepared by reacting dibasic alcohol, unsaturated dibasic anhydride and / or unsaturated dicarboxylic acid, a phosphaphenanthrene anhydride derivative and boric acid at the temperature of 150-205 DEG C. The volatilization loss rate in the curing process of unsaturated polyester is less than 1 percent, the appearance is transparent before curing and after curing, and vertical combustion passes through a grade UL94 V-0; and the ultraviolet-cured transparent halogen-free flame-retardant unsaturated polyester has the advantages of low volatilization loss, freeness from halogen, flame retardance, transparence and the like.

Description

technical field [0001] The invention relates to a halogen-free flame-retardant unsaturated polyester resin, in particular to a UV-cured transparent halogen-free flame-retardant unsaturated polyester and a preparation method thereof. This kind of unsaturated polyester has a transparent appearance and moderate viscosity, and can be used as ink, electronic packaging, adhesive, printing plate, etc. Background technique [0002] Unsaturated polyester (UPR for short) is a thermosetting resin with a large output, which is commonly used for heating and curing. Due to the high saturated vapor pressure (853Pa at 25°C), strong volatility, strong odor, and irritating styrene Thinners will emit unpleasant odors during the process of dipping and baking, which is not only a serious waste, but also a great hazard to operators and the surrounding environment. Ultraviolet (UV) curing has the advantages of fast curing speed, energy saving, high production efficiency, and good coating performa...

Claims

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Application Information

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IPC IPC(8): C08F283/01C08G63/698
Inventor 刘述梅孙志松赵建青袁彦超
Owner SOUTH CHINA UNIV OF TECH
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