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Transparent reaction type phosphorus-boron-silicon flame-retardant unsaturated polyester and preparation method thereof

An unsaturated and reactive technology, applied in the field of transparent reactive phosphorus silicon boron flame retardant unsaturated polyester and its preparation, to achieve the effect of good thermal bond strength

Inactive Publication Date: 2012-12-05
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 field of unsaturated polyester resin flame retardant technology, so as to provide unsaturated polyester with transparent, high-efficiency halogen-free flame retardant and its preparation method

Method used

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  • Transparent reaction type phosphorus-boron-silicon flame-retardant unsaturated polyester and preparation method thereof
  • Transparent reaction type phosphorus-boron-silicon flame-retardant unsaturated polyester and preparation method thereof
  • Transparent reaction type phosphorus-boron-silicon flame-retardant unsaturated polyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 2 mol of dimethylsilanediol to a 2000ml four-necked flask connected with an HCl absorption device, add 1 mol of phenylphosphoryl dichloride dropwise under stirring, react at 30°C for 4 hours after dropping, and raise the temperature to 100-120°C Heated for 2 hours to obtain a phosphorus-containing silicon monomer, which is denoted as a phosphorus-containing silicon monomer (I);

[0026] Get 0.3mol above-mentioned synthetic phosphorus-containing silicon monomer (I), 0.9mol propylene glycol, 0.5mol maleic anhydride, 0.3mol phthalic anhydride, 0.2mol boric acid and place in 250ml four-necked flask, N 2 Stir under air protection, heat up, raise the temperature to 150-160°C, keep the temperature for 2 hours, further raise the temperature to 180-200°C, react until the acid value of the system remains basically unchanged, stop heating, and obtain an unsaturated polyester pre-prepared polyester containing phosphorus, boron and silicon elements Polymer; cooling to 100°C, add...

Embodiment 2

[0028] Add 2mol Under stirring, add 1 mol of phenylphosphoryl dichloride dropwise, react at 40°C for 6 hours after dropping, heat up to 120-140°C for 3 hours, and obtain a colorless phosphorus-containing silicon monomer, which is recorded as phosphorus-containing silicon monomer ( II);

[0029] Get 0.13mol above-mentioned synthetic phosphorus-containing silicon monomer (II), 0.3mol ethylene glycol, 0.6mol propylene glycol, 0.55mol maleic anhydride, 0.15mol maleic acid, 0.14mol isophthalic anhydride, 0.16mol boric acid in 250ml four-neck flask, N 2 Stir under air protection, heat up, heat up to 150-160°C, react at constant temperature for 2 hours, further raise the temperature to 190-210°C, react until the acid value of the system remains basically unchanged, stop heating, and obtain unsaturated polyester containing phosphorus, boron, and silicon elements Prepolymer; cool to 120°C, add styrene; continue to cool to 50°C, add hydroquinone inhibitor and dicumyl peroxide initiat...

Embodiment 3

[0031] Add 2mol Under stirring, add 1 mol of phenylphosphoryl dichloride dropwise, react at 60°C for 5 hours after dropping, heat up to 140-150°C for 2 hours, and obtain a colorless phosphorus-containing silicon monomer, which is recorded as phosphorus-containing silicon monomer ( III);

[0032] Get 0.15mol of the above-mentioned synthetic phosphorus-containing silicon monomer (III), 0.5mol neopentyl glycol, 0.6mol propylene glycol, 0.4mol maleic anhydride, 0.2mol fumaric anhydride, 0.2mol isophthalic acid, and 0.2mol boric acid in 250ml four-neck flask, N 2 Stir under air protection, raise the temperature to 150-160°C, keep the temperature constant for 2 hours, further raise the temperature to 185-205°C, react until the acid value of the system remains basically unchanged, stop heating, and obtain an unsaturated polyester prepolymer containing phosphorus, boron, and silicon elements ; Cool to 110°C, add vinyl toluene; continue to cool to 40°C, add hydroquinone inhibitor an...

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Abstract

The invention discloses transparent reaction type phosphorus-boron-silicon flame-retardant unsaturated polyester and a preparation method thereof. The transparent reaction type phosphorus-boron-silicon flame-retardant unsaturated polyester consists of the following components in part by mass: 58.5 to 69.85 parts of unsaturated polyester prepolymer containing phosphorus, boron and silicon elements, 30 to 40 parts of crosslinking monomer, 0.05 to 0.5 part of hydroquinone, and 0.1 to 1 part of initiator. The transparent reaction type phosphorus-boron-silicon flame-retardant unsaturated polyesteris prepared by the following steps of: adding the crosslinking monomer when the temperature of the unsaturated polyester prepolymer containing the phosphorus, boron and silicon elements is reduced to100 to 120 DEG C, further reducing the temperature to 35 to 50 DEG C, and adding the hydroquinone and the initiator. The flame retardance of the transparent reaction type phosphorus-boron-silicon flame-retardant unsaturated polyester is high, the limiting oxygen index of a curing product can be increased from 19 percent to 30 percent, and the vertical burning tested by using a 3.2mm spline reaches class UL94V-0; and the three flame-retardant elements, namely phosphorus, silicon and boron are directly introduced to an unsaturated polyester molecular chain, so the thermal-state bonding strengthof the curing product is high.

Description

technical field [0001] The invention relates to unsaturated polyester resins, in particular to a transparent reactive phosphorous silicon boron flame retardant unsaturated polyester and a preparation method thereof. The transparent reactive phosphorous silicon boron flame retardant unsaturated polyester can be used for high performance requirements Insulating materials for electronic and electrical products, building fireproof coatings, shipbuilding materials, flame-retardant glass fiber reinforced plastics, etc. Background technique [0002] Unsaturated polyester (Unsaturated Polyester Resins, referred to as UPR) is a thermosetting plastic widely used in construction, shipbuilding, automobile industry, chemical equipment, electrical and electronic fields. Like most polymer materials, UPR is easy to burn, the limiting oxygen index LOI value is only 19%, and produces a lot of harmful smoke when burning. In many occasions, such as hull parts, electronic and electrical componen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/01C08G63/698C08G63/695C08G63/692
Inventor 刘述梅赵建青
Owner SOUTH CHINA UNIV OF TECH
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