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Reaction-type transparent halogen-free flameproof unsaturated polyester and preparation method thereof

An unsaturated and reactive technology, applied in the synthesis field of reactive transparent halogen-free flame retardant unsaturated polyester, to achieve the effect of moderate viscosity and long-term stable electrical properties

Inactive Publication Date: 2009-03-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention focuses on solving the problems existing in the field of unsaturated polyester resin flame retardant technology, so as to provide transparent unsaturated polyester resin with reactive halogen-free flame retardant performance

Method used

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  • Reaction-type transparent halogen-free flameproof unsaturated polyester and preparation method thereof
  • Reaction-type transparent halogen-free flameproof unsaturated polyester and preparation method thereof
  • Reaction-type transparent halogen-free flameproof unsaturated polyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 102.6 mL of ethylene glycol to the three-necked flask, stir with a magnetic stirrer, and slowly drop 100 mL of phenylphosphoryl dichloride under the condition of ice water cooling. After the reaction was stopped, the excess ethylene glycol was distilled off under reduced pressure at 100° C. to obtain 161.5 g of a colorless liquid flame retardant phenyl di(ethylene glycol) phosphate.

[0036] Take 30g of the above synthesized flame retardant, add 16.6g of phthalic anhydride, 25g of maleic anhydride and 28.4g of propylene glycol, and place them in a 250ml four-necked flask. 2 Stir mechanically under air protection, heat with an electric heating mantle, slowly raise the temperature to 150°C at a rate of 5°C / min, react at a constant temperature for 1 hour, continue to slowly increase the reaction temperature at a rate of 5°C / min, and control the distillation outlet temperature to be lower than 100°C. The heating is stopped when the acid value of the unsaturated polyester is...

Embodiment 2

[0038] A three-necked flask was charged with 192.4 g of resorcinol and 112 mL of xylene. N 2 protection. The temperature was raised to 125°C and refluxed. After the resorcinol was completely melted, it was stirred with a magnetic stirrer, and 113.5g of phenylphosphoryl dichloride was slowly dropped into it. After the addition was completed, the reaction was continued at 125°C for 9 hours. After stopping the reaction, xylene was distilled off under reduced pressure at 120°C. NaHCO for crude products 3 The aqueous solution is washed until no gas is released, and then washed twice with distilled water. After vacuum drying at 45°C for 24 hours, 99.6 g of a reddish-brown liquid flame retardant phenylphosphonate bis(resorcinol) ester was obtained.

[0039] Take 40g of the above synthesized flame retardant, 20.7g of isophthalic anhydride, 12g of maleic acid, 18.6g of propylene glycol and 8.7g of ethylene glycol, and place them in a 250ml four-necked flask. 2 Stir under air protection, he...

Embodiment 3

[0041] Melt polycondensation reaction of 100g of fumaric acid, phthalic anhydride, bis(2-carboxyethyl)methyl phosphorous oxide, propylene glycol, and neopentyl glycol with a molar ratio of 2:1:1:2:2 , Heating up to 155°C at a rate of 9°C / min, N 2 Stir mechanically under air protection, react at a constant temperature for 1 hour, then slowly increase the temperature at a rate of 5°C / min, and control the distillation outlet temperature to be lower than 100°C. The acid value of the unsaturated polyester was monitored. At the end of the reaction, the temperature was lowered to 110°C, and 35% of the total mass of the resin, 0.03g tert-butylcatechol and 2g tert-butyl peroxybenzoate were added in sequence to obtain a certain viscosity The light yellow transparent unsaturated polyester product.

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Abstract

The invention discloses a method for preparing a reaction type transparent halogen-free flame retardation unsaturated polyester. A program temperature control melting polycondensation reaction method is adopted; C2-6 dihydric alcohol, C3-8 saturated binary acid or anhydride, C4 unsaturated binary acid or anhydride, and a difunctional reactivity phosphatic flame retardant are used to synthesize an unsaturated polyester oligomer; styrene is taken as a crosslinking agent to prepare the unsaturated polyester which can be solidified at room temperature with transparent appearance, moderate viscosity and lower cost. After solidification, no added dissociated flame retardant component is contained in the cross linked network of the unsaturated polyester. The mechanical property, the flame retardation property and the electricity property of the product can be stable in a long period, the oxygen index of the product can be increased from 19 to 29 percent, and the product can pass the vertical firing UL94-V0 level. The reaction type transparent halogen-free flame retardation unsaturated polyester can be applied to the field of electronic and electric appliance insulating materials with higher performance requirements, construction flame retardation coating, ship-building material, flame retardation fiber glass reinforced plastics, and the like.

Description

Technical field [0001] The invention relates to an unsaturated polyester resin, in particular to a synthesis method of a reactive transparent halogen-free flame-retardant unsaturated polyester. Background technique [0002] Unsaturated Polyester Resins (UPR) is a thermosetting plastic with the largest output. It is widely used in construction, shipbuilding, automobile industry, chemical equipment, electronic appliances and sporting goods. In 2007, in the context of the slowdown in global economic and trade growth and the world economy entering a period of cyclical adjustment, according to the survey and statistics of 157 UPR companies in my country, the total UPR in the country exceeded 1.3 million tons, reaching 1.35 million tons, compared with 2006 Annual increase of 11%. The annual import of 80,000 tons and the export of 20,000 tons, the actual market consumption exceeded 1.4 million tons (Chen Hong, Hou Yuncheng, Zou Lin, etc., 2006-2007 domestic and foreign unsaturated polye...

Claims

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Application Information

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IPC IPC(8): C08F283/01C08G63/91C08G63/692
Inventor 赵建青张臣刘述梅黄君仪
Owner SOUTH CHINA UNIV OF TECH
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