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Method for producing modified unsaturated polyester resins by low purity technical grade dicyclopentadiene

A technology of dicyclopentadiene and polyester resin, which is applied in the fields of fine chemicals and polymer materials, can solve the problems of dark resin color, unsuitable high-grade resin, poor storage stability, etc., and achieve the effect of low resin cost

Active Publication Date: 2008-04-02
泉州永悦新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The temperature of hydrolysis and addition is 130-150°C, and the temperature of polycondensation is 210-220°C. The resulting resin has the problems of dark color and poor storage stability, so it is not suitable for high-grade resin (USP6515071)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 0.2mol maleic anhydride and 0.2mol industrial grade dicyclopentadiene to a 250mL four-neck flask equipped with nitrogen protection, stirrer, thermometer, and condensation fractionation device, heat to 100°C to melt, drop 0.2mol after 35min mol distilled water, hydrolyze maleic acid at 100°C under temperature control, keep warm at this temperature for 40 minutes, then add 0.22mol ethylene glycol dropwise, add catalyst dibutyltin dilaurate 0.1mL, and control temperature at 150°C for polycondensation dehydration React for 8 hours, remove excess water and small molecules under reduced pressure in the later stage, and end the reaction until the acid value of the reactant is less than 40mgKOH / g. Cool the reactant to 90°C, add 0.02g of hydroquinone, and stir fully at 120 Adding 30% styrene of the total amount of the resin below ℃ to dilute, then cooling down and discharging to obtain a modified unsaturated polyester resin prepared from low-purity industrial grade dicyclopen...

Embodiment 2

[0018] Add 0.25mol maleic anhydride, 0.1mol phthalic anhydride, and 0.2mol industrial grade dicyclopentadiene to a 250mL four-necked flask equipped with nitrogen protection, stirrer, thermometer, and condensation fractionation device, and heat to Melt at 90°C, add 0.25mol of distilled water dropwise after 30min, hydrolyze maleic anhydride at 120°C under temperature control, keep warm at this temperature for 50min, then add 0.35mol of propylene glycol dropwise, add catalyst methanesulfonic acid 0.3mL after dropwise, control temperature Polycondensation and dehydration reaction at 155°C for 9 hours, remove excess water and small molecules under reduced pressure in the later stage, and end the reaction until the acid value of the reactant is less than 40mgKOH / g, cool the reactant to 100°C, and add 0.05g tert-butyl p-phenylene After fully stirring the diphenol, add 35% styrene of the total amount of the resin below 110°C to dilute, then cool down and discharge to obtain a modified ...

Embodiment 3

[0020] In the 250mL four-neck flask with nitrogen protection, stirrer, thermometer, condensation fractionation device, add 0.22mol maleic anhydride, 0.1mol phthalic anhydride, 0.22mol industrial grade dicyclopentadiene, heat to Melt at 100°C, add 0.22mol of distilled water dropwise after 30min, hydrolyze maleic anhydride at 130°C under temperature control, keep warm at this temperature for 40min, then add 0.33mol of propylene glycol dropwise, add catalyst p-toluenesulfonic acid 0.3g after dropwise, control The temperature is between 150°C for polycondensation and dehydration reaction for 8 hours, and the excess water and small molecules are removed under reduced pressure in the later stage, and the reaction is terminated after the acid value of the reactant is less than 40mgKOH / g. After fully stirring the diphenol, add 30% styrene of the total amount of the resin below 120°C to dilute, then cool down and discharge the material to obtain a modified unsaturated polyester resin pr...

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PUM

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Abstract

The present invention relates to a novel method of using industrial dicyclopentadiene of purity of 75 percent to 85 percent to prepare modified unsaturated polyester resin. In the preparation of the resin, the industrial dicyclopentadiene separated from the saturated or unsaturated dicarbonic acid or acidic anhydride and the distilled part of mixed C5 is used as the raw material. After hydrolysis and addition reaction, the diol or polyol of appropriate amount is added. The polymerization and dehydration reaction is done with the influence of acidic catalyst. When the mixture is condensed to the designated acid value, the inhibitor and cross-linking monomer of appropriate amount are added and then stirred to prepare the product. The present invention has the advantage that the cost of resin is lower than the common type unsaturated resin. At the same time, the air-drying performance, heat resistance, volumetric shrinkage rate and other performances are all superior to the common type unsaturated polyester resin. The product can be widely used in the fields of glass steel, mold, plastic clothing, sealing, and adhesive and so on.

Description

technical field [0001] The invention belongs to the field of fine chemical industry and macromolecular materials, and relates to a method for preparing modified unsaturated polyester resin from low-purity industrial-grade dicyclopentadiene. Background technique [0002] Unsaturated polyester resin refers to the thermosetting resin formed by polycondensation of saturated diol, saturated acid and unsaturated dibasic acid (or anhydride). Due to its good mechanical properties, electrical properties and chemical corrosion resistance, raw materials Easy to obtain, simple processing technology and other advantages, it has been widely used in many fields such as glass fiber reinforced materials, chemical anticorrosion, casting products, sanitary furniture, handicraft manufacturing, etc. It has become an important thermosetting resin material and has won worldwide recognition. Wide range of applications, annual consumption of millions of tons, and the consumption is increasing every ...

Claims

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Application Information

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IPC IPC(8): C08G63/52
Inventor 张龙韩晓辉
Owner 泉州永悦新材料有限公司
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