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Preparation method for epoxy polyester plasticizer

A technology of epoxy polyester and plasticizer, applied in the field of preparation of epoxy polyester plasticizer and epoxy polyester plasticizer, can solve the problem of poor migration resistance, material aging, polyester plasticizer Small molecular weight and other problems, to achieve good plasticizing effect

Active Publication Date: 2011-10-12
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Due to the relatively small molecular weight of these monomeric polyester plasticizers, the compatibility with materials is poor, and they are easily extracted by organic solvents in the use of polymer materials, and have poor migration resistance, which affects to product application performance
For example, during the use of rubber products or plastic materials, the "sweating" phenomenon is caused by the seepage of plasticizers, which leads to rapid aging of the materials; for cables immersed in oil wells for a long time, the plasticizers have poor resistance to extraction It will accelerate the cracking and aging of the cable
And in recent years, due to the potential hazards of phthalate plasticizers, it has been restricted in many application fields. Many countries, including the European Union, have formulated corresponding laws and regulations to restrict phthalate plasticizers. Use in children's toys, food packaging and other fields

Method used

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  • Preparation method for epoxy polyester plasticizer
  • Preparation method for epoxy polyester plasticizer
  • Preparation method for epoxy polyester plasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Esterification reaction: Add 0.20mol (30.72g) tetrahydrophthalic anhydride, 0.22mol diethylene glycol, 0.06mol isooctyl alcohol, 10mL cyclohexane, 0.30g titanic acid into a 250mL four-neck flask Tetra-n-butyl ester, nitrogen gas for 20 minutes, start stirring, slowly heat up, start timing when water comes out, keep the heating rate at 20°C / h, and the maximum temperature does not exceed 220°C, measure the acid value every 1h, the acid value The calculation refers to GB / T 1668-2008, after 5 hours of reaction, the acid value is reduced to 0.38mgKOH / g, and the esterification rate is greater than 99%. Stop heating, cool to room temperature under nitrogen, change to a vacuum distillation device, and slowly raise the temperature to 220 °C, stop heating when no liquid drops, and cool to room temperature under reduced pressure.

[0030] (2) Epoxidation reaction: Add 10g of formic acid with a mass fraction of 88% to the esterification product, stir, and heat in a water bath t...

Embodiment 2

[0032] (1) Esterification reaction: Add 0.20mol tetrahydrophthalic anhydride, 0.24mol diethylene glycol, 0.08mol isooctyl alcohol, 10mL cyclohexane, and 0.20g tetra-n-butyl titanate to a 250mL four-necked flask. , pass nitrogen gas for 20 minutes, start stirring, slowly heat up, start timing when water comes out, keep the heating rate at 20°C / h, and the maximum temperature does not exceed 220°C, measure the acid value every 1h, the calculation of the acid value refers to GB / T 1668-2008, react for 5 hours, the acid value drops to 0.35mgKOH / g, the esterification rate is greater than 99%, stop heating, cool to room temperature under nitrogen, change to a vacuum distillation device, slowly raise the temperature to 220°C, and wait until no Stop heating when the liquid drops, and cool to room temperature under reduced pressure.

[0033] (2) Epoxidation reaction: Add 15g of formic acid with a mass fraction of 88% to the esterification product, stir, and heat in a water bath to 65°C....

Embodiment 3

[0035] (1) Esterification reaction: Add 0.20mol tetrahydrophthalic anhydride, 0.26mol diethylene glycol, 0.1mol isooctyl alcohol, 10mL cyclohexane, and 0.40g tetra-n-butyl titanate to a 250mL four-necked flask. , pass nitrogen gas for 20 minutes, start stirring, slowly heat up, start timing when water comes out, keep the heating rate at 20°C / h, and the maximum temperature does not exceed 220°C, measure the acid value every 1h, the calculation of the acid value refers to GB / T 1668-2008, react for 4 hours, the acid value is reduced to 0.40mgKOH / g, the esterification rate is greater than 99%, stop heating, cool to room temperature under nitrogen, change to a vacuum distillation device, slowly heat up to 220°C, and wait for Stop heating when the liquid drops, and cool to room temperature under reduced pressure.

[0036](2) Epoxidation reaction: Add 20g of formic acid with a mass fraction of 88% to the esterification product, stir, and heat in a water bath to 70°C. After the tempe...

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Abstract

The invention relates to a preparation method for an epoxy polyester plasticizer, belonging to the technical field of chemical synthesis. The preparation method comprises the following steps of: firstly carrying out reaction on an unsaturated dicarboxylic anhydride and a saturated dibasic alcohol under catalysis action to generate a polyester with a certain molecular weight, and then carrying out epoxidation reaction on the polyester under the conditions of introducing an oxygen source and using formic acid as a carrier to obtain the epoxy polyester plasticizer with a certain epoxide number. The product provided by the invention has the characteristics of light color and luster, low residual iodine value and high heat stability and are basically nontoxic; and the reaction process is short, is easy to operate, is low in energy consumption and cost, and meets pollution-free and clean production process.

Description

technical field [0001] A method for preparing an epoxy polyester plasticizer, specifically, relates to an epoxy polyester plasticizer with superior extraction resistance, good migration resistance, good thermal stability, non-toxic and environmental protection, belonging to The field of chemical synthesis technology. Background technique [0002] Plasticizer is one of the most used plastic additives, which plays an extremely important role in improving the application performance of plastic and rubber products. At present, the main types of plasticizers at home and abroad are phthalate plasticizers, such as dibutyl phthalate (DBP), dioctyl phthalate (DOP), bicyclic phthalate Hexyl ester (DCHP), etc., among which di-isooctyl phthalate (DEHP) is the most used. [0003] Due to the relatively small molecular weight of these monomeric polyester plasticizers, the compatibility with materials is poor, and they are easily extracted by organic solvents in the use of polymer materia...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08G63/676C08L27/06C08L67/02
Inventor 蒋平平李成成董玉明周永芳张萍波苗红艳
Owner JIANGNAN UNIV
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