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Preparation method of glyceryl polyester used as PVC (Polyvinyl Chloride) plasticizer

A technology of plasticizer and dibasic acid glyceride, which is applied in the field of chemical synthesis, can solve the problems of poor compatibility, single performance, and small molecular weight of plasticizers, and achieve the effects of low price, simple synthesis process, and low energy consumption

Inactive Publication Date: 2013-08-14
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method of glycerol-based polyester used as a PVC plasticizer, which overcomes the shortcomings of traditional plasticizers such as small molecular weight, single performance, and poor compatibility with PVC, and provides a high thermal stability Glyceryl polyester plasticizer with strong resistance, extraction resistance and good migration resistance and preparation method thereof

Method used

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  • Preparation method of glyceryl polyester used as PVC (Polyvinyl Chloride) plasticizer
  • Preparation method of glyceryl polyester used as PVC (Polyvinyl Chloride) plasticizer
  • Preparation method of glyceryl polyester used as PVC (Polyvinyl Chloride) plasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 0.25mol (92×0.25=23g) glycerin, 0.35mol (154.16×0.35=54g) hexahydrophthalic anhydride, 0.20mol (130.23×0.20=26.05g) 2-ethylhexanol, 10mL cyclohexane, 0.90g antimony trioxide, nitrogen protection, start stirring, slowly raise the temperature, 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 Calculate with reference to GB / T1668-2008, react until the acid value no longer decreases, stop heating, cool to room temperature under nitrogen, replace the vacuum distillation device, distill the excess alcohol, water-carrying agent and small molecule products, and wait until there is no liquid Stop heating when dropping, and cool to room temperature under reduced pressure to obtain polyhexahydrophthalic anhydride glyceride. The final acid value of product 1 is 1.78 mg KOH g -1 , the esterification rate is 98.71%, and the color of the product is clear and light yellow. It is confirmed to be polyh...

Embodiment 2

[0026] Add 0.25mol glycerin, 0.30mol (154.16×0.30=46.25g) hexahydrophthalic anhydride, 0.2mol (26.05g) 2-ethylhexanol, 10mL cyclohexane, 0.95g tetrahydrotitanate to a 250mL four-necked flask. Butyl ester, nitrogen protection, start stirring, slowly raise the temperature, keep the heating rate at 20°C / h, and the maximum temperature does not exceed 220°C, measure the acid value every 1h, and stop heating until the acid value no longer decreases. Cool to room temperature under nitrogen, replace the vacuum distillation device, distill off excess alcohol, water-carrying agent and small molecule products, stop heating when no liquid drops, and cool to room temperature under reduced pressure to obtain polyhexahydrophthalic anhydride Glycerides. The final acid value of product 2 is 1.56 mg KOH g -1 , the esterification rate is 99.21%, and the color of the product is clear and light yellow. It is confirmed to be polyhexahydrophthalic anhydride glyceride after infrared test and charact...

Embodiment 3

[0029] Add 0.25mol glycerol, 0.35mol (54g) hexahydrophthalic anhydride, 0.2mol (26.05g) 2-ethylhexanol, 10mL cyclohexane, and 1.10g tetra-n-butyl titanate to a 250mL four-neck flask, and Under nitrogen protection, start stirring, slowly raise the temperature, keep the heating rate at 20°C / h, and the maximum temperature does not exceed 220°C, measure the acid value every 1h, stop heating until the acid value no longer decreases, and cool under nitrogen To room temperature, replace the vacuum distillation device, distill off excess alcohol, water-carrying agent and small molecule products, stop heating when no liquid drops, and cool to room temperature under reduced pressure to obtain polyhexahydrophthalic anhydride glyceride. The final acid value of product 3 is 1.77 mg KOH g -1 , the esterification rate is 99.51%, the color of the product is clear and light yellow, and the viscosity is moderate. It is confirmed to be polyhexahydrophthalic anhydride glyceride by infrared test. ...

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Abstract

The invention discloses a preparation method of glyceryl polyester used as a PVC (Polyvinyl Chloride) plasticizer and belongs to the technical field of chemical synthesis. The preparation method comprises the following steps of: synthesizing by a one-step process under the combined action of a catalyst, an end-capping reagent and a water-carrying agent by using cheap bio-based glycerol, non-orthophthalic binary acid (for example hexahydrophthalic anhydride, adipic acid or the like) as the materials; and carrying out the post-treatment processes including dehydration poly-condensation, reduced pressure distillation and the like to obtain the poly-binary acid glyceride plasticizer. The glyceride plasticizer has a final acid value of 0.7mgKOH.g<-1>-2mgKOH.g<-1>, an esterification rate higher than 97%, relative molecular weight of about 5000, a dispersion coefficient of 1.00-1.13, appropriate viscosity and stable physical and chemical characteristics; the glyceride plasticizer is added to the PVC according to a certain formula to be refined into a PVC plastic test block, so that application performances including heat stability, drawing resistance, tensile performance and the like of the test block are tested; and the test block has good heat stability, tensile performance and excellent mobility resistance. The preparation method of the glyceryl polyester used as the PVC plasticizer is low in material price, simple in preparation process, low in energy consumption, excellent in product performance and good in application prospect.

Description

technical field [0001] The invention discloses a preparation method of glycerin-based polyester used as a PVC plasticizer, belonging to the technical field of chemical synthesis. Background technique [0002] Plasticizer is a plastic additive that can reduce the glass transition temperature of polymer materials and improve the plasticity of materials in a huge amount. It can be added to a variety of objects, including plastic and rubber products, medical materials, building materials, etc. Agents play different roles in different additive objects. At present, the plasticizers occupying the mainstream market are phthalates, such as dioctyl phthalate (DOP) and dibutyl phthalate (DBP), which are used in large amounts. However, studies have confirmed that such plasticizers have toxic effects on multiple systems of the body after entering the human body, especially harmful to women and children. The U.S. Environmental Protection Agency and the European Parliament have restricte...

Claims

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Application Information

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IPC IPC(8): C08G63/12C08G63/78C08L27/06C08L67/00
Inventor 蒋平平张彩芹苗红艳
Owner JIANGNAN UNIV
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