Synthesis method of polyether ester plasticizer

A polyether ester and plasticizer technology, applied in the field of chemical engineering, can solve problems such as poor toughness, poor processing performance, and poor material durability, and achieve the effect of improving plasticity and high flexibility

Inactive Publication Date: 2015-11-25
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the era of advocating environmental protection, biodegradable materials have attracted attention, especially polylactic acid (PLA), polybutylene succinate (PBS), and poly-β-hydroxybutyric acid (PHB) have good biodegradable materials. And biocompatibility, but most of them have poor toughness, lack of flexibility, and need to be modified by increasing speed. At present, most of the plasticizers used in plasticizing biodegradable materials are small molecule plasticizers such as: butyl citrate Classes, triacetin, etc., although these plasticizers have better speed-up effects, but the plasticizers are easy to precipitate, which eventually leads to poor durability of the material
Most of the currently used polyester plasticizers are relatively low molecular weight, poor processing performance, easy to migrate, threatening human health

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Embodiment 1: a kind of plasticizer synthetic method of polydiethylene glycol adipate-copoly-neopentyl adipate, its synthetic method is as follows:

[0014] (1) Preparation of carboxyl-terminated prepolymer: add 1.2mol (175.39g) adipic acid and 1mol (106.11g) diethylene glycol in a four-necked flask, and heat up to 180° C., stirred and reacted for 4 hours to obtain a carboxyl-terminated prepolymer with an esterification rate of 91.4%.

[0015] (2) Preparation of hydroxyl-terminated prepolymer: add 1mol (146.16g) of adipic acid and 1.2mol (124.99g) of neopentyl glycol in a four-neck medium flask, and under a nitrogen atmosphere, the reaction temperature is 200°C. After 6 hours, a hydroxyl-terminated prepolymer was finally obtained, and the esterification rate was 90.2%.

[0016] (3) The above two prepolymers carry out esterification reaction according to the mass ratio of 1: 1, carry out esterification and polycondensation reaction under the conditions that the temperat...

Embodiment 2

[0018] Embodiment 2: a kind of plasticizer synthetic method of polydipropylene glycol adipate-copoly-neopentyl adipate, its synthetic method is as follows:

[0019] (1) Preparation of hydroxyl-terminated prepolymer: add 1.2mol (175.39g) adipic acid and 1mol (134.17g) dipropylene glycol in a four-necked flask, and heat up to 180° C., stirred and reacted for 4 hours to obtain a carboxyl-terminated prepolymer with an esterification rate of 89.0%.

[0020] (2) Preparation of hydroxyl-terminated prepolymer: Add 1mol (146.16g) of adipic acid and 1.2mol (124.99g) of neopentyl glycol to a four-necked flask. After 6 hours, a hydroxyl-terminated prepolymer was finally obtained with an esterification rate of 87.1%.

[0021] (3) The above two kinds of prepolymers carry out esterification reaction according to the mass ratio of 1:1, carry out esterification and polycondensation reaction under the conditions that the temperature is 190°C, the vacuum degree is 0.01MPa, and the catalyst is 0...

Embodiment 3

[0023] Embodiment 3: a kind of synthetic method of the plasticizer of polyadipate di-alcohol-copoly-adipate in glycol ester, the steps are as follows:

[0024] (1) Preparation of carboxyl-terminated prepolymer: add 1.2mol (175.39g) of adipic acid and 1mol (134.17g) of diethylene glycol in a four-necked flask, and heat up in an oil bath under a nitrogen atmosphere to 180° C., stirred and reacted for 4 hours to obtain a carboxyl-terminated prepolymer with an esterification rate of 90.2%.

[0025] (2) Preparation of carboxyl-terminated prepolymer: add 1 mol (146.16 g) of adipic acid and 1.2 mol (124.99 g) of butanediol in a four-necked flask, and in a nitrogen atmosphere, the reaction temperature is 200 ° C. Reaction 6 Hours, a carboxyl-terminated prepolymer was finally obtained with an esterification rate of 87.8%.

[0026] (3) The above two kinds of prepolymers carry out esterification reaction according to the mass ratio of 1:1, carry out esterification and polycondensation r...

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Abstract

The present invention discloses a method for preparation of a novel polyether ester green plasticizer from adipic acid, C4-C6 dihydric alcohols, and ether-bond-containing C4-C6 dihydric alcohols as main raw materials by addition of a catalyst for three-step esterification, neutralization, water washing, bleaching, reduced pressure distillation, and purification, wherein the catalyst is n-tetrabutyl titanate, stannous octoate and stannous chloride. The designed preparation process is simple and efficient, and rich in source of raw materials. The designed novel polyether ester exhibits better durability, and anti-migration property, and large-scale industrial production can be performed.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to the synthesis, preparation and application of a novel polyether ester plasticizer. Background technique [0002] Plasticizers are widely used in the plastic industry as an auxiliary agent, and the demand is increasing year by year. However, some plasticizers such as dioctyl phthalate (DOP) have been found to be carcinogenic to the human body in recent years. the scope of its use. Therefore, it is imperative to develop green plasticizers. In the era of advocating environmental protection, biodegradable materials have attracted attention, especially polylactic acid (PLA), polybutylene succinate (PBS), and poly-β-hydroxybutyric acid (PHB) have good biodegradable materials. And biocompatibility, but most of them have poor toughness, lack of flexibility, and need to be modified by increasing speed. At present, most of the plasticizers used in plasticizing biodegradable ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/78C08L67/02
Inventor 万同林燕燕
Owner TIANJIN UNIV OF SCI & TECH
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