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A kind of fully bio-based unsaturated polyester prepolymer for dynamic vulcanization with polylactic acid and preparation method thereof

A dynamic vulcanization and prepolymer technology, applied in the field of polymer materials, can solve the problems affecting the biodegradability of polylactic acid, the loss of blend strength and modulus, etc., to ensure full bio-based characteristics, low price, The effect of the simple preparation process

Active Publication Date: 2022-04-26
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of fully bio-based unsaturated polyester prepolymer for dynamic vulcanization with polylactic acid and its preparation method, after overcoming the non-bio-based added phase in the prior art and blending with polylactic acid, Problems that affect the biodegradability of polylactic acid itself and the large loss of strength and modulus of the blend

Method used

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  • A kind of fully bio-based unsaturated polyester prepolymer for dynamic vulcanization with polylactic acid and preparation method thereof
  • A kind of fully bio-based unsaturated polyester prepolymer for dynamic vulcanization with polylactic acid and preparation method thereof
  • A kind of fully bio-based unsaturated polyester prepolymer for dynamic vulcanization with polylactic acid and preparation method thereof

Examples

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preparation example Construction

[0041] The present invention provides a kind of preparation method of the all bio-based unsaturated polyester prepolymer that is used for dynamic vulcanization with polylactic acid, comprises the following steps:

[0042] Step 1. Weigh the polybasic acid and diol in the container according to the proportion, add a certain amount of polymerization inhibitor, pass through the protective gas, heat and stir for a period of time to undergo preliminary esterification, and obtain a preliminary esterification product.

[0043] In a specific embodiment of the present invention, the polybasic acid in step 1 is formed by mixing citric acid and itaconic acid;

[0044] Preferably, citric acid accounts for 60-90% (such as 60%, 65%, 70%, 75%, 80%, 85%, 90%) of the molar weight of polybasic acid; itaconic acid accounts for 10-90% of the molar weight of polybasic acid. 40% (such as 10%, 15%, 20%, 25%, 30%, 35%, 40%).

[0045] In a specific embodiment of the present invention, the dihydric alc...

Embodiment 1

[0063] In the embodiment of the present invention, a method for preparing a fully bio-based unsaturated polyester prepolymer for dynamic vulcanization with polylactic acid comprises the following steps:

[0064] Step 1. Weigh 17.9716g of polybasic acid and 8.6754g of 1,3-propanediol in a container, add 0.1332g of p-hydroxyanisole, pass nitrogen gas to fill the container, heat to 165°C and stir for 20min, then cool down To 145 ° C, stirring and melting for 20 minutes to undergo preliminary esterification, and obtain a preliminary esterification product; (wherein, the polybasic acid is a mixture of citric acid and itaconic acid, and the molar ratio of citric acid and itaconic acid is 0.08mol: 0.02mol; The molar ratio of carboxyl and hydroxyl groups in acid and 1,3-propanediol is 1:1.1; the amount of p-hydroxyanisole added is 0.5wt% of the total mass of polybasic acid and 1,3-propanediol);

[0065] Step 2. The preliminary esterification product obtained in step 1 is maintained at...

Embodiment 2

[0080] The preparation method of the fully bio-based unsaturated polyester prepolymer used for dynamic vulcanization with polylactic acid in this example is different from the preparation method in Example 1 in that:

[0081] In step 1, take by weighing 22.3078g of 1,10-decanediol, and add 0.2014g of p-hydroxyanisole (wherein, the molar ratio of polyacid and 1,10-decanediol in carboxyl to hydroxyl is 1: 1.2); step 3, washing 7 times; other methods and steps are the same as those in Example 1, and will not be repeated here.

[0082] The fully bio-based unsaturated polyester prepolymer and polylactic acid prepared in this example were dynamically vulcanized, and the specific steps were the same as those in Example 1, which will not be repeated here.

[0083] The mechanical property test method of the polylactic acid / fully bio-based unsaturated polyester prepolymer blend prepared in this example is the same as that of Example 1, and will not be repeated here.

[0084] By testing...

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Abstract

The invention provides a fully bio-based unsaturated polyester prepolymer for dynamic vulcanization with polylactic acid and a preparation method thereof. Then, the preliminary esterification product is subjected to polycondensation reaction under vacuum conditions to obtain a first prepolymer; the first prepolymer is freeze-dried to prepare a fully bio-based unsaturated polyester prepolymer. The invention adopts polybasic acid and diol as biomass raw materials, and the price is low; a one-pot method is adopted to prepare a fully bio-based unsaturated polyester prepolymer, the process is simple, easy to operate, and the prepolymer is successfully purified in the purification process The double bond is preserved, and the active functional group is reserved for the subsequent dynamic vulcanization. After dynamic vulcanization with polylactic acid, it can not only significantly improve the physical and mechanical properties of polylactic acid such as toughness, but also ensure the prepared biodegradable polylactic acid. Fully bio-based properties of blend materials.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a fully bio-based unsaturated polyester prepolymer used for dynamic vulcanization with polylactic acid and a preparation method thereof. Background technique [0002] As a biocompatible and biodegradable plastic, polylactic acid has become the best choice to replace traditional petroleum-based non-degradable plastics due to its excellent mechanical properties. However, the toughness of polylactic acid is poor, which limits its application in fields requiring high toughness, such as textiles, automobiles, medical treatment, food and other industries. Blending polylactic acid with flexible polymers to improve the toughness of polylactic acid is the most cost-effective and industrialized method. [0003] Dynamic vulcanization is one of the most widely used methods of polymer blending modification. This method refers to the melt blending of elastomers (or monom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/60C08G63/52C08L67/04C08L67/06C08K5/14
CPCC08G63/60C08G63/52C08L67/04C08L2205/02C08L2201/06C08L67/06C08K5/14
Inventor 陈金周刘文涛陈鸿燕刘旭影杨会歌段瑞侠牛明军
Owner ZHENGZHOU UNIV
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