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Pyrrolidone-terminated polylactic acid and preparation method thereof, and polylactic acid composite material and preparation method thereof

A technology of pyrrolidone and composite materials, which is applied in the field of degradable plastics, can solve the problems of PDLA safety, insignificant toughening improvement, and low heat distortion temperature, and achieve shortened nucleation time, reduced exercise difficulty, and excellent toughness. Effect

Active Publication Date: 2021-11-23
WANHUA CHEMICAL (NINGBO) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN109265941A discloses a translucent heat-resistant polylactic acid, adding cyclic phosphoric anhydride, 4,4'-difluorobenzophenone (C13H8F2O) as a nucleating agent, with a low heat distortion temperature of about 110 ° C, and does not involve molding time
However, the compatibility between polyvinylpyrrolidone and PLA is not good, it will migrate to the surface, the toughening improvement is not obvious, and it will be lost and consumed during the continuous surface migration process.
CN110903620A discloses a preparation method of string crystallized high heat-resistant polylactic acid composite material, using 20% ​​PBAT to blend 80% polylactic acid, oriented crystallization in repeated shearing, with certain toughness, but the heat distortion temperature is below 110 °C , and the production efficiency is low
CN110922729A discloses a heat-resistant polylactic acid material and its preparation method, adding 20% ​​PDLA and 80% PLLA to form a stereo crystal, which has good heat resistance, and does not mention the molding speed, but the safety of PDLA exists Doubtful and more expensive

Method used

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  • Pyrrolidone-terminated polylactic acid and preparation method thereof, and polylactic acid composite material and preparation method thereof
  • Pyrrolidone-terminated polylactic acid and preparation method thereof, and polylactic acid composite material and preparation method thereof
  • Pyrrolidone-terminated polylactic acid and preparation method thereof, and polylactic acid composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 100 parts of toluene and place it in a four-necked flask as a solvent, then slowly add 88 parts of lactide, 5 parts of L-pyrrolidone carboxylic acid, and 5 parts of glycerin into the four-necked flask, heat to 50°C, and Stir at a speed of 1 / min until the lactide is completely melted, then add 1 part of stannous isooctanoate to keep the temperature at 110°C, and condense and reflux for 6 hours. After the reaction was completed, 1 part of hydroquinone was added, the flask was transferred to a rotary evaporator to evaporate most of the solvent, and the reaction solution was poured out, washed three times with chloroform to obtain a precipitate. The precipitate was vacuum-dried at 70° C. for 3 hours to obtain a white solid which was pyrrolidone-terminated polylactic acid. The weight average molecular weight was 5000.

[0028] Weigh 76.5 parts of polylactic acid with a weight average molecular weight of 120,000, 20 parts of pyrrolidone-terminated polylactic acid, 2 part...

Embodiment 2

[0031] The synthesis steps of pyrrolidone-terminated polylactic acid are the same as in Example 1, except that the reaction time is controlled to 3.5 hours and the weight average molecular weight is 3000.

[0032] Weigh 76.5 parts of polylactic acid with a weight average molecular weight of 120,000, 20 parts of pyrrolidone-terminated polylactic acid, 2 parts of zinc stearate, 1 part of sebacic acid dihydrazide, and 0.5 part of Stabilizer 9000, and pelletize in a twin-screw extruder , the steps are as shown in Example 1.

[0033] The injection molding machine is used for extrusion molding, and the standard sample bar of 0.8mm×13mm×125mm is used for injection molding test performance. The injection speed is set at 200mm / s, and the mold temperature is set at 120°C.

Embodiment 3

[0035] The synthesis steps of pyrrolidone-terminated polylactic acid are the same as in Example 1, the difference is that the reaction time is controlled to 4 hours, and the weight average molecular weight is 4000.

[0036] Weigh 88 parts of polylactic acid with a weight average molecular weight of 120,000, 10 parts of pyrrolidone-terminated polylactic acid, 0.5 part of zinc stearate, 0.5 part of sebacic acid dihydrazide, and 1 part of Stabilizer 9000, and pelletize in a twin-screw extruder , the steps are as shown in Example 1.

[0037] The injection molding machine is used for extrusion molding, and the standard sample bar of 0.8mm×13mm×125mm is used for injection molding test performance. The injection speed is set at 200mm / s, and the mold temperature is set at 120°C.

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Abstract

The invention discloses pyrrolidone-terminated polylactic acid and a preparation method thereof, and a polylactic acid composite material and a preparation method thereof. The structural formula of the pyrrolidone-terminated polylactic acid is shown as follows: the weight-average molecular weight of the pyrrolidone-terminated polylactic acid is 1000-5000. The polylactic acid composite material comprises polylactic acid, pyrrolidone-terminated polylactic acid, a nucleating agent, a plasticizer and an end-capping reagent. According to the present invention, in the injection molding process, the molding time can be reduced to less than 20 s, the thermal deformation temperature of 120 DEG C or more is provided, the toughness is substantially improved, the defects in the prior art are solved, the rapid molding of the polylactic acid product is achieved, the defects of slow molding time, long demolding time, crisp product and the like of the existing heat-resistant polylactic acid are improved, and the production efficiency is improved; the potential market value is realized.

Description

technical field [0001] The invention belongs to the field of degradable plastics, and in particular relates to a pyrrolidone-terminated polylactic acid and a rapidly prototyping heat-resistant polylactic acid composite material. Background technique [0002] Petroleum-based materials, as one of the most important sources of pollution in the world, are increasingly damaging the environment, which makes the environment require plastic products to be degradable. Therefore, in recent years, biodegradable plastics have achieved rapid development and expansion. With the continuous development of social economy and the continuous promotion of policies, degradable plastic products are gradually replacing traditional polyolefin products, facing a huge vacancy in production capacity. As a commercialized degradable plastic, polylactic acid has excellent biocompatibility and degradability, and can replace traditional olefin plastic products in many fields. However, PLA has its inheren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/685C08G63/91C08L67/04C08L67/00C08K5/098C08K5/25B29C48/04B29C48/92B29C45/78
CPCC08G63/685C08G63/91C08L67/04B29C48/04B29C48/92B29C45/78C08L2205/24C08L2201/08B29C2948/92704B29C2945/76531C08L67/00C08K5/098C08K5/25
Inventor 李熠宇陈连清孙晓燏李保印李芬香黄建詹佐民邵成立蒲霄杨峰王金祥何亚洲
Owner WANHUA CHEMICAL (NINGBO) CO LTD
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