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以负载型磷钨酸为多相催化剂，通过D，L-乳酸缩聚制备聚乳酸共混物。

Preparation of PLA blends by polycondensation of D,L-lactic acid using supported 12-tungstophosphoric acid as a heterogeneous catalyst.

作者信息

Chafran Liana S, Paiva Mateus F, Freitas Juliene O C, Sales Maria José A, Dias Sílvia C L, Dias José A

机构信息

Universidade de Brasília, Campus Darcy Ribeiro - Asa Norte, Instituto de Química, Laboratório de Catálise (A1-62/21), Brasília-DF, 70910-900, Brazil.

出版信息

Heliyon. 2019 May 28;5(5):e01810. doi: 10.1016/j.heliyon.2019.e01810. eCollection 2019 May.

DOI:10.1016/j.heliyon.2019.e01810
PMID:31193779
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6539807/
Abstract

Poly(lactic acid) (PLA) is a significant polymer that is based on renewable biomass resources. The production of PLA by polycondensation using heterogeneous catalysis is a focus for sustainable and economical processes. A series of samples comprising 12-tungstophosphoric acid (HPW) supported on activated carbon, silica, and alumina induced the catalytic polymerization of D,L-lactic acid to form blends of PLA. The catalysts were characterized by multiple techniques to confirm the integrity of the Keggin anion as well as the acidity, which is the key property for relating structure to activity. The best reaction conditions were established for HPW/C and tested for the other supported catalysts. The obtained polymer was a blend that was characterized as an enantiomeric excess (ee) of as much as 95% L-PLA (PLLA) with a mass average molar mass ( ) of approximately 14,900 daltons. The role of HPW in these polymerizations was demonstrated, i.e., without the Keggin acid, only oligomeric units ( < 10,000 daltons) could be obtained. Additionally, inverse relationships between the of PLA and the enthalpy (-Δ) of the strongest sites of the catalysts were distinguished, i.e., PLA > PLA > PLA, whereas the acidity (-Δ) order was as follows: HPW/SiO > HPW/AlO > HPW/C. These findings could be attributed to the correct tuning of strength and the accessibility of the sites to produce longer polymeric chains.

摘要

聚乳酸（PLA）是一种重要的基于可再生生物质资源的聚合物。使用非均相催化通过缩聚反应生产PLA是可持续和经济过程的一个重点。一系列由负载在活性炭、二氧化硅和氧化铝上的12 - 钨磷酸（HPW）组成的样品引发了D，L - 乳酸的催化聚合反应，形成了PLA共混物。通过多种技术对催化剂进行了表征，以确认Keggin阴离子的完整性以及酸度，酸度是将结构与活性相关联的关键性质。确定了HPW/C的最佳反应条件，并对其他负载型催化剂进行了测试。所得到的聚合物是一种共混物，其特征为L - PLA（PLLA）的对映体过量（ee）高达95%，质均摩尔质量（ ）约为14,900道尔顿。证明了HPW在这些聚合反应中的作用，即没有Keggin酸时，只能得到低聚单元（ < 10,000道尔顿）。此外，区分了PLA的 与催化剂最强位点的焓（-Δ）之间的反比关系，即PLA > PLA > PLA，而酸度（-Δ）顺序如下：HPW/SiO > HPW/AlO > HPW/C。这些发现可归因于对强度的正确调节以及位点的可及性，从而产生更长的聚合物链。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/34e31a23361e/gr13.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/da9da3f53c8e/gr6.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/b6fa4a35278b/gr10.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/af93f4696d07/gr11.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/830f26b3fb9e/gr12.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/34e31a23361e/gr13.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/8e5494e1732c/gr1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/73aab2f87def/gr2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/4bcd0de3a0f2/gr3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/b04a0c238ee3/gr4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/a93fcda8a966/gr5.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/da9da3f53c8e/gr6.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/6d0fdfbd0e38/gr7.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/2a6dc9def732/gr8.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/6591cd014aa9/gr9.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/b6fa4a35278b/gr10.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/af93f4696d07/gr11.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/830f26b3fb9e/gr12.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7748/6539807/34e31a23361e/gr13.jpg

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本文引用的文献

[1]
From lactic acid to poly(lactic acid) (PLA): characterization and analysis of PLA and its precursors.

Biomacromolecules. 2011-2-18

[2]
Chiral salan aluminium ethyl complexes and their application in lactide polymerization.

Chemistry. 2009-9-28

[3]
An overview of polylactides as packaging materials.

Macromol Biosci. 2004-9-16

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