In Situ Polymerization of Polylactic Acid/Quaternary Fulvic Acid Intercalated Saponite Nanocomposites and Structure Characterizazion

Wen-tao Wang; Wei-jun Zhen; Sheng-zhen Bian; Xi Xi

doi:10.11777/j.issn1000-3304.2015.14422

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In Situ Polymerization of Polylactic Acid/Quaternary Fulvic Acid Intercalated Saponite Nanocomposites and Structure Characterizazion

Research Article | 更新时间：2021-03-19

- In Situ Polymerization of Polylactic Acid/Quaternary Fulvic Acid Intercalated Saponite Nanocomposites and Structure Characterizazion
- Acta Polymerica Sinica Issue 7, Pages: 769-777(2015)
- 作者机构：
  
  1. 石油天然气精细化工教育部(自治区)重点实验室新疆大学化学化工学院,乌鲁木齐,830046
  2. 新疆轻工职业技术学院,乌鲁木齐,830021
- 作者简介：
- 基金信息：
- DOI：10.11777/j.issn1000-3304.2015.14422
  CLC：
- Published：20 July 2015，
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Wen-tao Wang, Wei-jun Zhen, Sheng-zhen Bian, Xi Xi. In Situ Polymerization of Polylactic Acid/Quaternary Fulvic Acid Intercalated Saponite Nanocomposites and Structure Characterizazion. [J]. Acta Polymerica Sinica (7):769-777(2015)
DOI：

Wen-tao Wang, Wei-jun Zhen, Sheng-zhen Bian, Xi Xi. In Situ Polymerization of Polylactic Acid/Quaternary Fulvic Acid Intercalated Saponite Nanocomposites and Structure Characterizazion. [J]. Acta Polymerica Sinica (7):769-777(2015) DOI： 10.11777/j.issn1000-3304.2015.14422.

摘要

以新疆地产风化煤(weathered coal)为原料通过硝酸氧解工艺制备黄腐植酸(fulvic acid

FA)

并对黄腐植酸进行季铵化改性

合成黄腐植酸季铵盐(quaternary fulvic acid

QFA).以皂石为原料通过超声波辐照法制备黄腐植酸季铵盐插层皂石(QFA-saponite).以丙交酯和QFA-saponite为原料

在辛酸亚锡催化作用下

制备了聚乳酸/黄腐植酸季铵盐插层皂石(PLA/QFA-saponite)纳米复合材料.通过正交实验探讨了聚合时间、聚合温度、催化剂和QFA-saponite加量对PLA分子量的影响

其最优反应条件为反应12 h、辛酸亚锡加量3%、温度150 ℃、QFA-saponite加量为2%

该正交优化条件下合成的PLA/QFA-saponite纳米复合材料的重均分子量可达95300.红外光谱分析表明黄腐植酸中引入了季铵根离子.X-射线衍射(XRD)对QFA-saponite的分析表明

QFA-saponite呈现部分剥离与插层共存的状态

其层间距达到1.57 nm

比皂石层间距增大0.17 nm.用XRD、示差扫描量热仪(DSC)、偏光显微镜(POM)、热重分析(TGA)等方法对复合材料进行结构表征.结果表明

PLA/QFA-saponite纳米复合材料具有剥离型结构

QFA-saponite有效改善复合材料的结晶性能和热稳定性.抗菌实验表明

黄腐植酸季铵盐插层皂石对大肠杆菌(Escherichia coli)

枯草杆菌(Bacillus subtilis)

黑曲霉菌(Aspergillus) 及青霉(Penicillium)有较强的抑菌效果

同时聚乳酸/黄腐植酸季铵盐插层皂石纳米复合材料也有良好的抗菌性能.

Abstract

The fulvic acid (FA) was prepared with Xinjiang local weathered coal by HNO3 oxidation technology

and then quaternary fulvic acid (QFA) was synthesized with FA.The QFA intercalated saponite (QFA-saponite) was prepared with saponite by ultrasonic intercalation.Poly(lactic acid) (PLA)/QFA-saponite nanocomposites were in situ polymerized with D

L-lactide and QFA-saponite and with stannous octoate as the catalyst.The effects of polymerization time

polymerization temperature

the addition amount of catalyst and QFA-saponite on the molecular weight of PLA were investigated by orthogonal experiment

respectively.The optimum conditions were as follows:polymerization time was 12 h

the addition amount of stannous octoate was 3 wt%

polymerization temperature was 150 ℃ and the addition amount of QFA-saponite was 2 wt%

respectively.Under the optimum conditions

the molecular weight of PLA/QFA-saponite nanocomposites was 95300.FTIR analysis showed that the quaternary ammonium ions were introduced into fulvic acid.The structure of QFA-saponite was characterized by X-ray diffraction (XRD).It was shown that QFA-saponite had co-existence structure with intercalation and partial exfoliation

and its basal spacing was 1.57 nm

which was increased by 0.17 nm compared with that of saponite.The structure of PLA/QFA-saponite nanocomposites was investigated by XRD

polarized optical microscopy (POM) and thermal gravimetric analysis (TGA)

respectively.The results showed that exfoliated PLA based nanocomposites were obtained by in situ polymerization

and QFA-saponite significantly improved the crystallinity properties and thermal stability of PLA.Antibacterial experiments showed that QFA-saponite had antibacterial and sterilization properties against Escherichia coli

Bacillus subtilis

Aspergillus and Penicillium.Meanwhile

PLA/QFA-saponite nanocomposites also had good antibacterial properties.

关键词

聚乳酸黄腐植酸季铵盐插层皂石原位聚合纳米复合材料

Keywords

PLAQFA-saponiteIn situ polymerizationNanocomposites

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Related Institution

Department of Chemical Engineering, Tsinghua University

The Key Laboratory of Synthetic and Biological Colloids, Ministry of Education, School of Chemical and Material Engineering, Jiangnan University

State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Materials Science and Engineering, Donghua University

State Key Laboratory of Power System, Department of Electrical Engineering, Tsinghua University

College of Materials and Metallurgy, Guizhou University

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