改性水滑石调控聚乳酸-马来酸酐接枝聚丙烯复合材料及其性能

黎晓杰; 成晓琼; 段书谦; 袁婷; 辛佳礼; 付海

doi:10.13801/j.cnki.fhclxb.20211217.002

改性水滑石调控聚乳酸-马来酸酐接枝聚丙烯复合材料及其性能

doi: 10.13801/j.cnki.fhclxb.20211217.002

黎晓杰^1,,
成晓琼¹,
段书谦¹,
袁婷¹,
辛佳礼¹,
付海^{1, 2, ,}

1.
贵州师范大学　材料与建筑工程学院，贵阳 550025
2.
国家复合改性聚合物工程技术研究中心，贵阳 550014

基金项目: 国家自然科学基金地区项目(21764004)；贵州省科学计划项目黔科合平台人才[2017]5726；黔科合基础[2016]1100

详细信息

通讯作者:
付海，博士，副教授，研究方向为功能复合材料　E-mail:599726614@qq.com

中图分类号: TB332
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出版历程
- 收稿日期: 2021-10-14
- 修回日期: 2021-12-02
- 录用日期: 2021-12-03
- 网络出版日期: 2021-12-20
- 刊出日期: 2022-12-01

Properties of polylactic acid/maleic anhydride grafted polypropylene composites regulated by modified hydrotalcite

1.
School of Materials & Architectural Engineering, Guizhou Normal University, Guiyang 550025, China
2.
National Research Center of Composite Modified Polymer Engineering Technology, Guiyang 550014, China

摘要

摘要: 为了研究水滑石复合材料的力学性能、热稳定性、动态热机械性能、结晶行为和界面相容性等，通过共沉淀法制备镁铝水滑石，再将水滑石进行焙烧，得到焙烧镁铝水滑石，以控制变量法考察温度和时间对水滑石层间结构的影响，利用TG、SEM、XRD分别表征测试了300℃下焙烧后的水滑石(LDHs(300))的形貌和热稳定性，证实其层间水已经大部分除去，且保持层状结构而不损害其原有的性能。利用FTIR、XRD表征测试了十二烷基苯磺酸钠(SDBS)能成功插层改性焙烧后的水滑石。再采用熔融共混法，将不同表面改性的水滑石颗粒添加到聚乳酸-马来酸酐接枝聚丙烯(PLA-PP-g-MAH)得到不同的复合材料。结果表明，焙烧改性后的水滑石复合材料的性能最优。通过SEM进行的形态分析表明，随着水滑石添加到PLA-PP-g-MAH中，PP-g-MAH颗粒相畴尺寸显著减小，PP-g-MAH相具有更好的润湿性，从而产生更高的冲击强度，冲击性能与纯PLA相比提高了37.72%。从流变行为发现，焙烧改性后的水滑石复合材料的流变性能比PLA显著增加。DMA表明，在PLA-PP-g-MAH共混物中添加焙烧改性后的水滑石，PLA的玻璃化转变温度$ \left({T}_{\mathrm{g}}\right) $升高和冷结晶温度$ {(T}_{\mathrm{c}\mathrm{c}}) $降低。从DSC和POM表明，焙烧改性后的水滑石复合材料提高了结晶速率，结晶度比PLA提高了62.8%。
- 焙烧水滑石 /
- 焙烧温度 /
- 聚乳酸 /
- 马来酸酐接枝聚丙烯 /
- 三元复合物
Abstract: In order to study the mechanical properties, thermal stability, dynamic thermomechanical properties, crystallization behavior and interfacial compatibility of hydrotalcite composites, Mg-Al hydrotalcite was prepared by coprecipitation method, and then calcined to obtain calcined Mg-Al hydrotalcite. The effects of temperature and time on the interlayer structure of hydrotalcite were investigated by variable control method. The hydrotalcite calcined at 300℃ (LDHs(300)) was characterized and tested by TG, SEM and XRD. The morphology and thermal stability confirmed that most of the interlayer water had been removed, and the layered structure was maintained without damaging its original properties. The calcined hydrotalcite was successfully intercalated with sodium dodecylbenzene sulfonate (SDBS) by FTIR and XRD. Then different surface modified hydrotalcite particles were added to polylactic acid/maleic anhydride grafted polypropylene (PLA-PP-g-MAH) by melt blending to obtain different composites. The results show that the properties of hydrotalcite composites modified by calcination are the best. The morphological analysis by SEM shows that with the addition of hydrotalcite to PLA-PP-g-MAH, the domain size of PP-g-MAH particles decreases significantly, and the PP-g-MAH phase has better wettability, resulting in higher impact strength, compared with pure PLA, it increased by 37.72%. From the rheological behavior, it is found that the rheological properties of calcined hydrotalcite composites are significantly higher than those of PLA. DMA shows that when calcined hydrotalcite is added to PLA-PP-g-MAH blend, the glass transition temperature (T_g) of PLA increased and the cold crystallization temperature (T_cc) decreased. DSC and POM show that the crystallization rate and crystallinity of calcined hydrotalcite composites are higher than those of PLA by 62.8%.
- calcined hydrotalcite /
- calcination temperature /
- polylactic acid /
- maleic anhydride grafted polypropylene /
- ternary complex

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图 1 不同温度下焙烧水滑石24 h的热重曲线

Figure 1. Thermogravimetric diagram of hydrotalcite calcined at different temperatures for 24 h

DTG—Differential thermogravimetric

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图 2 (a) 300℃焙烧4 h和24 h的水滑石热重曲线； (b) 300℃焙烧24 h和300℃焙烧24 h后放置两周的水滑石热重曲线

Figure 2. (a) Thermogravimetric curves of hydrotalcite calcined at 300℃ for 4 h and 24 h; (b) Thermogravimetric curves of hydrotalcite calcined at 300℃ for 24 h and placed for 2 weeks

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图 3 未焙烧水滑石和300℃下焙烧水滑石SEM图像：((a)、(c)) 未焙烧Mg-Al水滑石；((b)、(d)) 300℃下焙烧24 h Mg-Al水滑石

Figure 3. SEM images of unburned hydrotalcite and calcined hydrotalcite at 300℃: ((a), (c)) Unburned Mg-Al hydrotalcite; ((b), (d)) Mg-Al hydrotalcite calcined at 300℃ for 24 h

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图 4 未焙烧水滑石和250℃、300℃、350℃及400℃下焙烧水滑石XRD图谱

Figure 4. XRD patterns of unburned hydrotalcite and calcined hydrotalcite at 250℃, 300℃, 350℃ and 400℃

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图 5 LDHs(300)和LDHs(300)-十二烷基苯磺酸钠(SDBS)的FTIR图谱

Figure 5. FTIR spectra of LDHs(300)和LDHs(300)-sodium dodecyl benzene sulfonate (SDBS)

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图 6 LDHs(300)和LDHs(300)-SDBS的XRD图谱，其中扫描范围为2°~70°

Figure 6. XRD patterns of LDHs(300) and LDHs(300)-SDBS scanned from 2° to 70°

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图 7 水滑石复合材料的纯样品及共混物的SEM图像：(a) PLA-PP-g-MAH；(b) LDHs(300)-SDBS/PLA-PP-g-MAH；(c) LDHs(300)/PLA-PP-g-MAH；(d) LDHs-SDBS/PLA-PP-g-MAH；(e) LDHs/PLA-PP-g-MAH；(f) Neat PLA；((a′)~(f′)) 对应的局部放大图

Figure 7. SEM images of the pure samples and blends of hydrotalcite composites: (a) PLA-PP-g-MAH; (b) LDHs(300)-SDBS/PLA-PP-g-MAH; (c) LDHs(300)/PLA-PP-g-MAH; (d) LDHs-SDBS/PLA-PP-g-MAH; (e) LDHs/PLA-PP-g-MAH; (f) Neat PLA; ((a′)~(f′)) Corresponding local enlarged view

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图 8 水滑石复合材料的纯样及共混物的热重图

Figure 8. Thermogravimetry of the pure samples and blends of hydrotalcite composites

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图 9 不同频率下PLA-PP-g-MAH、LDHs(300)-SDBS/PLA-PP-g-MAH、LDHs(300)/PLA-PP-g-MAH、LDHs-SDBS/PLA-PP-g-MAH、LDHs/PLA-PP-g-MAH和纯PLA的储能模量G′(a)、损耗模量G′′ (b) 和复数黏度η* (c)

Figure 9. Storage modulus G′ (a), loss modulus G′′ (b) and complex viscosity η* (c) of PLA-PP-g-MAH, LDHs(300)-SDBS/PLA-PP-g-MAH, LDHs(300)/PLA-PP-g-MAH, LDHs-SDBS/PLA-PP-g-MAH, LDHs/PLA-PP-g-MAH and neat PLA at different frequencies

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图 10 水滑石复合材料的纯样及共混物的储能模量 (a)、损耗模量 (b) 和损耗因子tanδ (c)

Figure 10. Storage modulus (a), loss modulus (b) and loss factor (c) of pure samples and blends of hydrotalcite composites

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图 11 纯PLA、PLA-PP-g-MAH及LDHs(300)-SDBS/PLA-PP-g-MAH复合材料的DSC降温 (a) 和升温 (b) 曲线

Figure 11. DSC cooling (a) and heating (b) curves of neat PLA, PLA-PP-g-MAH and LDHs(300)-SDBS/PLA-PP-g-MAH composite

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图 12 纯PLA (a)、PLA-PP-g-MAH (b)、LDHs(300)-SDBS/PLA-PP-g-MAH (c)的POM图像

Figure 12. Polarizing images of neat PLA (a), PLA-PP-g-MAH (b) and LDHs(300)-SDBS/PLA-PP-g-MAH (c)

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图 13 PLA-PP-g-MAH、LDHs(300)-SDBS/PLA-PP-g-MAH、LDHs(300)/PLA-PP-g-MAH、LDHs-SDBS/PLA-PP-g-MAH、LDHs/PLA-PP-g-MAH和纯PLA的力学性能：(a) 冲击性能；(b) 拉伸强度

Figure 13. Mechanical properties of PLA-PP-g-MAH, LDHs(300)-SDBS/PLA-PP-g-MAH, LDHs(300)/PLA-PP-g-MAH, LDHs-SDBS/PLA-PP-g-MAH, LDHs/PLA-PP-g-MAH and neat PLA: (a) Impact strength; (b) Tensile strength

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表 1 不同温度焙烧后的水滑石(LDHs)

Table 1. Hydrotalcite (LDHs) calcined at different temperatures

Sample	Calcination temperature/℃
LDHs(200)	200
LDHs(250)	250
LDHs(300)	300
LDHs(350)	350
LDHs(400)	400

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表 2 不同温度下焙烧水滑石24 h的集中热分解温度

Table 2. Concentrated thermal decomposition temperature of hydrotalcite calcined at different temperatures for 24 h

Sample	T_1max of stage 1/℃	T_2max of stage 2/℃	∆T_max of stage 1/℃	Residual quantity/wt%
LDHs(200)	87.5	453.4	—	64.20
LDHs(250)	90.0	391.3	2.5	63.76
LDHs(300)	93.7	523.8	6.2	68.96
LDHs(350)	96.2	397.7	8.7	76.00
LDHs(400)	108.8	495.9	21.3	84.01
Notes: T_1max and T_2max—Maximum decomposition temperature in the first and second stage; ∆T_max—T₁_max–T₁_max(LDHs(200)).

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表 3 水滑石复合材料的纯样及共混物的集中热分解温度

Table 3. Temperature of concentrated thermal decomposition of the pure samples and blends of hydrotalcite composites

Sample	T_max of stage 1/℃	∆T_max of stage 1/℃	Char residue at 600℃/wt%
PLA-PP-g-MAH	364.5	−21.9	0.52
LDHs(300)-SDBS/PLA-PP-g-MAH	342.6	—	1.96
LDHs(300)/PLA-PP-g-MAH	327.3	15.3	1.46
LDHs-SDBS/PLA-PP-g-MAH	308.6	34.1	6.94
LDHs/PLA-PP-g-MAH	338.9	3.7	1.46
Neat PLA	363.9	−21.3	0.52
Notes: T_max—Maximum decomposition temperature in the first stage.

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表 4 水滑石复合材料纯样及共混物的玻璃转化温度T_g

Table 4. Glass transition temperature T_g of pure samples and blends of hydrotalcite composites

Sample	$ {T}_{\mathrm{g}} $(PLA)/ ℃	$ {T}_{\mathrm{g}} $(PP-g-MAH)/ ℃
PLA-PP-g-MAH	64.3	86.9
LDHs(300)-SDBS/PLA-PP-g-MAH	65.2	83.1
LDHs(300)/PLA-PP-g-MAH	65.5	83.9
LDHs-SDBS/PLA-PP-g-MAH	65.8	85.0
LDHs/PLA-PP-g-MAH	67.6	89.7
Neat PLA	64.9	—

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表 5 纯PLA、PLA-PP-g-MAH及LDHs(300)-SDBS/PLA-PP-g-MAH复合材料的DSC所得参数

Table 5. DSC parameters of neat PLA, PLA-PP-g-MAH and LDHs(300)-SDBS/PLA-PP-g-MAH composites

Sample	$ {T}_{\mathrm{g}}/{}^\circ \text{C} $	$ {T}_{\mathrm{c}\mathrm{c}} /{}^\circ \text{C}$	$ {T}_{\mathrm{m}}/{}^\circ \text{C} $	$ {\mathrm{\Delta }H}_{\mathrm{c}\mathrm{c}}\text{/}\left( \text{kJ}\cdot \text{mo}{{\text{l}}^{{-1}}} \right) $	$ {\mathrm{\Delta }H}_{\mathrm{m}} \text{/}\left( \text{kJ}\cdot \text{mo}{{\text{l}}^{{-1}}} \right) $	${\chi }_{\mathrm{c} }$/%
Neat PLA	56.6	117.4	149.4	−22.52	23.54	1.09
PLA-PP-g-MAH	59.4	110.7	147.1	−22.13	24.87	1.24
LDHs(300)-SDBS/PLA-PP-g-MAH	59.4	110.0	147.1	−25.94	28.41	2.93
Notes: $ {T}_{\mathrm{c}\mathrm{c}} $—Cold crystallization peak; $ {\mathrm{\Delta }H}_{\mathrm{c}\mathrm{c}} $—Cold crystallization enthalpy; $ {\mathrm{\Delta }H}_{\mathrm{m}} $—Melt crystallization; $ {\chi }_{\mathrm{c}} $—Degree of crystallinity; T_m—Meliling temperature.

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