超声辅助法制备片状Ca-Mg复相碳酸盐及其对PBAT复合材料性能的影响

罗文倩; 何丽秋; 黎京鸿; 王吉林; 李世令; 阳鹏; 莫淑一; 龙飞

超声辅助法制备片状Ca-Mg复相碳酸盐及其对PBAT复合材料性能的影响

罗文倩¹,
何丽秋¹,
黎京鸿¹,
王吉林^{1, 2},
李世令³,
阳鹏³,
莫淑一^{1, 2, ,},
龙飞^{1, 2}

1.
桂林理工大学材料科学与工程学院, 广西无机纳米粉体及应用工程研究中心, 桂林 541000
2.
广西光电材料与器件重点实验室, 桂林 541004
3.
桂林金山新材料有限公司, 桂林 541000

基金项目: 广西重大科技专项(桂科AA18242041)

详细信息

通讯作者:
莫淑一，硕士，助理研究员，研究方向：精细碳酸钙开发和产业化　E-mail: moshuyi@glut.edu.cn

中图分类号: TB332;TQ623.4
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- 文章访问数: 23
- HTML全文浏览量: 21
- 被引次数: 0
出版历程
- 收稿日期: 2024-02-01
- 修回日期: 2024-03-10
- 录用日期: 2024-03-16
- 网络出版日期: 2024-04-17

Preparation of flake Ca-Mg composite carbonate by ultrasonic assisted method and its effect on the properties of PBAT composites

LUO Wenqian¹,
HE Liqiu¹,
LI Jinghong¹,
WANG Jilin^{1, 2},
LI Shiling³,
YANG Peng³,
MO Shuyi^{1, 2
, ,},
LONG Fei^{1, 2}

1.
College of Materials Science and Engineering, Guilin University of Technology, Guangxi Research Center of Inorganic Nano Powder and Application Engineering, Guilin 541000, China
2.
Guangxi Key Laboratory of Optical and Electronic Materials and Devices, Guilin 541000, China
3.
Guilin Jinshan New Material Co., Ltd, Guilin 541000, China

Funds: Financial support from Guangxi Science and Technology Plan Project (Guike AA18242041)

摘要

摘要: 片状碳酸盐类材料凭借无毒、价廉和原料来源丰富等优点已成为重要的热塑性聚合物增强增刚无机填料，但其制备工艺复杂，难以实现量产。本文结合石灰石产业中低品位石灰石附加值不高的问题，以含Mg的石灰石为原料，采用超声辅助碳化法制备了片状Ca-Mg复相碳酸盐(FCM)。探究了不同Mg含量、不同碳化反应温度、不同超声功率等工艺参数对产物形貌的影响。在此基础之上，将活性FCM与聚对苯二甲酸-己二酸丁二醇酯(PBAT)树脂共混挤出造粒后加工成复合材料，对比研究了添加不同种类的填料和不同配比对复合材料性能影响。结果表明，Mg含量、超声功率、反应温度对Ca-Mg复相碳酸盐的形貌有显著的影响，随着Mg含量提升到20.61wt%、反应温度提升至70℃、超声功率提升到400 W，得到了具有大量片状结构、比表面积为23.5 m²/g的Ca-Mg复相碳酸盐产物；添加了活性FCM的复合材料展现出优异的力学性能，当活性FCM添加量为20wt%时，复合材料的冲击强度、弯曲强度和弯曲模量分别较纯PBAT提升1倍、2倍和2.8倍；当添加量为40wt%时，这些性能指标进一步提升，分别比纯PBAT提升了1.2倍、2.6倍和4.8倍；更重要的是，添加了活性FCM的复合材料土壤降解率显著提高，这将有效促进复合材料在使用后降解，使其在完成服役使命后能够迅速融入自然环境，进一步体现其环保和可持续的特性。
- 片状Ca-Mg复相碳酸盐 /
- 超声辅助 /
- PBAT /
- 复合材料 /
- 力学性能 /
- 土壤降解
Abstract: Flaky carbonate materials have become important thermoplastic polymer reinforced rigid inorganic fillers due to their advantages of non-toxicity, low cost and abundant raw materials. However, their preparation process is complex and difficult to achieve mass production. In this paper, combined with the problem of low added value of low-grade limestone in limestone industry, flaky Ca-Mg complex carbonates (FCM) were prepared by ultrasonic-assisted carbonization method using Mg-containing limestone as raw material. The effects of process parameters such as different Mg content, different carbonization reaction temperature and different ultrasonic power on the morphology of the product were investigated. On this basis, the active FCM and poly (butylene adipate-co-terephthalate) (PBAT) resin were blended and extruded into composites. The effects of different kinds of fillers and different ratios on the properties of composites were compared. The results show that Mg content, ultrasonic power and reaction temperature have a significant effect on the morphology of Ca-Mg composite carbonate. With the increase of Mg content to 20.61wt%, reaction temperature to 70℃ and ultrasonic power to 400 W, Ca-Mg composite carbonate products with a large number of flake structures and a specific surface area of 23.5 m²/g were obtained. The composites with active FCM showed excellent mechanical properties. When the content of active FCM was 20wt%, the impact strength, flexural strength and flexural modulus of the composites were 1 time, 2 times and 2.8 times higher than those of pure PBAT, respectively. When the addition amount is 40wt%, these performance indexes are further improved, which are 1.2 times, 2.6 times and 4.8 times higher than that of pure PBAT, respectively. More importantly, the soil degradation rate of the composite material added with the active FCM is significantly improved, which will effectively promote the degradation of the composite material after use, so that it can quickly integrate into the natural environment after completing the service mission, further reflecting its environmental protection and sustainable characteristics.
- Flaky Ca-Mg complex carbonate /
- ultrasound assistance /
- PBAT /
- composite materials /
- mechanical properties /
- soil degradation

HTML全文

图 1 Ca-Mg复相碳酸盐(FCM)的制备工艺

Figure 1. Preparation process of Ca-Mg complex phase carbonate (FCM)

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图 2 不同制备工艺所得Ca-Mg复相碳酸盐的XRD图谱以及局部放大图

(a) 不同Mg含量、不同碳化反应温度、不同超声功率制备的Ca-Mg复相碳酸盐的XRD图谱; (b) 局部放大图

Figure 2. XRD patterns and local magnification of Ca-Mg composite carbonates obtained by different preparation processes

(a) XRD patterns of Ca-Mg composite carbonates prepared with different Mg contents, different carbonization reaction temperatures and different ultrasonic powers; (b) Local enlargement

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图 3 不同制备工艺所得Ca-Mg复相碳酸盐的微观形貌图及Ca-Mg-20.61的EDS面谱图

(a) Ca-Mg-0.459, (b) Ca-Mg-4.89, (c) Ca-Mg-14.05, (d) Ca-Mg-20.61, (e) 200 W-Ca-Mg-20.61, (f) 0 W-Ca-Mg-20.61, (g) RT-Ca-Mg-20.61, (h) Ca-Mg-20.61的EDS面谱图

Figure 3. SEM images of Ca-Mg composite carbonate obtained by different preparation processes and the EDS spectra of Ca-Mg-20.61 were obtained

(a) Ca-Mg-0.459, (b) Ca-Mg-4.89, (c) Ca-Mg-14.05, (d) Ca-Mg-20.61, (e) 200 W-Ca-Mg-20.61, (f) 0 W-Ca-Mg-20.61, (g) RT-Ca-Mg-20.61, (h) EDS elemental mapping of Ca-Mg-20.61

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图 4 不同种类填料的微观形貌图

(a) 活性FCM,(b) 活性PCC,(c) 活性UGCC,(d) 活性GCC

Figure 4. SEM of different kinds of inorganic filler

(a) Active FCM, (b) Active PCC, (c) Active UGCC, (d) Active GCC

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图 5 聚对苯二甲酸-己二酸丁二醇酯(PBAT)复合材料的熔融指数变化曲线

Figure 5. Melt index curve of poly (butylene adipate-co-terephthalate) (PBAT) composite materials

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图 6 PBAT复合材料的微观形貌图

(a, b) P-0, (c) P-20 FCM, (d) P-40 FM, (e) P-20 PCC, (f) P-40 GCC, (g) P-20 UGCC, (h) P-40 UGCC, (i) P-20 GCC, (j) P-40 GCC

Figure 6. The SEM Morphology of PBAT matrix composites

(a, b) P-0, (c) P-20 FCM, (d) P-40 FM, (e) P-20 PCC, (f) P-40 GCC, (g) P-20 UGCC, (h) P-40 UGCC, (i) P-20 GCC, (j) P-40 GCC

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图 7 不同填充量、不同填料对PBAT力学性能的影响

(a) 复合材料的拉伸强度和冲击强度图, (b) 复合材料的弯曲强度和弯曲模量图

Figure 7. The effect of different filling amounts and inorganic filler on the mechanical properties of PBAT

(a) Tensile strength and impact strength diagram of the composite material, (b) Flexural strength and flexural modulus diagram of the composite material

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图 8 PBAT复合材料的土壤降解率

Figure 8. Soil degradation rate of PBAT composite materials

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表 1 石灰石的主要成分及含量(wt%)

Table 1. Main components and content of limestone (wt%)

Sample	CaO	MgO	SiO₂	Al₂O₃	Loss on ignition
Ca-0.459	54.99	0.459	0.353	0.108	44.09
Ca-4.89	48.87	4.89	0.658	0.233	45.349
Ca-14.05	37.56	14.05	1.16	0.414	46.816
Ca-20.61	34.65	20.61	1.08	0.387	43.273

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表 2 Ca-Mg复相碳酸盐反应条件

Table 2. Reaction conditions of Ca-Mg composite calcium carbonate

Sample	Mg content (MgOwt%)	Ultrasonic power /W	Reaction temperature /℃
Ca-Mg-0.459	0.459	400	70
Ca-Mg-4.89	4.89	400	70
Ca-Mg-14.05	14.05	400	70
Ca-Mg-20.61	20.61	400	70
200 W-Ca-Mg-20.61	20.61	200	70
0 W-Ca-Mg-20.61	20.61	0	70
RT- Ca-Mg-20.61	20.61	400	30
Note: Mg content was used as the pronoun of MgO content detected by X-ray fluorescence spectrometer

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表 3 复合材料的加工配方比例

Table 3. Processing formula ratio of composite materials

Sample	Type of fillers	Filler/wt%	PBAT/wt%	Assistant/wt%
P-0	/	/	95	5
P-20FCM	Active FCM	20	75	5
P-40FCM	Active FCM	40	55	5
P-20PCC	Active PCC	20	75	5
P-40PCC	Active PCC	40	55	5
P-20UGCC	Active UGCC	20	75	5
P-40UGCC	Active UGCC	40	55	5
P-20GCC	Active GCC	20	75	5
P-40GCC	Active GCC	40	55	5
Notes: PCC—Precipitated Calcium Carbonate; GCC—Ground Calcium Carbonate; UGCC—Ultrafine Ground Calcium Carbonate.

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表 4 不同种类填料性能测试

Table 4. Performance test of different kinds of fillers

Sample	Type	Oil absorption value/%	Whiteness/%	Degree of activation/%	Contact angle /(°)	specific surface area /(m²·g⁻¹)
Active FCM	PCC	59.7	97.5	99.9	122.1	23.5
Active PCC	PCC	24.8	94.3	99.8	119.6	7.1
Active UGCC	GCC	20.0	96.2	99.9	120.1	9.8
Active GCC	GCC	15.6	90.0	99.7	116.8	3.6

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表 5 活性FCM添加量为50wt%时PBAT复合材料的配方比例及力学性能测试结果

Table 5. Formula ratio and mechanical properties of the PBAT composites with 50wt% active FCM addition were tested

Sample	FCM addition amount/wt%	PBAT/wt%	assistant/wt%	Mechanical property
Sample	FCM addition amount/wt%	PBAT/wt%	assistant/wt%	Tensile strength /MPa	Impact strength/ (kJ·m⁻²)	Flexural strength/ MPa	Flexural Modulus/ MPa
P-50 FCM	50	45	5	3.57	12.85	11.81	498.73
				3.68	11.15	12.78	481.35
				3.40	12.43	14.90	486.91
				3.76	9.32	10.67	497.66
				3.31	10.78	10.09	500.10
				3.54(Average)	11.30(Average)	12.05(Average)	492.95(Average)

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