新型PVC辅助热稳定剂乙酰丙酮镁的制备及热稳定性能

doi:10.16085/j.issn.1000-6613.2018-1298

摘要/Abstract

摘要：

以氢氧化镁[Mg(OH)₂]和乙酰丙酮为原料，乙醇为溶剂，通过一步异相沉淀转化法制备配合物乙酰丙酮镁[Mg(acac)₂]，用作聚氯乙烯（PVC）辅助热稳定剂。首先，采用XRD、FTIR、TG对产物进行了结构表征，然后通过静态热老化试验和刚果红试验，对乙酰丙酮镁的热稳定性能进行研究。结果表明，成功制备出产物乙酰丙酮镁，且含有2个结晶水；在PVC中，当主效热稳定剂与辅助热稳定剂的质量比为3∶5时，PVC 的热稳定时间长达57min。该生产技术克服了乙酰丙酮镁传统合成方法产率低、操作过程复杂、污染等缺点，制备的产物乙酰丙酮镁与主效热稳定剂具有良好的协同作用，可以有效提高PVC的热稳定性能。

关键词: 乙酰丙酮镁, 配合物, 优化, 制备, PVC热稳定剂

Abstract:

Magnesium acetylacetonate used as a polyvinyl chloride (PVC) auxiliary heat stabilizer was synthesized from magnesium hydroxide [Mg(OH)₂] and acetylacetone as raw materials and ethanol as solvent by one-step heterogeneous precipitation conversion technology. The as-prepared magnesium acetylacetonate was characterized by XRD, FTIR and TG-TGA, and its thermal stability was studied by static thermal aging and Congo red test paper.The results show that the prepared product is magnesium acetylacetonate and contains two crystalline water. In PVC, when the mass ratio of the main thermal stabilizer and the auxiliary heat stabilizer is 3∶5, the thermal stability time of PVC is up to 57min. The production technology overcomes the disadvantages of low yield, complex operation and pollution of the traditional method of synthesis of magnesium acetylacetonate. The prepared product has a good synergistic effect with the main heat stabilizer, and can effectively improve the thermal stability of PVC.

Key words: magnesium acetylacetonate, complex, optimization, preparation, PVC heat stabilizer.

中图分类号:

TQ314.24

李晓斌, 陈颖, 胡程程, 陈祥迎, 李平, 黄先胜. 新型PVC辅助热稳定剂乙酰丙酮镁的制备及热稳定性能[J]. 化工进展, 2019, 38(04): 1862-1871.

Xiaobin LI, Ying CHEN, Chengcheng HU, Xiangying CHEN, Ping LI, Xiansheng HUANG. Preparation and properties of a new PVC auxiliary heat stabilizer——magnesium acetylacetonate[J]. Chemical Industry and Engineering Progress, 2019, 38(04): 1862-1871.

图/表 18

图1 一步异相沉淀转化技术反应机理图

图2 样品与标样的红外光谱图

图3 样品与标样的XRD图谱

图4 样品热失重曲线图

图5 样品与标样的热失重曲线图

表1 乙酰丙酮镁元素含量分析

元素	测定值/%	理论值/%
C	45.58	46.51
H	7.53	6.98
Mg	9.22	9.30

表2 主辅热稳定剂协同作用试验配方

样品编号	PVC/g	Mg(acac)₂/g	CaSt₂/g	ZnSt₂/g
1	50	0	0	0
2	50	0	0.375	0.125
3	50	0.3	0	0
4	50	0.3	0.375	0.125

图6 主辅热稳定剂协同作用刚果红试验结果图

表3 主辅热稳定剂热老化试验结果图

样品	热老化时间/min
样品	0	10	20	30	40	50	60	70	80	90
1
2
3
4

表4 主效热稳定剂中钙锌含量最佳配比试验配方

样品编号	PVC/g	Mg(acac)₂/g	CaSt₂/g	ZnSt₂/g
1	50	0	0	0
2	50	0.3	0.25	0.25
3	50	0.3	0.33	0.17
4	50	0.3	0.375	0.125
5	50	0.3	0.4	0.1

图7 不同钙锌含量配比刚果红试验结果

表5 不同钙锌含量主效热稳定剂热老化试验结果图

样品	热老化时间/min
样品	0	10	20	30	40	50	60	70	80	90
1
2
3
4
5

表6 主辅热稳定剂质量比配方

样品编号	PVC/g	Mg(acac)₂/g	CaSt₂/g	ZnSt₂/g
1	50	0	0.375	0.125
2	50	0.1	0.375	0.125
3	50	0.2	0.375	0.125
4	50	0.3	0.375	0.125
5	50	0.4	0.375	0.125

图8 不同主辅热稳定剂质量比刚果红试验结果

表7 不同主辅热稳定剂质量比热老化试验结果图

样品	热老化时间/min
样品	0	10	20	30	40	50	60	70	80	90
1
2
3
4
5

图9 样品与商业化产品对比刚果红试验结果

表8 样品与商业化产品对比热老化试验结果图

辅助稳定剂	热老化时间/min
辅助稳定剂	0	10	20	30	40	50	60	70	80	90
乙酰丙酮钙
乙酰丙酮锌
环氧大豆油
乙酰丙酮镁

图10 热稳定剂作用机理图

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