Page 174 - 《精细化工》2020年第4期
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第 37 卷第 4 期                             精   细   化   工                                  Vol.37, No.4
             202 0 年 4 月                             FINE CHEMICALS                                 Apr.    2020


              橡塑助剂
                          α-酮戊二酸镧的制备、复配及其对 PVC


                                            热稳定性能的影响



                                                于   静    1,2 ,李敏贤      1,2

                 (1.  唐山师范学院  化学系,河北  唐山    063000;2.  唐山市绿色专用化学品重点实验室,河北  唐山    063000)

                 摘要:以α-酮戊二酸、硝酸镧、氢氧化钠为原料,水为溶剂,经两步法制备了α-酮戊二酸镧(ATAL)。采用元
                 素分析、ICP-OES 和 FTIR 对产物结构进行了表征。通过刚果红试纸法和转矩流变仪法分别测试了产品对聚氯
                 乙烯(PVC)的静态热稳定作用和动态热稳定作用,通过 TGA 研究了产品对 PVC 热降解动力学的影响,并将
                 产品与二苯甲酰基甲烷(β-二酮)、亚磷酸-苯二异辛酯(PDOP)、季戊四醇(PER)、环氧豆油(ESO)等辅助
                 热稳定剂复配,考察其协同性能,采用 SEM 观察热降解不同时间的 PVC 的微观表面形貌。结果表明,α-酮戊
                 二酸镧对 PVC 具有较好的热稳定作用,添加 3%(质量分数,以 PVC 粉为基准)时,静态热稳定时间可达 13 min,
                 动态热稳定时间可达 1820 s,可将 PVC 热降解过程的平均活化能提高 15.78 kJ/mol,其与 PER 之间协同作用最
                 佳,复合热稳定剂对 PVC 的静态热稳定时间达 37  min,动态热稳定时间达 3480  s。SEM 观察发现复合热稳定
                 剂能较好地抑制 PVC 降解着色。
                 关键词:α-酮戊二酸镧;热稳定剂;热稳定性能;复配;橡塑助剂
                 中图分类号:TQ325.3      文献标识码:A      文章编号:1003-5214 (2020) 04-0808-07


                     Preparation and composition of lanthanum α-ketoglutarate and its

                                      effect on the thermal stability of PVC


                                                                      1,2
                                                         1,2
                                                 YU Jing , LI Minxian
                 (1. Department of Chemistry,  Tangshan Normal University,  Tangshan  063000, Hebei, China;  2.  Tangshan Key
                 Laboratory of Green Specialty Chemicals, Tangshan 063000, Hebei, China)

                 Abstract: Lanthanum  α-ketoglutarate (ATAL) was prepared by  two-step  method using α-ketoglutarate,
                 lanthanum  nitrate  and  sodium  hydroxide  as  raw  materials  and  water  as  solvent.  Its  structure  was
                 characterized by elemental analysis, ICP-OES and FTIR. The static thermal stability and dynamic thermal
                 stability of lanthanum α-ketoglutarate as a thermal stabilizer on polyvinyl chloride (PVC) was tested by
                 Congo  red  test  paper  and  torque  rheometer,  respectively.  The  effect  of  the  product  on  the  thermal
                 degradation kinetics of PVC was studied by TGA. The product was compounded with auxiliary thermal
                 stabilizers such as dibenzoylmethane (β-dione), diisooctyl phenyl phosphite (PDOP), pentaerythritol (PER)
                 and  epoxidized  soybean  oil  (ESO)  to  investigate  their  synergistic  effects.  The  microscopic  surface
                 morphology of PVC degraded at different time was observed by SEM. The results show that lanthanum
                 α-ketoglutarate has good thermal stability for PVC. When 3% (mass fraction, based on the mass of PVC
                 powder) lanthanum α-ketoglutarate was added, the static thermal stabilization time of PVC could reach 13
                 min and the dynamic thermal stabilization time could reach 1820 s. The average activation energy of PVC
                 thermal degradation process could be increased by 15.78 kJ/mol. The synergistic effect between lanthanum
                 α-ketoglutarate and PER was the best. For the composite thermal stabilizer [m(ATAL)∶m(PER)=1∶1.5],
                 the static thermal stabilization time of PVC was 37 min and the dynamic thermal stabilization time was
                 3480 s. SEM results revealed that the composite thermal stabilizer could inhibit the degradation coloring of PVC.


                 收稿日期:2019-08-24;  定用日期:2019-11-18; DOI: 10.13550/j.jxhg.20190813
                 基金项目:河北省科技厅重点研发计划项目(17211411);唐山市科技计划项目(17110214a);唐山师范学院团队重点项目(2018B02)
                 作者简介:于   静(1982—),男,副教授,E-mail:yeyue130@163.com。
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