首先制备了2种磺酸功能化的有机聚苯乙烯/无机磷酸氢锆非均相催化剂,运用傅里叶红外光谱(FT-IR)、N2吸附-脱附测试、X射线衍射(XRD)、扫描电子显微镜(SEM)等测试技术对催化剂进行了表征,提出了催化剂可能的模型。其次,考察了非均相催化...首先制备了2种磺酸功能化的有机聚苯乙烯/无机磷酸氢锆非均相催化剂,运用傅里叶红外光谱(FT-IR)、N2吸附-脱附测试、X射线衍射(XRD)、扫描电子显微镜(SEM)等测试技术对催化剂进行了表征,提出了催化剂可能的模型。其次,考察了非均相催化剂催化合成环氧化大豆油的催化性能。结果表明:以叔丁基过氧化氢(TBHP)为氧化剂,固体催化剂对大豆油的环氧反应具有良好的催化性能,相比于催化剂1(磺酸化低聚苯乙烯基膦酸-磷酸氢锆),在相同的条件下,催化剂2(磺酸化聚(苯乙烯-苯乙烯膦酸)-磷酸氢锆)表现出更高的催化活性(产率:58.6% vs 53.3%),这主要归因于催化剂2拥有更大的比表面积、孔容以及孔径,为底物和催化剂的接触提供足够的催化场所。催化剂2重复使用7次后,催化活性未见明显降低。第8次反应结束后,将其置于2 mol·L^-1稀盐酸中静置过夜后,在进行第9和10次循环时,催化活性又得以恢复。展开更多
Chloromethyl-zirconium oligo-polystyrenyl-phosphonatephosphate was used as the support of salen Mn(Ⅲ) which was synthesized by statistical method.The chloromethyl group of the support reacted with the free hydroxy of...Chloromethyl-zirconium oligo-polystyrenyl-phosphonatephosphate was used as the support of salen Mn(Ⅲ) which was synthesized by statistical method.The chloromethyl group of the support reacted with the free hydroxy of salen,and then with Mn(OAc)2·4H2O,so a new type of salen Mn(Ⅲ) catalyst supported on zirconium oligo-polystyrenyl-phosphonate-phosphate was synthesized.The catalyst was characterized by IR,SEM,element analysis and BET surface area.展开更多
：The crystalline layered and amorphous samples of Zr(HPO4)[O3PCH2N(CH2CO2H)2]· nH2O(n=1,2)(c-or a-ZPPMIDA) and Zr(HPO4)[O3PCH2N(CH2CH2)2O]· nH2O)(n=1,2) (c- or a-ZPMMPA) were prepared with zirconium oxychlo...：The crystalline layered and amorphous samples of Zr(HPO4)[O3PCH2N(CH2CO2H)2]· nH2O(n=1,2)(c-or a-ZPPMIDA) and Zr(HPO4)[O3PCH2N(CH2CH2)2O]· nH2O)(n=1,2) (c- or a-ZPMMPA) were prepared with zirconium oxychloride, sodium dihydrogen phosphate and H2O3PCH2N(CH2CH2)2O(MMPA) or H2O3PCH2N(CH2CO2H)2(PMIDA) in the presence or absence of hydrofluoric acid for the first time.The samples were comparatively characterized by XRD,IR, TG-DTA and elemental analysis. The interlayer spacings of c-ZPPMIDA and c-ZPMMPA were also measured and calculated. XRD results showed that interlayer spacings of c- ZPMMPA and c-ZPPMIDA were 16.055? and 15.384? respectively. The similar structure Zr[(O3PCH2)2NCH2 CO2H]· H2O(ZGDMP) were used to analytically compare with c-ZPMMPA and c-ZPPMIDA. The influences of distribution and rigidity of organic groups on the interlayer spacing were discussed.展开更多
基金supported by the Basic and Frontier Research Project of Chongqing (cstc2013jcyjA50013)Scientific and Technological Research Program of Chongqing Municipal Education Commission (KJ131504)the Innovation Team Building at Institutions of Higher Education in Chongqing (KJTD201325)~~
文摘首先制备了2种磺酸功能化的有机聚苯乙烯/无机磷酸氢锆非均相催化剂,运用傅里叶红外光谱(FT-IR)、N2吸附-脱附测试、X射线衍射(XRD)、扫描电子显微镜(SEM)等测试技术对催化剂进行了表征,提出了催化剂可能的模型。其次,考察了非均相催化剂催化合成环氧化大豆油的催化性能。结果表明:以叔丁基过氧化氢(TBHP)为氧化剂,固体催化剂对大豆油的环氧反应具有良好的催化性能,相比于催化剂1(磺酸化低聚苯乙烯基膦酸-磷酸氢锆),在相同的条件下,催化剂2(磺酸化聚(苯乙烯-苯乙烯膦酸)-磷酸氢锆)表现出更高的催化活性(产率:58.6% vs 53.3%),这主要归因于催化剂2拥有更大的比表面积、孔容以及孔径,为底物和催化剂的接触提供足够的催化场所。催化剂2重复使用7次后,催化活性未见明显降低。第8次反应结束后,将其置于2 mol·L^-1稀盐酸中静置过夜后,在进行第9和10次循环时,催化活性又得以恢复。
文摘Chloromethyl-zirconium oligo-polystyrenyl-phosphonatephosphate was used as the support of salen Mn(Ⅲ) which was synthesized by statistical method.The chloromethyl group of the support reacted with the free hydroxy of salen,and then with Mn(OAc)2·4H2O,so a new type of salen Mn(Ⅲ) catalyst supported on zirconium oligo-polystyrenyl-phosphonate-phosphate was synthesized.The catalyst was characterized by IR,SEM,element analysis and BET surface area.
文摘：The crystalline layered and amorphous samples of Zr(HPO4)[O3PCH2N(CH2CO2H)2]· nH2O(n=1,2)(c-or a-ZPPMIDA) and Zr(HPO4)[O3PCH2N(CH2CH2)2O]· nH2O)(n=1,2) (c- or a-ZPMMPA) were prepared with zirconium oxychloride, sodium dihydrogen phosphate and H2O3PCH2N(CH2CH2)2O(MMPA) or H2O3PCH2N(CH2CO2H)2(PMIDA) in the presence or absence of hydrofluoric acid for the first time.The samples were comparatively characterized by XRD,IR, TG-DTA and elemental analysis. The interlayer spacings of c-ZPPMIDA and c-ZPMMPA were also measured and calculated. XRD results showed that interlayer spacings of c- ZPMMPA and c-ZPPMIDA were 16.055? and 15.384? respectively. The similar structure Zr[(O3PCH2)2NCH2 CO2H]· H2O(ZGDMP) were used to analytically compare with c-ZPMMPA and c-ZPPMIDA. The influences of distribution and rigidity of organic groups on the interlayer spacing were discussed.
