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1.
 应用X射线衍射(XRD)、扫描电镜(SEM)、红外光谱(FT-IR)、核磁共振(NMR)和热重分析(TGA)等表征手段研究了以HF-三乙胺复合模板剂合成SAPO-34分子筛的晶化历程.结果表明,在晶化过程中有SAPO-5分子筛生成,而随着晶化时间的延长,SAPO-5逐渐消失.通过SEM可以看出,SAPO-34的晶化在60h内不断进行,直到生成晶面完美的SAPO-34分子筛晶体.NMR研究表明,晶化过程中先生成磷酸铝结构,随后硅原子逐渐进入SAPO-34分子筛骨架.对晶化不同时间的SAPO-34分子筛进行了甲醇制低碳烯烃反应的性能评价,发现晶化12h的分子筛样品已经具有良好的催化性能.  相似文献   

2.
模板剂对SAPO─34分子筛性能的影响   总被引:1,自引:0,他引:1  
分别以三乙胺、四乙基氢氧化铵以及二者的混合物为模板剂,采用水热法合成了三种SAPO-34分子筛样品。用化学分析、XRD、TPD和IR方法研究了不同模板剂对SAPO-34分子筛性能的影响。实验结果表明,四乙基氢氧化铵有利于硅进入分子筛骨架;三乙胺有利于生成较多的强酸中心;将三乙胺与四乙基氢氧化铵联用,能有效地调变所合成的SAPO-34的酸中心分布,使其对甲醇转化制低碳烯烃具有较高的选择性。  相似文献   

3.
分别以三乙胺、四乙基氢氧化铵以及二者的混合物为模板剂,采用水热法合成了三种SAPO-34分子筛样品。用化学分析、XRD、TPD和IR方法研究了不同模板剂对SAPO-34分子筛性能的影响。实验结果表明,四乙基氢氧化铵有利于硅进入分子筛骨架;三乙胺有利于生成较多的强酸中心;将三乙胺与四乙基氢氧化铵联用,能有效地调变所合成的SAPO-34的酸中心分布,使其对甲醇转化制低碳烯烃具有较高的选择性。  相似文献   

4.
杂原子ZSM-5、ZSM-11和ZSM-48型分子筛的合成   总被引:2,自引:0,他引:2  
在Na_2O-SiO_2-M_xO_y-H_2O体系中,以HMDA为模板剂用动态法和静态法合成了Ti-ZSM-48型分子筛,首次以85%(wt)HMDA+15%(wt)TPA ̄+为模板剂用低温陈化的静态法合成了第四周期过渡金属杂原子M-ZSM-5型分子筛,并与以HMDA、TPA ̄+为模板剂合成M-ZSM-5和以TBA ̄+为模板剂合成M-ZSM-11进行了对比研究。利用XRD技术跟踪晶体生长过程,考查了模板剂、合成方法、pH值、Na ̄+含量等因素对晶化动力学的影响,得出了合成各种杂原子分子筛的最佳条件。各种测试均表明杂原子进入了分子筛骨架。  相似文献   

5.
MCM-41中孔分子筛的合成及其性质   总被引:2,自引:2,他引:0  
以十六烷基三甲基溴化铵(CTAB)作模板剂,研究了水热体系中中孔MCM-41分子筛的合成条件。在H_2O/Si介于12~100,Si/Al介于10~∞,CTAB/Si介于0.08~0.2时,可以合成出MCM-41分子筛。在加入煤油等混合烃的合成体系中,可以合成出孔径大于4nm的MCM-41分子筛。用XRD、SEM、N_2吸附对合成样品加以表征,证明它们具有典型的中孔分子筛特性。探针反应证明它具有中强酸中心。  相似文献   

6.
汪杰  涂永善  杨朝合 《催化学报》2003,24(6):452-456
 采用阳离子表面活性剂十六烷基三甲基溴化铵为模板剂,以正硅酸乙酯为硅源,以硫酸铝为铝源,水热合成了以催化油浆窄馏分为添加剂的高比表面积Al-MCM-41介孔分子筛,并利用XRD,HREM,TG-DTA及N2吸附-脱附等测试手段对合成样品进行了表征.合成的Al-MCM-41分子筛的比表面积和孔体积分别达到1295m2/g和1.5cm3/g,其平均孔径为4.3nm.重点研究了Al-MCM-41分子筛结晶度、晶胞参数、比表面积、孔体积及平均孔径等结构性质随催化油浆窄馏分添加量及其组成的变化规律,并从合成机理上进行了解释.  相似文献   

7.
分别以三乙胺,四乙基氢氧化铵及二者的混合物为模板剂合成了硅磷酸铝分子筛SAPO-34。应用XRD,SEM,DTA和NH3-TPD等方法考察了合成产品的物化性能,所得结果表明,模板剂的种类对SAPO-34的晶粒大小和酸性质有显著影响。在甲醇转化制低碳烯烃的过程中,以不同模板剂合成的SAPO-34的催化性能也不同,其中,以双模板剂合成的分子筛具有较高的低碳烯烃选择性。  相似文献   

8.
 以吗啉(C4H9NO)为主要模板剂,以少量四乙基氢氧化铵(TEAOH)为辅助模板剂合成了SAPO -34分子筛,并用氨吸附红外、核磁共振和氮吸附等手段对合成的SAPO-34分子筛进行了表 征. 结果表明,与单独以吗啉为模板剂合成的样品相比,用复合模板剂合成的分子筛样品的比 表面积和孔体积均有所增大; 由于在分子筛骨架中形成了“硅岛”,使其B酸量有所增加 ,对甲醇制低碳烯烃反应的催化性能有所改善.  相似文献   

9.
Cu-HMS分子筛的合成条件及其催化性能   总被引:12,自引:0,他引:12  
张美英  王乐夫  黄仲涛 《催化学报》2003,24(12):914-918
 以十二胺(DDA)为模板剂,正硅酸乙酯(TEOS)为硅源,在中性介质中于室温条件下合成了含Cu的中孔杂原子分子筛Cu-HMS.在85℃及常压下,以异丙苯氧化(O2为氧化剂)为探针反应考察了Cu源、Cu/Si摩尔比、DDA/TEOS摩尔比和晶化时间等合成条件对分子筛催化氧化性能的影响.实验结果发现,在Cu/Si摩尔比为0.02~0.03,DDA/TEOS摩尔比为0.1~0.3,晶化时间为1h以上,Cu源为Cu(NO3)2的条件下得到的Cu-HMS分子筛催化活性最高.用XRD,29SiMASNMR,FT-IR,低温N2吸附和原子发射光谱(ICP)等手段对催化活性最高的分子筛样品的结构及表面性质进行了表征,证明该分子筛具有典型的HMS结构,同时发现Cu元素已进入分子筛骨架结构.  相似文献   

10.
CoAPSO-34分子筛的合成与性能   总被引:3,自引:0,他引:3  
以三乙胺为模板剂,在碱性条件下用水热晶化法将钴元素引入了硅磷铝分子筛骨架,合成出CoAPSO-34分子筛.实验表明,在碱性介质中以低价态引入的钴元素首先转化为高价态Co(Ⅲ),然后才进入分子筛骨架。利用X射线粉末衍射和红外光谱对其进行了结构分析,确认钴元素进入了分子筛骨架.利用程序升温氨脱附和氨法红外光谱考察了CoAPSO-34的表面酸性.将CoAPSO-34用作甲醇转化的催化剂时,随钴含量增高,催化剂稳定性下降,反应产物中C=2~C=4烯烃的选择性升高  相似文献   

11.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

12.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

13.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

14.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

15.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

16.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

17.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.  相似文献   

18.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

19.
Zhanhui Yang  Shiyi Yang  Jiaxi Xu 《Tetrahedron》2017,73(23):3240-3248
Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.  相似文献   

20.
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