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Frontiers of Chemical Science and Engineering 2013年第2期7卷 202-209页

作者： Hainan SHI Yaquan WANG Guoqiang WU Wenping FENG Yi Lin Teng ZHANG Xing JIN Shuhai WANG Xiaoxue WU Pengxu YAO Key Laboratory for Green Chemical Technology of the Ministry of Education School of Chemical Engineering & Technology Yianjin University Tianjin 300072 China

ts-1/sio2 catalyst for the epoxidation of propylene with hydrogen peroxide in a fixed-bed reactor has been investigated. The catalyst activity decreases gradually with the online reaction time, but the selectivity of propylene epoxide is kept at about 93%. The fresh, deactivated and regenerated catalysts were characterized with X-ray diffraction, Fourier transform infrared spectro- scopy, ultra-violet-visible diffuse reflectance, Brunner- Emmett-TeUer method and thermogravimetric analysis, and the deactivated catalyst was regenerated with H2O2/ methanol solution. Compared with the fresh catalyst, both the framework structure and the content of titanium in the framework of the deactivated and regenerated ts-1/sio2 catalysts were not changed. The major reason of the catalyst deactivation was the blockage of the channels of the catalyst by bulky organic by-products, which covered the active centers of titanium in ts-1. The deposited materials on the deactivated ts-1/sio2 catalyst could be removed by treatment with hydrogen peroxide/methanol solution or pure methanol; the higher the treatment temperature and the higher the concentration of H2O2 in methanol, the higher the extent of the regeneration. The regeneration treatment did not influence the product selectivity in the propylene epoxidation.

关键词： ts-1/sio2 epoxidation of propylene fixed-bed reactor deactivation regeneration

TPA+在ts-1/sio2催化剂表面修饰过程中的作用

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TPA+在TS-1/SiO2催化剂表面修饰过程中的作用

Highly Effective Propylene Epoxidation over ts-1/sio_(2) Hydrothermally Treated

第18届全国分子筛学术大会

作者：宋万仓龙化云王祥生大连理工大学化工与环境生命学部化工学院工业催化系

HPPO技术是一种清洁生产环氧丙烷(PO)的工艺,该工艺为原子经济反应,副产物只有水。ts-1催化剂是HPPO工艺的核心,制备高性能的ts-1催化剂对HPPO工艺具有重要意义。采用碱溶液对分子筛催化剂进行水热处理,能显著改善催化剂的扩散性能,从... 详细信息

HPPO技术是一种清洁生产环氧丙烷(PO)的工艺,该工艺为原子经济反应,副产物只有水。ts-1催化剂是HPPO工艺的核心,制备高性能的ts-1催化剂对HPPO工艺具有重要意义。采用碱溶液对分子筛催化剂进行水热处理,能显著改善催化剂的扩散性能,从而提高催化剂的催化性能。

关键词：钛硅分子筛(ts-1) ts-1/sio2 水热改性 TPABr

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Chinese Chemical Letters 2005年第1期16卷 103-106页

作者： WeiGuoCHENG XiangShengWANG GangLI XinWenGUO QingSongLIN DepartmentofCatalysisChemistryandEngineeringandStateKeyLab.ofFineChem. DalianUniv.ofTechnol.Dalian116012

The propylene epoxidation over ts-1/sio2 catalyst hydrothermally treated was investigated. It was found by EPR characterization that two types of Ti (IV)-superoxide radicals, A (gz=2.0271; gy=2.0074; gx=2.0010) and B (gz=2.0247; gy= 2.0074; gx= 2.0010), were observed for ts-1/sio2. The superoxo species A converted to B after ts-1/sio2 catalyst was hydrothermally treated. The results show that over ts-1/sio2 catalyst hydrothermally treated at 170℃, about 95% conversion of H2O2 with above 94% PO selectivity is obtained during continuous running for 300 h under the conditions of reaction temperature 45℃, 0.5 h-1WHSV of propylene.

关键词： Hydrothermal ts-1/sio2 propylene epoxidation EPR radical.

Post-treatment of ts-1 with Mixtures of TPAOH and Ammonium Salts and the Catalytic Properties in Propylene Epoxidation

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Transactions of Tianjin University 2018年第5期24卷 461-470页

作者： Yaquan Wang Xinpeng Han Haoyang Li Xiao Wang Key Laboratory for Green Chemical Technology of Ministry of Education School of Chemical Engineering and TechnologyTianjin University

ts-1/sio_2 extrudate was post-treated with mixed solution of tetrapropyl ammonium hydroxide(TPAOH)and various ammonium salts solution(NH_4F,(NH_4)_3PO_4,(NH_4)_2CO_3,(NH_4)_2SO_4,NH_4CH_3CO_2,NH_4NO_3,NH_4Cl and(NH_4)_2TiF_6).The obtained hierarchical ts-1 catalysts were characterized by many techniques and tested for propylene epoxidation using hydrogen peroxide as an oxidant in a fixed-bed *** was shown that the physicochemical and catalytic properties of the treated ts-1/sio_2 extrudate depended on the types of ammonium salts *** to the treatment with TPAOH alone,the treatment with a mixed solution of TPAOH and some ammonium salts can greatly improve the catalytic properties of the treated ts-1/sio_2 *** of these ammonium salts were favorable for the incorporation of titanium in the framework,and the beneficial effect depended on the types of ammonium ***-1/sio_2 extrudate treated with a mixed solution of TPAOH and(NH_4)_3PO_4 exhibited the highest catalyst stability in propylene *** catalytic property can be correlated to high crystallinity,more framework titanium,large specific surface area and large external surface area.

关键词： Ammonium salt Post-treatment Catalyst stability ts-1/sio2 extrudate Epoxidation

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钛硅催化剂的酸碱改性处理

大连理工大学学报 2002年第1期42卷 42-46页

作者：闫海生刘靖王祥生大连理工大学精细化工国家重点实验室辽宁大连116012

在甲醇 -水体系中进行丙烯环氧化反应时 ,丙烯与双氧水在骨架钛上生成环氧丙烷 .ts-1中含有的微量酸中心能够导致环氧丙烷与溶剂反应生成丙二醇、1 -甲氧基 -2 -丙醇和 2 -甲氧基 -1 -丙醇 ;还能促进双氧水的分解 ,降低双氧水的有效利用... 详细信息

在甲醇 -水体系中进行丙烯环氧化反应时 ,丙烯与双氧水在骨架钛上生成环氧丙烷 .ts-1中含有的微量酸中心能够导致环氧丙烷与溶剂反应生成丙二醇、1 -甲氧基 -2 -丙醇和 2 -甲氧基 -1 -丙醇 ;还能促进双氧水的分解 ,降低双氧水的有效利用率 .这种酸中心主要来自于ts-1中硅羟基、配位不饱和的 Ti4+产生的 L酸中心与微量铝产生的 B酸中心 .考察了 ts-1催化的丙烯与双氧水环氧化过程中的酸碱效应 ,以及微量添加物的作用 .结果表明 :添加微量钠盐 ( Na2 CO3 或 Na2 SO4)或 NH4OH可以明显提高环氧丙烷选择性 .采用氨水作为微量添加物能够明显提高催化剂的稳定性 .酸处理无法脱除催化剂中微量铝 ,反而引入了部分酸中心。

关键词：丙烯环氧化反应 ts-1/sio2 酸碱效应添加物钛硅催化剂环氧丙烷酸碱改性

Effects of the Water in Mixed Solvent on the Epoxidation Reaction of Propylene with ts-1 Catalyst

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Journal of Donghua University(English Edition) 2001年第4期18卷 70-73页

作者：苏泉声王彪张玉梅王华平 Chemical Fiber Engineering Research Center Dong Hua University Shanghai 200051

The epoxidation reaction of propylene and hydrogen peroxide with zeolite catalyst containing titaniumsilicalite (ts-1)has been studied, and the reaction in the mixed solvent of water/methanol has been discussed. It is shown that the selective of epoxidation propylene decreases while the selective of propylene glycol increases, when the water content increases in the mixed solvent of methanol/water.

关键词： titanium-silicalite ts-1/sio2 epoxidation reaction methanol/water mixed solvent

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钛硅分子筛后处理及催化丙烯环氧化性能研究

钛硅分子筛后处理及催化丙烯环氧化性能研究

作者：韩鑫鹏天津大学

学位级别：硕士

环氧丙烷(PO)是重要化工中间体,基于氯醇法和共氧化法的PO生产工艺不能满足当今社会可持续发展的基本要求。钛硅分子筛(ts-1)催化丙烯环氧化生产PO(HPPO)的方法具有产物选择性高,工艺简单,环保等优点,引起各国企业及学术界的广泛关注。... 详细信息

环氧丙烷(PO)是重要化工中间体,基于氯醇法和共氧化法的PO生产工艺不能满足当今社会可持续发展的基本要求。钛硅分子筛(ts-1)催化丙烯环氧化生产PO(HPPO)的方法具有产物选择性高,工艺简单,环保等优点,引起各国企业及学术界的广泛关注。尽管HPPO法已成功实现工业化,但进一步提高ts-1使用寿命可显著减少PO生产成本。本论文工作采用混合碱对ts-1成型物进行处理,以期提高其使用寿命。首先,用四丙基氢氧化铵(TPAOH)/NH?HO混合碱处理ts-1成型物并研究了不同NH?HO浓度对ts-1物理化学性质和催化丙烯环氧化反应性能的影响。结果表明,用TPAOH-NH?HO混合碱处理ts-1,催化剂稳定性明显提高;随处理液中NH?HO浓度提高,催化剂介孔体积,比表面积和外表面积明显上升。但NH?HO浓度高到0.09 mol?L,ts-1晶粒出现明显刻蚀痕迹,骨架钛含量减少,催化剂稳定性明显降低。TPAOH/NH?HO溶液处理ts-1的最佳条件:TPAOH浓度为0.06 mol?L,NH?HO浓度为0.03 mol?L。其次,研究了TPAOH和不同铵盐((NH)PO,(NH)SO,NHCHCH,NHCl,NHF,(NH)CO,NHNO和(NH)TiF)混合物处理对ts-1物化性质和催化丙烯环氧化反应性能的影响。结果表明,TPAOH-不同铵盐(NHF和(NH)TiF除外)混合物处理能在保持原有骨架钛含量的同时降低再结晶过程中非骨架钛物种产生,从而提高催化剂稳定性。其中采用TPAOH和(NH)PO混合物处理的催化剂表现出低的非骨架钛含量,最高的骨架钛含量以及最高的催化剂稳定性(30 h)。催化剂稳定性的提高可能是由于后处理过程中铵盐延缓了ts-1再结晶过程,使处理液中钛置入骨架速率和再结晶速率较好匹配,降低了非骨架钛的产生。因此,在水热后处理中,适量添加铵盐对制备高性能ts-1催化剂至关重要。

关键词： ts-1/sio2 丙烯环氧化四丙基氢氧化铵铵盐氨水