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Study on Crystallization of Titanium Silicalite(Ⅰ)

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China Petroleum Processing & Petrochemical Technology 2008年第4期10卷 19-24页

作者： Lin Min Zhu Bin shu xingtian Wang Xieqing Research Institute of Petroleum Processing Beijing 100083

In order to investigate the rules on preparation of titanium silicalite （TS-1） the ^1H →^13C CP/ MAS NMR spectrometers were applied to track the function of template TPAOH in the process of crystallization of titanium silicalite. The research results revealed that at the initial stage of crystallization the TPA＋ ions acting as the template could predominantly absorb the polymers of negatively charged silicatitania sol and the interactions between silica sol and titania sol could gradually lead to the formation of tiny crystal nuclei that could slowly grow up to form molecular sieves. Upon investigating the course of crystallization of titanium silicalite the ^1H →^13C CP/MAS NMR spectrometers were applied to effectively enhance the resolution of 29Si signals in the titanium silicalite. Study results have shown that during the formation of tiny crystal nuclei upon interaction between titania sol and silica sol the influence of titania sol on the silica sol was insignificant. However, when tiny crystal nuclei broke out into molecular sieves the titania sol could enter the zeolite framework that could apparently impose an enhanced effect on the silica sol.

关键词： titanium silicalite TS-1 hollow titanium silicalite(HTS) crystallization characterization nuclear magnetic resonance

Synthesis of Nanosized SSZ-13 Zeolite and Performance of Its Mixed Matrix Membrane for CO2/CH4 Separation

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China Petroleum Processing & Petrochemical Technology 2019年第2期21卷 19-26页

作者： Liu Jianqiang Luo Yibin Li Minggang shu xingtian SINOPEC Research Institute of Petroleum Processing

Nanosized SSZ-13 zeolite was synthesized by traditional hydrothermal method using N,N,N-trimethyl-1-adamantanaminium hydroxide as the structure-directing agent (SDA). The influence of different preparative conditions of nanosized SSZ-13 was investigated systematically. The synthetic zeolites were characterized by X-ray powder diffraction (XRD), nitrogen physisorption, and scanning electron microscopy (SEM). By means of the self-assembled method, the thin SSZ-13/polyvinyl alcohol nanocomposite membranes were obtained by incorporating the nanosized SSZ-13 zeolite into the polymeric precursor (polyvinyl alcohol (PVA)). The permeation properties of pure CO2 and CH4 through the mixed matrix membranes (MMMs) were measured. The results showed that the highly crystalline SSZ-13 zeolite in a dispersed nanocrystal form with a controllable particle size of 100 nm could be hydrothermally synthesized by optimizing the synthetic parameters and the selectivity of CO2/CH4 of the MMMs could reach a value of 40 by changing the amount of nanosized SSZ-13 zeolite.

关键词： nanosized SSZ-13 polyvinyl alcohol permeation

Study on the Mechanisms for Baeyer-Villiger Oxidation of Cyclohexanone with Hydrogen Peroxide in Different Systems

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China Petroleum Processing & Petrochemical Technology 2012年第2期14卷 7-17页

作者： Xia Changjiu Lin Min Zhu Bin shu xingtian State Key Laboratory of Catalytic Material and Reaction Engineering Research Institute of Petroleum ProcessingSINOPECBeijing 100083

The green and effective Baeyer-Villiger oxidation reaction of cyclohexanone for preparing e-caprolactone is of particular importance in the synthesis of new polymer materials. We have discussed here several mechanism types of Baeyer-Villiger oxidation of cyclohexanone with H2O2 in different reaction systems. Five main types have been addressed, i. e.：（1） the non-catalyzed reaction type, where the C=O of ketones is activated by H＋, which is electrolytically dissociated from H202 and H20, to improve the capability of C=O group for accepting the electron pairs; （2） the thermally activated radical reaction type, where the Criegee intermediate is produced via two steps of radical reaction with -OH attack, with much more hydroxyl radicals being excited in the presence of TS-1 zeolite; （3） the Bronsted acid catalysis reaction type, where both O-O moiety and C=O group could be activated by BriSnsted acid; （4） the solid Lewis acid catalyzed C=O of the substrate activation reaction type through enhancing the donor-acceptor interaction between the antibonding π＊c-o orbital of cyclohexanone and HOMO of Sn-containing zeolites; and （5） the solid Lewis acid catalyzed H202 to form Me-OOH oxidative species by converting the highest occupied molecular orbital （HOMO） of Ti-OOH into a singly occupied molecular orbital （SOMO）, making the O--O group highly electrophilic to attack the C--O of cyclohexanone during the Baeyer-Villiger oxidation process. In the end, we have also compared the different mechanisms and put forward our opinions on the development direction of catalytic materials aiming at eco-friendly Baeyer-Villiger oxidation of cyclohexanone in the years to come.

关键词： reaction mechanism Baeyer-Villiger oxidation Lewis acid Br'6nsted acid thermally activated radical hydrogen peroxide

Synthesis and Characterization of Hollow Titanium Silicalite Zeolite(HTS)

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China Petroleum Processing & Petrochemical Technology 2008年第3期10卷 1-5页

作者： Lin Min Zhu Bin shu xingtian Wang Xieqing Research Institute of Petroleum Processing SINOPEC Beijing 100083 China

29Si-NMR and 1H-NMR were used to follow up the basic hydrolysis of tetraethyl orthosilicate （TOES） and the results showed that species of monomer, dimer, trimer, cyclic and polymer silicates were formed. The monomer and dimer were favorable for the high activity of zeolite. XRD, 13C CP/MAS and 29Si NMR were used to trace the crystallization process of hollow titanium silicalite zeolites （HTS）. The results showed that the induction period of HTS was 80 min, and subsequently it took next 10 min to form HTS and the remaining time of the crystallization period might function for cleaning up the pores and/or washing off the impurities from the HTS zeolite. The catalytic oxidation performance of HTS zeolite is different from that of the acid activity of zeolite in which the conventional definition of crystallinity does not reflect the catalytic oxidation activity proportionally. The synthesized HTS samples were character- ized by XRD, FT-IR, UV-Vis and Raman spectra. It was confirmed that Ti was incorporated into the zeolite framework. The synthesized HTS samples revealed good repeatability and high activity for oxidation of phenol into diphenol.

关键词： titanium silicate zeolite HTS synthesis characterization oxidation

A “Green” Cyclohexanone Oxidation Route Catalyzed by Hollow Titanium Silicate Zeolite for Preparing ε-Caprolactone,6-Hydroxyhexanoic Acid and Adipic Acid

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China Petroleum Processing & Petrochemical Technology 2012年第4期14卷 33-41页

作者： Xia Changjiu Zhu Bin Lin Min shu xingtian State Key Laboratory of Catalytic Material and Reaction Engineering Research Institute of Petroleum ProcessingSINOPEC

Hollow titanium silicalite （HTS） molecular sieve has been synthesized, and information on its structure, physico- chemical characterization, as well as surface property was investigated by a host of analytical methods, such as XRF, XRD, low-temperature N2 adsorption/desorption, TEM, FT-IR, UV-Vis, 29Si MAS NIVIR, and XPS techniques. The characterization results suggest that HTS zeolite has a special hollow crystal structure and its mesopore volume is larger than that of TS-1 zeolite. The titanium species in this zeolite are composed of the framework tetrahedral Ti （IV） ions and extra-framework octahedral Ti （IV） ions, which tend to disperse into its bulk phase. This zeolite material also has been applied to catalyze the cyclohexanone oxidation process, and the products are not completely consistent with those results obtained by using TS-1 zeolite, which might be caused by their difference in pore structure and pore volume, especially the mesopore volume. Cy- clohexanone oxidation catalyzed by HTS zeolite is a representative consecutive reaction, the main target products of which are e-caprolactone, 6-hydroxyhexanoic acid and adipic acid. The effect of H202/cyclohexanone mole ratio on the cyclohexa- none conversion, the total target product selectivity, the distribution of three target products selectivity and their variations along with reaction time is also researched and analyzed, which indicate that HTS zeolite shows a high performance for the Baeyer-Villiger reaction of cyclohexanone and catalytic oxidation of 6-hydroxyhexanoic acid under mild conditions, and the quantity of active surface titanium species as well as the pore structure and mesopore volume controlling the mass diffusion rate are the key factors determining the catalytic activity of HTS zeolite and product selectivity.

关键词： catalytic oxidation cyclohexanone HTS zeolite Baeyer-Villiger reaction consecutive reaction

The Function of β Zeolite for Enhancing the Propylene Yield in FCC Process

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China Petroleum Processing & Petrochemical Technology 2017年第4期19卷 6-10页

作者： Ouyang Ying Luo Yibin shu xingtian SINOPEC Research Institute of Petroleum Processing Beijing 100083

The ultra-stable Y zeolite, modified β zeolite, and modified ZSM-5 zeolite were characterized by NH3-TPD analysis. The results showed that the acidic substance of modified β zeolite is between that of the Y zeolite and the ZSM-5 zeolite. These three kinds of zeolites were evaluated by using hexane, decane and light diesel serving as feedstocks with different molecular size. The results showed that these three kinds of zeolites had different cracking capability and product distribution obtained for cracking hydrocarbons with different molecular sizes as a result of the difference in pore structure and acidic substances. The modified β zeolite can produce much more C_5~= —C_8~= olefins, which are excellent precursors of propylene. Then the mixed samples of these three kinds of zeolites were tested in the VGO microreactor unit, and the test results showed that the modified β zeolite played a ‘relay role' between the ultra-stable Y zeolite and the modified ZSM-5 zeolite, so that the composite made of the ultra-stable Y zeolite, the modified β zeolite, and the modified ZSM-5 zeolite showed a highest propylene yield and selectivity.

关键词： fluid catalytic cracking β zeolite propylene

MMC——High Propylene Selectivity DCC Catalyst

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China Petroleum Processing & Petrochemical Technology 2007年第1期9卷 13-18页

作者： Li Zheng Xie Chaogang Luo Yibin Zhao Liuzhou shu xingtian SINOPEC Research Institute of Petroleum Processing Beijing 100083

RIPP has developed the third generation novel DCC catalysts aimed at increasing the propylene yield, named as the MMC series catalysts. This catalyst is of the MFI structure composed of the ZSP zeolite as the main active component, which has higher capability for producing low-carbon olefins, in particular the propylene. The commercial application of this catalyst at SINOPEC Anqing Petrochemical Company has revealed that the adoption of the MMC-2 catalyst has resulted in a 1.6-4.0 percentages increase in propylene yield under basically similar conditions in terms of the feedstock property and process operating regime coupled with reduction in gasoline olefin COntent and increase in aromatic content to improve the gasoline quality.

关键词： deep catalytic cracking catalyst metallic components propylene low-carbon olefins

Research on Bipolar Membrane Electrodialysis for Ion Exchange of Molecular Sieves

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China Petroleum Processing & Petrochemical Technology 2018年第2期20卷 1-5页

作者： Chen Beiyan Liu Zhongqing Zhou Lina Luo Yibin shu xingtian SINOPEC Science&Technology Department Beijing 100728 SINOPEC Research Institute of Petroleum Processing Beijing 100083

In view of the problems associated with large amount of discharged wastewater and serious pollution in the existing technology for removing sodium species from molecular sieves,this research work introduces the bipolar membrane electrodialysis into the process of removing sodium species from molecular sieves,and proposes a novel method of cleanly removing sodium from molecular *** results show that the technology for removing sodium ions from the molecular sieves with an indirect electrodialysis process is feasible,and can recover Na OH *** bipolar membrane electrodialysis is especially suitable for treating the USY,ZSM-5 and Beta molecular sieves with high acid-resistance,and the physicochemical properties and catalytic performance of the prepared molecular sieves are roughly equivalent to those of the ammonium ion-exchange *** comparison with the ammonium ion-exchange method,the process is clean and environmentally friendly,which consumes less water,and does not discharge wastewater to exhibit a rosy prospect of industrial application.

关键词： molecular sieve ionexchange bipolarmembrane electrodialysis

Investigation on Organic Solvent Free Toluene Oxidative Bromination Reaction Catalyzed by HTS Zeolite

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China Petroleum Processing & Petrochemical Technology 2020年第4期22卷 1-9页

作者： Peng Xinxin Xia Changjiu Lin Min Zhu Bin Luo Yibin shu xingtian State Key Laboratory of Catalytic Materials and Reaction Engineering SINOPEC Research Institute of Petroleum ProcessingBeijing 100083

The toluene oxidative bromination reaction catalyzed by hollow titanium silicalite(HTS)zeolite in aqueous medium was investigated by employing H2O2 and HBr under mild conditions without the need for organic solvent.A high toluene conversion(90.7%)and high selectivity of mono-bromotoluene(99.0%)was achieved under the optimal reaction *** UV-Raman spectroscopy was applied for the mechanism study and the result reveals that HTS is efficient for catalyzing the oxidation reaction of HBr with H2O2 to produce abundant active bromine species,which can further facilitate the toluene electrophilic bromination reaction.A two-step toluene bromination reaction mechanism involving the HTS catalyzed active bromine species“generation-conversion-utilization”process is proposed based on the UV-Raman spectroscopy analysis.

关键词： titanium silicalite oxidative bromination organic solvent free H2O2/HBr polybromine ion