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A Study on Novel Synthesis Methods for New Titanium-containing Molecular Sieves and Their Catalytic Properties

Author: LiuYueMing
Tutor: HeMingYuan；WuPeng；ZhaoDongYuan
School: East China Normal University
Course: Physical and chemical
Keywords: Titanium-containing molecular sieve Synthesis Green catalytic materials Microporous molecular sieves Mesoporous molecular sieves Liquid phase selective oxidation
CLC: O643.3
Type: PhD thesis
Year: 2005
Downloads: 817
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Abstract


The oxygen-containing organic compounds is very important intermediate petrochemical and fine chemical industry, however, its preparation process urgently needed improvement of green, environmentally friendly green chemistry and chemical processes to replace the environmental load and energy consumption of non-catalytic, and measurement of chemical reaction process. Titanium-containing molecular sieve, as the excellent hydrocarbon selective oxidation catalytic materials, has been a concern for the catalytic materials researchers study object. However, stable performance and high activity of TS-1 zeolite prepared difficulties and molecular sieve expensive seriously hampered the further industrial application of TS-1 zeolite;, TS-1 molecular sieve Macromolecular Reaction due to the constraints of the pore size can not meet the requirements of . In view of this, the subject first to the TS-1 study, and solve their problems in industrial applications; then, to meet the the macromolecular reaction requires the main line, a new molecular sieve, the relationship between the new synthetic methods and molecular sieve structure and catalytic properties The research, development, structural stability, high activity, high selectivity of the catalytic oxidation of molecular sieve material. The main contents include: the first part, first of all, for the catalytic properties stable TS-1 zeolite the difficult industrial production problems in fully understanding the impact of TS-1 zeolite catalytic performance factors based on the optimization of industrial production process conditions to achieve a stable catalytic performance TS-1 zeolite industrial scale production. TS-1 zeolite in the industrial products, the successful application of cyclohexanone oxime ammonia process 70,000 tons / year. Second, the TS-1 zeolite with a high production cost for the current problem, developed the hydrolyzed into gum concentration conditions in the lower base (OH - ), and higher templating agent (the TPA ) concentrations launching new thermal crystallization method, industrial tests showed that the TS-1 zeolite improve production efficiency from 18Kg / (m 3 · d), under the premise of maintaining catalytic activity quite to 70 Kg / (m 3 · d), and effectively reducing the production costs. Third, in order to further enhance the catalytic activity of TS-1 zeolite, for the after-treatment of pickling modified found that the modified TS-1 molecular sieve of the phenol hydroxylation activity was significantly increased, the reaction conditions of: phenol / H 2 O 2 molar ratio is 3, TS-1 / phenol weight ratio of 0.05, and the phenol / acetone weight ratio 1.25,80 ° C for 6h, conditions, the conversion of phenol rate of 39.2%, the the hydroquinone selectivity of 99.2%. Finally, a preliminary exploration of the TS-1 synthetic inorganic raw materials found to Ti (SO 4 ) 2 Ti source, solid silica gel as a silicon source, through the pre- calcining a mixture of both, the better catalytic performance of the low cost of production can be synthesized TS-1 molecular sieve. The second part, in order to get a new stable cell structure TAPO-11 zeolite SAPO-11 molecular sieve as a research model, detailed examination of the sol-gel process, its cell structure stability, and from the molecular sieve microstructure explain why. At the same time, in order to the nC 8 ° as a probe molecule to study different unit cell structure of the catalytic performance of SAPO molecular sieve 11, to establish the relationship between the molecular sieve pore structure and reactivity. Second, the optimal synthesis conditions, found, can be well controlled by simple control crystallization temperature TAPO n a molecular sieve unit cell structure stability, and get a new cell structure stability TAPO 11 molecular sieves. Finally, different transition metal-containing the AEL structure of zeolite synthesis preliminary exploration, such as C. The wonderful O 11, M recognized PO 11 FAPO a 11, NAPO a 11 zeolite. The third part of the novel Chin Chin-containing MWW structure of zeolite as the object of study, the development of new synthetic methods and novel Chin zeolite microporous and mesoporous double catalytic characteristics in order to be suitable for Macromolecular Reaction molecular sieve. First, Adhesive Ti-MWW zeolite synthesis to explore, to reduce the amount of boric acid crystallization auxiliaries. Through Si older than a Si / Ti ratio, Na content, type of the templating agent, different silicon source, etc. conditions of synthesis of the investigated and found that well Ganjiao method can synthesize Ti-MWW zeolite; and hydrothermal synthesis phase than Ganjiao Synthesis, boric acid in an amount of crystallization auxiliaries significantly reduced, si Shinobu molar ratio increased from 0.75 to 12; When the introduction of seed crystals, the amount thereof can also be dynasties lower reach 51 / B molar ratio is 92. Next, using the the layer peeling technical success of Ti-MWW molecular sieve layer peeling novel Chin zeolite: Del Ti-MWW zeolite. Del Ti-MWW molecular sieve zeolite by fully stripped MWW structure of the basic structural unit flakes composed of showing the the dual structural characteristics of microporous and mesoporous molecular sieves. The reaction evaluation showed that, regardless of cyclic olefin or linear olefins, Del-Ti-MWW molecular sieve shows high conversion number (TON), even higher than the Ti-MCM-41. It is by its only maintained the basic structure of the molecular sieve MWW, to both reactants reaction space accessible structural characteristics of the decision. Part IV, to obtain a high quality of mesoporous containing Qin zeolite material target, the \the skeleton structure of the anatase the novel TIOZ mesoporous molecular sieve. At the same time, new ideas introduced the Si Ti-based mesoporous molecular sieves, the successful synthesis of the Ti content can be adjusted new Khin mesoporous molecular sieves. XRD, BET, SEM, TEM, FT-IR, UV-Vis, MAS N MR, ICP characterized by means of detailed characterization of the Chin zeolite, and investigated its physicochemical the intrinsic relationship of nature and catalytic properties, containing Chin design all kinds of new methods and new techniques of molecular sieve. Cold short, the subject response requirements to meet different size molecules containing Chin molecular sieve for the study of the main line, focus on solving problems restricting the TS-1 zeolite industrial applications, the development of new synthetic methods and Novel Chin molecular sieve performance the new stable industrial scale production products TS-1 zeolite stable cell structure TAPO n molecular sieve with a double catalytic characteristics of microporous and mesoporous molecular sieves Chin silicalite Del a Ti-MWW zeolite, anatase skeleton structure of the new TIOZ mesoporous molecular sieve and Chin content of any adjustable chin silicon mesoporous molecular sieves. Development of TS-1 zeolite production costs significantly lower concentration of low-alkali hydrolysis into plastic high template concentration of hydrothermal crystallization process, a significant new technology to improve the post-processing of the TS-1 zeolite catalytic activity modified, and established a crystallization aid The agent amount of boric acid significantly reduced Ti-MWW the molecular sieve Ganjiao Synthesis France. Keyword

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CLC: > Mathematical sciences and chemical > Chemistry > Physical Chemistry ( theoretical chemistry ),chemical physics > Chemical kinetics,catalysis > Catalytic
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