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Preparation, Characterization and Catalytic Performance of Tin-Based Mesoporous Materials

Author: ZhangJiLong
Tutor: LiRuiFeng；FanBinBin
School: Taiyuan University of Technology
Course: Industrial Catalysis
Keywords: Organotin Mesoporous materials Dimethyl carbonate Organosilica Heterogeneous catalyst
CLC: O643.36
Type: Master's thesis
Year: 2007
Downloads: 149
Quote: 2
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Abstract


Reflects the significant catalytic activity of the tin-containing catalyst in the esterification, cyclization, addition and the ester exchange reaction. Of this thesis is to proceed from the reaction and catalyst, for the first time prepared by hydrothermal synthesis out SnMCM-48 mesoporous molecular sieve material characterization and its catalytic performance in phenol hydroxylation. Then focus on organic tin silane [(MeO) to the 2 ) 3 SnCl 3 ] introduced by post-processing grafting and direct hydrothermal synthesis method to mesoporous molecular sieve (SBA-15, MCM-41, MCM-48) the structure and properties of the catalyst prepared in CO 2 and This green chemical reaction of methanol synthesis of dimethyl carbonate (DMC) and its catalytic properties. Designed to enrich the organic tin catalyst, organic tin heterogeneous catalyst is introduced into the mesoporous molecular sieves prepared not only to overcome the defects in the performance of the modified mesoporous molecular sieve homogeneous catalysts are difficult to separate. Including the following: (1) prepared by hydrothermal synthesis of tin-containing mesoporous molecular sieve MCM-48 by XRD and nitrogen adsorption experiments showed that SnMCM-48 has a regular pore structure and high specific surface area. FTIR and UV-vis prove tin into the framework, and with the increased portion of the tin content tin in the pores. Reflects the excellent catalytic activity in phenol hydroxylation reaction. (2) organic tin silane [(MeO) 2 ClSi (CH 2 ) 3 SnCl 3 ] grafted to the pore surface of SBA-15 using methanol and triethylamine treated Mesoporous Composites. By XRD, nitrogen adsorption experiments and TEM characterization of materials, the regular structure of the sample after grafting; 29 Si MAS NMR by FTIR 13 C MAS NMR confirmed that organic tin successfully grafted into the pores on the surface of the SBA-15, and the highest graft amounted 1.05mmol / g. Exhibit high catalytic activity in CO 2 and methanol DMC synthesis reaction, under the conditions of 18MPa, 200 ℃ DMC's molar number (TON) of 3.57, the conversion of methanol was 0.89 % (with the calculated value consistent). The catalytic performance of the catalyst and reaction conditions correlated with the decrease in the content of tin catalyst, the DMC the TON increases. The repeated use of the catalyst experiments show that the stable catalytic performance. (3) [(MeO) 2 ) 3 SnCl 3 ] and n ethyl silicate ester (TEOS) as the silicon source, P123 (EO 20 PO 70 the EO 20 ) as template, using the hydrothermal synthesis were prepared containing organotin SBA-15 mesoporous molecular sieve. XRD results show that with the increase in the content of organotin the molecular sieves orderly reduction. TEM, nitrogen adsorption equilibrium isotherms reveal a very regular pore structure of the sample. FTIR, 29 Si MAS NMR, 13 C MAS NMR confirmed organotin bridging the wall of the hole, while EDS reflects organotin distribution more uniform. CO 2 and methanol DMC synthesis reaction, a TON of the DMC with the decrease in the content of tin is increased, when the tin content of 0.09mmol / g, TON of 18.3. (4) roasting method, solvent extraction, H 2 O 2 oxidation off in addition to the MCM-41 template agent, the effects of the removal of the templating agent MCM-41 structure. MCM-41 are three ways to make orderly and specific surface area were increased, the surface silanols roasting method to reduce condensation, its comparison solvent extraction method and H 2 O 2 oxidation method retains more surface silanols. After removal of the templating agent to the three methods of MCM-41 as a carrier, the preparation of the organic tin functionalized mesoporous molecular sieves. Organotin functionalized MCM-41 prepared after extraction method stripper agent obtained a higher tin content (0.48mmol / g). CO 2 and methanol DMC synthesis reaction, H 2 O 2 organotin functionalized MCM-41 prepared by oxidation stripper plate agent exhibited high catalytic activity, a TON of DMC reached 4.52. (5) after treatment with the same grafting were prepared containing tin MCM-48. Under the same conditions, using different carrier (SBA-15, MCM-41, MCM-48) the grafting amount of the catalyst prepared in a different amount of grafting on the MCM-48 is low, only 0.33mmol / g, grafted high for SBA-15 (1.05mmol / g). In CO 2 and the methanol synthesis DMC's reaction, the same organic under the conditions of tin content, MCM-48 as the carrier of the catalytic activity of the catalyst is low, the TON for DMC was only 2.72, while SBA -15 for the catalytic activity of the catalyst carrier, the DMC a TON 4.56.

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