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Preparation, Characterization of Solid Superacid and Its Application in Resin Deep Processing

Author: ChenShaoFeng
Tutor: GuoHaiFu
School: Inner Mongolia University of Technology
Course: Applied Chemistry
Keywords: Solid Superacid Preparation Characterization Metal ion Hydration reaction
CLC: TQ351.4
Type: Master's thesis
Year: 2009
Downloads: 119
Quote: 0
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Abstract


I acid catalyst plays an extremely important role in the modern chemical industry, and is widely used in many important chemical reactions in the catalyst is also part of the current environmental pollution, the research and development of new environmentally friendly catalyst to improve the current environmental pollution One of the effective way. SO42-/MxOy type solid super acid catalyst, because of its acid-catalyzed reactions can be activated in the milder conditions with simple preparation, high catalytic activity, high selectivity, fewer side effects, non-corrosive, non-\renewable reuse, and quickly became a research focus in the field of catalysts, and instead of the traditional acid catalysts are widely used in organic reactions. In this paper, the the hole track transition metal (Fe, Co, Ni) of tin dioxide matrix solid superacid improve the synthesis of a series of catalysts by FT IR, XRD, TG-DTA, XPS and BET means of characterization; catalyst and synthesis of Ni / SO the 4 / sub> the 2 - / SnO 2 applied to the hydration of α-pinene, to examine the hydration reaction conditions. Through experiments and research to get the following results: (1) preparation of the catalyst Ni / the SO 4 2 - / the SnO 2 to acetic acid n-butyl synthesis reaction as a probe reaction, the orthogonal experiment analyzes the optimal conditions of preparation of the catalyst activity: calcination temperature of 500 ° C, the nickel ion concentration of 0.5 mol / L, the roasting time of 2 h; in which the calcination temperature of the catalyst The catalytic activity of the greatest impact. (2) The means of FT IR, XRD, TG-DTA, XPS analysis of Ni / SO the 4 / sub> the 2 - / the SnO 2 solid super Characterization strong acid acid center structure, crystalline form, the size of the sulfur, the elemental form, and other physical characteristics. The results show that: Ni / SO 4 2 - / SnO 2 the solid superacid acid center model active ingredient sulfate sequestration and the bridge two coordination modes and metal combined to form the the superacid structure; closely related to the structure of the nickel ion concentration and calcination temperature, and the introduction of some nickel ions can superacid structural reinforcement, when certain calcination temperature is reached, the disappeared by the structure with the decomposition of the sulfate, catalyst surface mainly showing the tetragonal tin dioxide, with the raise of the activation temperature, the crystal structure is becoming full, nickel added with stable SO42-role, its loss becomes was more difficult; S in the presence of a valence of S (6) constituting the active ingredient. (3) Ni / SO 4 2 - / SnO 2 deactivation mechanism for discussion, the results show that for n-butyl acetate synthesis The esterification reaction catalyst deactivation mainly due to the catalyst surface area carbons and SO42-loss of activity can be restored by re-dipped in acid after roasting. (4) The preparation of the catalyst Ni / SO the 4 the 2 - / SnO the 2 for the hydration reaction of α-pinene by GC- MS product detection, and discusses the factors that affect the hydration reaction has been catalyzed α-pinene hydration reaction of synthesis of α-terpineol optimal conditions were as follows: n-(alpha-pinene): n (monochloroacetic acid): n (H2O) = 1:1:2, the reaction system temperature of 70 ° C, the reaction time of 10 h, the amount of catalyst for α-pinene quality 6%; α-pinene conversion rate of 100% α-terpineol the selectivity was 73.3%; with the unmodified catalyst of SO 4 2 - / SnO 2 compared, the catalyst showed a better The catalytic activity and selectivity. (5) by precipitation - impregnated two-step method to prepare the catalyst Co. / SO the 4 / sub> the 2 - / SnO 2 and Fe / SO 4 2 - / SnO 2 , applied to n-butyl acetate synthesis reaction, catalyst preparation conditions investigated by single factor experiment; and FT IR, XRD and TG-DTA analysis techniques to characterize the catalyst. (6) The experiments show that: Ni 2 the Co. 2 and Fe 3 can be a good modified SO 4 2 - / SnO 2 catalyst, improving the catalytic activity of the esterification reaction, Catalyst n-butyl acetate esterification reactive in descending order of: Ni / SO 4 2 - / SnO 2 gt; Fe / SO 4 2 - / SnO 2 gt; Co / SO 4 2 - / SnO 2 gt; SO 4 2 - / SnO 2 . Ni2 the modified SO 4 2 - / the SnO 2 catalyst thermal stability higher thermal stability than Co2 and Fe3 modified catalyst metal ion modified catalyst active component SO42-content descending order: Ni / SO 4 2 - / the SnO 2 gt; Fe / SO 4 2 - / SnO 2 gt; Co / SO 4 2 - / SnO 2 gt; SO 4 2 - / SnO 2 , with esterified rate results consistent.

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CLC: > Industrial Technology > Chemical Industry > Fiber quality of the chemical processing industry > Wood chemical processing industry > Resin Industry
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