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Research on the Separation of Biphenylcarboxylic Acid Isomers

Author: YangCaiXia
Tutor: ZhangWeiJiang
School: Tianjin University
Course: Chemical Engineering
Keywords: beta - cyclodextrin Associated acid Inclusion separation
CLC: TQ245.12
Type: Master's thesis
Year: 2009
Downloads: 22
Quote: 0
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Abstract


Shijiazhuang Refining \u0026 Chemical Company toluene production of acid unit will generate a large number of 3 - United benzoic acid and 4 - United benzoic acid mixture, both have a higher value in organic synthesis, petrochemical, materials chemistry. Especially 4 - the benzoic acid, can be used as polarographic analysis reagents and organic synthesis intermediates, with considerable economic value. However, the United benzoic acid in a mixture limited value, and a large number of their emissions will give the environment a lot of pressure. The purpose of this paper is to explore a reasonable and feasible way to achieve the 3 - associated acid and 4 - United benzoic acid separation and purification. The first 3 - associated acid and 4 - United benzoic acid nature of differences, a series of commonly used modern separation methods to filter mainly explore the feasibility of a reaction separation and inclusion separation. The study showed that: Poor feasibility of reactive separation method, the introduction of the reactants is not only reacts with 4 - associated acid, but also multi-position substituted with 3 - associated reaction benzoate, carboxylation reaction system more complex to be separated, the separation more difficult; beta-cyclodextrin inclusion separation-linked benzoic acid isomers effect, can be successful - United benzoic acid separated from the United benzoic acid mixture. View of the selective beta-cyclodextrin - United benzoic acid inclusion of the papers on the separation conditions emphasis on the heating temperature, mixing time, inclusion time, the ratio of raw materials on the separation results impact, and finally determine the stirring time was 2h30min, the heating temperature is controlled at 60 ~ 70 ° C when more appropriate. Subsequently, through orthogonal experiment was designed to establish the separation of the main factors: the ratio of beta-cyclodextrin materials and associated benzoic acid, and select the best separation conditions: When the beta-cyclodextrin and associated benzoic acid raw materials the molar ratio of materials to 1:2, the heating temperature of 60 ° C, stirring time is 2h30min inclusion 2days, separation, 4 - linked benzoic acid yield up to 35.47%, and the purity of up to 99% above. DSC differential scanning calorimetry, IR spectrometry, 1H NMR method for the inclusion of separating the resulting products and their Inclusion Complexes characterization confirmed that the resulting product is 4 - linked benzoic acid, also proves that generated in the process of inclusion 4 - Stock benzoic acid and beta-cyclodextrin inclusion thereof. In addition, the use of UV-Vis spectrometry analysis of beta-cyclodextrin with the United benzoic acid inclusion process, the results showed that: beta-cyclodextrin the different associated benzoic package knot priority selective separation conditions, so the determination is the key to successful implementation of inclusion separation.

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CLC: > Industrial Technology > Chemical Industry > Basic Organic Chemistry Industry > The production of aromatic compounds > Aromatic carboxylic acids and their derivatives > Aromatic acid > Benzene series acid
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