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Layered catalyst for selectively oxidizing 4-methylguaiacol-to-vanillin, and preparation method thereof

A technology of methyl guaiacol and layered catalyst is applied in the preparation of organic compounds, catalysts for physical/chemical processes, catalysts for organic compounds/hydrides/coordination complexes, etc. The catalyst and the product are difficult to separate and other problems, to achieve the effect of easy separation and purification, strong industrial application value and low price

Active Publication Date: 2014-11-26
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the synthesis of vanillin by 4-methylguaiacol is mainly based on homogeneous catalysis, but in practical applications, homogeneous catalysts have the disadvantages that it is difficult to separate the catalyst from the product and the catalyst is difficult to recycle.

Method used

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  • Layered catalyst for selectively oxidizing 4-methylguaiacol-to-vanillin, and preparation method thereof
  • Layered catalyst for selectively oxidizing 4-methylguaiacol-to-vanillin, and preparation method thereof
  • Layered catalyst for selectively oxidizing 4-methylguaiacol-to-vanillin, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Cobalt-nickel-aluminum layered hydrotalcite catalysts intercalated with carbonate (Co-Ni-Al-CO 3 2- What the preparation of -LDHs) adopts is dynamic urea method, and its preparation method is: first, accurately weigh reactant Co(NO 3 ) 2 ·6H 2 O, Ni(NO 3 ) 2 ·6H 2 O,Al(NO 3 ) 3 9H 2 O and (NH 2 ) 2 CO was added to 700mL of deionized water in turn, so that the Co(NO 3 ) 2 ·6H 2 The concentration of O is 0.5mol / L, Ni(NO 3 ) 2 ·6H 2 The concentration of O is 0.5mol / L, Al(NO 3 ) 3 9H 2 The concentration of O is 0.5mol / L, (NH 2 ) 2 The concentration of CO is 0.2 mol / L. Stir to fully dissolve various reactants in deionized water, and heat and stir in an oil bath at 130°C for 48 hours; then, the obtained cobalt-nickel-aluminum layered water Talc Co-Ni-Al-CO 3 2- -LDHs are first filtered and washed with deionized water, and then washed with absolute ethanol, after repeated operations and washings; finally, the cobalt-nickel-aluminum layered hydrotalcite c...

Embodiment 2

[0036] The preparation method of dodecylsulfonate intercalated cobalt-nickel-iron intercalated hydrotalcite catalysts (Co-Ni-Fe-DS-LDHs): first, the precursor carbonate-intercalated cobalt-nickel-iron layered hydrotalcites were synthesized by dynamic urea method. Talc catalyst (Co-Ni-Fe-CO 3 2- -LDHs), followed by the synthesis of dodecylsulfonate intercalated hydrotalcite catalysts (Co-Ni-Fe-DS-LDHs) using an ion-exchange method.

[0037] (A) Carbonate-intercalated cobalt-nickel-iron layered hydrotalcite catalyst (Co-Ni-Fe-CO 3 2- -LDHs) preparation

[0038] First, accurately weigh the reactants Co(NO 3 ) 2 ·6H 2 O, Ni(NO 3 ) 2 ·6H 2 O, Fe(NO 3 ) 3 9H 2 O, NH 4 F and (NH 2 ) 2 CO was sequentially added to 120mL of deionized water for reaction, so that the Co(NO 3 ) 2 ·6H 2 The concentration of O is 0.08mol / L, Ni(NO 3 ) 2 ·6H 2 The concentration of O is 0.03mol / L, Fe(NO 3 ) 3 9H 2 The concentration of O is 0.04mol / L, NH 4 The concentration of F is 0.02...

Embodiment 3

[0043] Preparation method of cobalt-nickel-iron-iron-samarium intercalated hydrotalcite catalyst (Co-Ni-Fe-Sm-DS-LDHs) intercalated with dodecylsulfonate: first, the precursor carbonate-intercalated cobalt-nickel-iron was synthesized by dynamic urea method Samarium layered hydrotalcite catalyst (Co-Ni-Fe-Sm-CO 3 2--LDHs), followed by the synthesis of dodecylsulfonate-intercalated cobalt-nickel-iron-samarium hydrotalcite catalysts (Co-Ni-Fe-Sm-DS-LDHs) using an ion-exchange method.

[0044] (A) Cobalt nickel iron samarium layered hydrotalcite catalyst intercalated with carbonate (Co-Ni-Fe-Sm-CO 3 2- -LDHs) preparation

[0045] First, accurately weigh the reactants Co(NO 3 ) 2 ·6H 2 O, Ni(NO 3 ) 2 ·6H 2 O, Fe(NO 3 ) 3 9H 2 O, Sm(NO 3 ) 3 ·6H 2 O, NH 4 F and (NH 2 ) 2 CO was sequentially added to 120mL of deionized water for reaction, so that the Co(NO 3 ) 2 ·6H 2 The concentration of O is 0.08mol / L, Ni(NO 3 ) 2 ·6H 2 The concentration of O is 0.03mol / L, F...

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Abstract

The invention relates to a layered catalyst for selectively oxidizing 4-methylguaiacol-to-vanillin, and a preparation method thereof, and belongs to the technical field of catalysts. A coactive site is added to change the electronic structure of a main catalytic active site Co; and anions with different selective dear anion effect by inserting different hydrophilic and hydrophobic properties are inserted into an interlayer in order to influence the selectivity on products. One or more of magnesium, zinc, copper, aluminum, iron, nickel, manganese, titanium, samarium, calcium, cerium and chromium, gallium, indium, tin and other elements is / are added as a coactive component. The preparation method comprises the following steps: preparing a solution by using nitrates or chlorides of active components and the coactive component(s), adding a precipitating agent, carrying out a heating reaction, washing a solid substance, and drying; adding the prepared layered hydrotalciteinto a solution containing anions to be exchanged, and carrying out an ion exchange process to obtain the intercalated hydrotalcite catalyst. The prepared catalyst can be applied to the oxidation reaction of 4-methylguaiacol. The catalyst has high activity and has high selectivity to vanillin.

Description

technical field [0001] The invention belongs to the technical field of catalysts and provides a heterogeneous catalyst for selectively catalytically oxidizing 4-methylguaiacol to generate vanillin and a preparation method thereof. Background technique [0002] Vanillin (3-hydroxy-4-methoxybenzaldehyde) has a very wide range of uses in human production and life, such as food additives and pharmaceutical intermediates. In recent years, the demand for vanillin has been increasing, and the synthesis method of vanillin has attracted more and more attention from researchers. As the production of natural vanillin produced by biosynthesis can no longer meet the growing demand of human beings, chemical synthesis of vanillin has gradually become a research hotspot. [0003] Industrially, there are two main synthesis methods of vanillin: one is the lignin method; the other is the guaiacol method, and the guaiacol method mainly includes the nitroso method and the glyoxylic acid method....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/232B01J31/26B01J27/25C07C47/58C07C45/36
Inventor 何静高俊芳安哲
Owner BEIJING UNIV OF CHEM TECH
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