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Catalyst for synthesizing vanillin by using a glyoxylic acid method and a one-pot method and preparation method thereof

A glyoxylic acid method and a catalyst technology are applied in the preparation of organic compounds, molecular sieve catalysts, carbon-based compounds, etc., which can solve the problem that the catalyst activity needs to be further improved, and achieve the inhibition of the formation of polymerization by-products, the high catalyst activity, and the preparation of The effect of the simple method

Inactive Publication Date: 2011-05-25
TIANJIN VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to simplify the production process of (ethyl) vanillin, improve the production capacity of the equipment and reduce the generation of waste liquid, the inventor proposed a one-pot synthesis of (ethyl) vanillin by the glyoxylic acid method, but the activity of the catalyst used needs to be further improved

Method used

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  • Catalyst for synthesizing vanillin by using a glyoxylic acid method and a one-pot method and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Catalyst preparation: Weigh 7.5g (0.03mol) of reagent copper sulfate and 2.4g (0.01mol) of reagent cobalt sulfate, and dissolve them in 100mL deionized water to prepare a metal salt solution. The rare earth Y-type molecular sieve (Re 2 o 3 ≥17%; SiO 2 / Al 2 o 3 ≥5;Na 2 O≤2%; loss on ignition ≥3%) 100g was added to the above metal salt solution and soaked for 30 minutes, then 5% sodium hydroxide solution was added dropwise to pH 11, the catalyst was separated by vacuum filtration, washed with a small amount of deionized water to remove sodium sulfate Salt, dry at 105°C, oxidize and roast in a high-temperature furnace at 550°C for 60 minutes, and set aside.

[0021] The catalyst is applied to the synthesis of vanillin: a 1000mL four-necked reaction flask equipped with an air distributor, a reflux condenser, a stirrer and three constant pressure dropping funnels is installed on a constant temperature water bath, and the three constant pressure dropping funnels 74.1g ...

Embodiment 2

[0023] Catalyst Preparation: The catalyst was prepared by the method in Example 1.

[0024] Catalyst is applied to the synthesis of ethyl vanillin: add 74.1g (0.4mol) 40% glyoxylic acid, 58.0g (0.42mol) ethyl guaiac respectively in the three constant pressure dropping funnels of embodiment 1 reactor Phenol and 100mL30% liquid caustic soda. Add 500 mL of deionized water and 106.6 g (0.8 mol) of 30% liquid caustic soda into the four-necked reaction flask, and add 5.0 g of the catalyst prepared by the method in Example 1, stir and blow in air, and the air pressure is 0.05 Mpa. After the solution was heated to 60°C, glyoxylic acid, ethyl guaiacol and alkali solution were added dropwise to the reaction bottle at the same time. The concentration of the 3-ethoxy-4-hydroxymandelic acid intermediate is less than 2.0%, and the dropping speed of the alkali solution is controlled to make the pH of the solution 11-13. The raw material solution was dropped in about 6 hours, then the tempe...

Embodiment 3

[0026] Catalyst preparation: Weigh 7.5g (0.03mol) of reagent copper sulfate and 7.2g (0.03mol) of reagent cobalt sulfate, and dissolve them in 100mL deionized water to prepare a metal salt solution. The rare earth Y-type molecular sieve (Re 2 o 3 ≥17%; SiO 2 / Al 2 o 3 ≥5;Na 2 O ≤ 2%; loss on ignition ≥ 3%) 100g was added to the above metal salt solution and soaked for 30 minutes, then 5% sodium hydroxide solution was added dropwise to pH 11, molecular sieves were separated by vacuum filtration, washed with a small amount of deionized water to remove sodium sulfate Salt, dry at 105°C, oxidize and roast in a high-temperature furnace at 550°C for 60 minutes, and set aside.

[0027]The catalyst is applied to the synthesis of vanillin: 74.1g (0.4mol) 40% glyoxylic acid, 54.0g (0.48mol) guaiacol and 100mL30% Liquid caustic soda. Add 500 mL of deionized water, 106.6 g (0.8 mol) of 30% liquid caustic soda into the four-necked reaction flask, add 5.0 g of catalyst, stir and blow...

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Abstract

The invention discloses a catalyst for synthesizing (ethyl) vanillin by using a glyoxylic acid method, and the method is characterized by taking a rare-earth Y-molecular sieve as carrier, and copper oxides and cobalt oxides as active components and comprising the steps of active-component salt solution preparation, carrier dipping, neutralization and precipitation, and oxidizing roasting. The molar ratio of copper to cobalt loaded on the catalyst is 1:(0.1-1); the selected rare-earth Y-molecular sieve comprises the following compositions in percentage by weight: no less than 17% of Re2O3, no less than 5% of SiO2 / Al2O3, and no more than 2% of Na2O; and the mass fraction of the copper and cobalt active components on the catalyst is 0.01-0.1. The invention has the advantages that because an industrial catalyst is adopted as the carrier, the method for preparing the catalyst is simple, the activity of the catalyst is high, the generation of polymeric by-products is restrained, and the yield of the synthesized vanillin is 89.2%.

Description

technical field [0001] The invention relates to a catalyst for synthesizing (ethyl) vanillin by glyoxylic acid method, especially a catalyst for synthesizing (ethyl) vanillin with rare earth Y-type molecular sieve as carrier and copper oxide and cobalt oxide as active components. Fine chemical industry. Background technique [0002] (Ethyl) vanillin is an important pharmaceutical chemical raw material and intermediate. There are many production routes for (ethyl) vanillin, and the glyoxylic acid process route is generally used at present. Jihua Group Corporation discloses in Chinese patent CN101012161 (2007-08-08) the improvement to glyoxylic acid synthesis (ethyl) vanillin condensation reaction, adopts quaternary ammonium salt catalyst, raw material glyoxylic acid, (ethyl) Base) The molar ratio of guaiacol and sodium hydroxide is 1:1.1-1.2:2.2-2.3, the optimum condensation temperature is 27-29°C, the condensation reaction time is 3.5-5 hours, and the condensation reaction ...

Claims

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Application Information

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IPC IPC(8): B01J29/14C07C47/58C07C47/575C07C45/54
Inventor 李霞李建生
Owner TIANJIN VOCATIONAL INST
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