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Catalyst for preparation of carboxylate and preparation method thereof

A catalyst and carrier technology, applied in the direction of carboxylate preparation, formation/introduction of carboxylate groups, chemical instruments and methods, etc., can solve the problems of low reaction rate of carboxylate and unexpected by-products, and achieve high The effect of reaction efficiency

Active Publication Date: 2011-10-05
LEE CHANG YUNG CHEM IND CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the aforementioned catalyzed methods for preparing carboxylates have low reactivity and unintended by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Niobium-modified oxyesterification catalyst

[0041] 11.08 grams of niobium oxalate were added to 170 grams of deionized water. After it dissolves, add 50 grams of SiO 2 support into the above solution to form mixture 1A, which was then dried under reduced pressure and calcined into niobium-modified SiO 2 carrier.

[0042] Add 4.33 grams of lead acetate and 8.28 grams of magnesium acetate to 141 grams of deionized water, and after they dissolve, add 47.43 grams of niobium-modified SiO 2 support into the above solution to form mixture 1B, which was then dried under reduced pressure and calcined into niobium / lead / magnesium-modified SiO 2 carrier.

[0043] Add 4.16 grams of palladium chloride to 199.4 grams of deionized water, and after it dissolves, add 49.85 grams of niobium / lead / magnesium modified SiO 2 Carrier into the above solution, the obtained suspension was concentrated into a dark brown mixture 1C, the mixture 1C was reduced and filtered, and the obtained fi...

Embodiment 2

[0046] Zirconium-modified oxyesterification catalyst

[0047] Add 18.99 grams of zirconyl nitrate to 350 grams of deionized water, and after it dissolves, add 100 grams of SiO 2 support into the above solution to form a mixture 2A, which was then dried under reduced pressure and calcined into zirconium-modified SiO 2 carrier.

[0048] 8.07 grams of lead acetate and 15.52 grams of magnesium acetate were added to 363.4 grams of deionized water. After it dissolves, add 87.71 g of zirconium-modified SiO 2 support into the above solution to form a mixture 2B, which was then dried under reduced pressure and calcined into zirconium / lead / magnesium modified SiO 2 carrier.

[0049] Add 7.93 grams of palladium chloride to 382.3 grams of deionized water, and after it dissolves, add 105.96 grams of zirconium / lead / magnesium modified SiO 2 The carrier is added to the above solution, the obtained suspension is concentrated into a dark brown mixture 2C, then the mixture 2C is reduced and ...

Embodiment 3

[0056] The catalyst A of embodiment 1 is placed in a high-temperature and high-pressure reactor with a stirrer, at 80 degrees Celsius, 5kg / cm 2 test under pressure.

[0057] Methacrolein (TCI reagent grade, supplied by Tokyo Kasei Kogyo Co., Ltd.) and methanol (supplied by Merck, purity 99.5%) were mixed to form a methanol reaction solution containing 30% methacrolein. In addition, lead acetate (provided by SHOWA, with a purity of 99.5%) is added to the reaction solution as a catalyst stabilizer, and the controlled release of the oxygen component is 2-4%, and the mol ratio between the aldehydes and alcohols in the reaction solution is 1:5, and the lead concentration in the reaction solution was 60ppm.

[0058] Under the condition of introducing air, when the reaction solution reacts with 20.5 grams of catalyst A, the reaction pressure is increased to 5kg / cm 2 , and the temperature was increased to 80 °C.

[0059] After feeding additional reaction solution, the feeding rate ...

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Abstract

Catalyst for the catalysis reaction of carboxylic acid-ester from an aldehyde and an alcohol in presence of molecular oxygen, exhibits a silicate containing matrix applied metals, where the metals are palladium, lead, an alkali- or alkaline earth metal, and at least niobium or zirconium, is new. An independent claim is included for a method for producing carboxylic acid-ester by reacting an aldehyde with an alcohol in the presence of molecular oxygen and the catalyst exhibiting metal.

Description

technical field [0001] The invention provides a catalyst capable of producing carboxylate, especially a catalyst capable of preparing carboxylate by one stage reaction of aldehydes and alcohols, and a preparation method of carboxylate. Background technique [0002] The known method for the preparation of carboxylic acid esters is to first oxidize aldehydes to carboxylic acids, and then react the carboxylic acids with alcohols. However, the disadvantage of this method is that a large amount of starting material is required because the process has a two-step reaction operation (oxidation and esterification). Furthermore, this process suffers from the low expressivity of the catalyst used in the reaction, and it obtains insufficient yields of carboxylic acid esters. [0003] Several methods have been disclosed for the one-stage liquid phase reaction of aldehydes and alcohols in the presence of specific catalysts for the production of carboxylic acid esters in high yields. For...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/00B01J23/44B01J32/00B01J23/14B01J23/02
CPCC07C67/39B01J23/6484C07B41/12B01J23/628B01J37/0205
Inventor 刘怀德卢敏彦林文淇张美元
Owner LEE CHANG YUNG CHEM IND CORP
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