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Method for preparing ester by catalytic oxidization of 1,3-propanediol

A technology for catalytic oxidation and propylene glycol, applied in the direction of catalyst activation/preparation, chemical instruments and methods, and preparation of organic compounds, which can solve the problem of low reaction rate and achieve high selectivity

Inactive Publication Date: 2010-12-08
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method needs to add difficult and highly corrosive sodium methoxide, and the reaction rate is low

Method used

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  • Method for preparing ester by catalytic oxidization of 1,3-propanediol
  • Method for preparing ester by catalytic oxidization of 1,3-propanediol
  • Method for preparing ester by catalytic oxidization of 1,3-propanediol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1 hydrothermal method prepares nanometer ceria of different shapes

[0022] Add 24 grams (or 0.4 grams) of sodium hydroxide and 1.95 grams of cerium nitrate into the reactor, conduct a hydrothermal reaction at 100-180°C for 24 hours, filter and wash until neutral. Dry at 80°C for 12 hours, and bake at 100-1000°C for 4 hours. respectively get CeO 2 Nano-cube, nano-rod and nano-polyhedron carrier, the above-mentioned catalyst carrier is made into 40-60 mesh particles for future use.

Embodiment 2

[0023] Embodiment 2 deposition-precipitation method prepares the catalyst of loading 1%Au (Pd)

[0024] One of urea, sodium carbonate or sodium hydroxide is added to the gold chloride (Pd metal) solution so that the molar ratio is 1:100, and deionized water and oxide carrier are added so that the precious metal:carrier mass ratio is 1 : 100, placed in a water bath at 70-100°C for 2-4h, then the mixture was washed, filtered with suction, and dried. That is, the test catalyst was obtained.

Embodiment 3

[0025] Embodiment 3 prepares Au colloid

[0026] 100μg / mlHAuCl 4 The aqueous solution was added dropwise with 2wt% PVA (M=10000) aqueous solution (PVA / Au(wt / wt)=0.62) under stirring, then stirred for 10min, and then added dropwise with 0.1M freshly prepared NaBH 4 Solution (NaBH 4 / Au (mol / mol)=4), that is, Au colloid is obtained.

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Abstract

The invention discloses a method for preparing an ester by catalytic oxidization of 1,3-propanediol. The catalyst adopted is a supported noble metal catalyst (gold or palladium); a carrier is made from metal oxides of different shapes and sizes or mixed oxides (such as CeO2, gamma-Al2O3, CuO, MgO, ZnO, ZSM-5, MoO3, V2O5 and the like), or a silicon dioxide-containing material or a carbon material; after the catalyst is treated by different preparation and treatment methods, the selective oxidization reaction of the 1,3-propanediol for preparing 3-methyl lactate, dimethyl malenate, 3-methoxypropionate and methyl acrylate is performed under a mild liquid-phase or liquid- and gas-phase reaction condition. The highest yield of the produced 3-methyl lactate is 81.5 percent (the conversion rate is 97.0 percent and the selectivity is 84.0 percent); the highest yield of the produced dimethyl malenate is 58.2 percent ( the conversion rate is 99.6 percent and the selectivity is 58.4 percent); and the highest yield of produced 3-methoxypropionate is 53.0 percent (the conversion rate is 97.0 percent and the selectivity is 58.4 percent) and the highest yield of produced methyl acrylate is 38.4 percent (the conversion rate is 92.2 percent and the selectivity is 41.6 percent).

Description

technical field [0001] The invention relates to heterogeneous catalytic technology, in particular to a method for preparing ester by catalytic oxidation of 1,3-propanediol. Background technique [0002] 1,3-propanediol (1,3-PDO) is an important chemical raw material, which can be used to synthesize polyester (PTT), polyether and polyurethane, synthetic medicine and organic synthesis intermediates, etc. In recent years, due to the development of 1,3-propanediol fermentation technology using renewable biomass resources as raw materials, it provides opportunities for 1,3-propanediol as a bio-based platform compound to replace non-renewable petrochemical resources to produce a variety of chemical products . Methyl 3-hydroxypropionate, dimethyl malonate, methyl 3-methoxypropionate and methyl acrylate produced by oxidative conversion of 1,3-propanediol are important chemical raw materials and have broad application prospects. [0003] U.S. Patent No. 4,973,741 carbonylates 3-hyd...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C67/08C07C69/38C07C69/708C07C69/54B01J23/52B01J29/44B01J23/44B01J37/10
CPCY02P20/50
Inventor 朱建航王相伟赵国明张永光张汝兵张帆
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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