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Rhodium-based catalyst for glycollic aldehyde synthesis and preparation method thereof

A catalyst and glycolaldehyde technology, applied in the direction of catalyst activation/preparation, carbon monoxide reaction preparation, molecular sieve catalyst, etc., can solve the problems of difficult catalyst separation, low conversion rate of formaldehyde, influence of Rh activity, etc., and achieve easy recovery and low conversion rate , the effect of increasing the load

Inactive Publication Date: 2021-02-09
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wu Xiaoman et al. (CN 105618035 A) prepared a supported Rh / SiO2 catalyst for the synthesis of glycolaldehyde by impregnation method. Although the catalyst can solve the defects such as difficult separation of the catalyst in the homogeneous system, the activity of Rh is obviously affected. , the conversion of formaldehyde is much lower than that of the homogeneous Rh catalyst

Method used

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  • Rhodium-based catalyst for glycollic aldehyde synthesis and preparation method thereof
  • Rhodium-based catalyst for glycollic aldehyde synthesis and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A. Accurately weigh 1.5g SiO 2 , placed in a 250ml three-necked flask, added 50mL of toluene, and continuously fed dry N 2 , stirred magnetically at room temperature for 30 minutes, added 2 mL of 3-aminopropyltriethoxysilane dropwise to a constant pressure funnel, raised the temperature to 110°C, stirred for 24 hours, filtered and washed, and vacuum-dried at 50°C for 12 hours to obtain amino-modified N -SiO 2 .

[0025] B. In a 250mL three-necked flask, 0.1g rhodium precursor Rh(acac)(CO) 2 Dissolve in 60ml of ethanol solution, stir magnetically for 30min, and prepare 6.4mmol / L rhodium solution.

[0026] C. Take the carrier N-SiO obtained in step A 2 1.0g is added in the rhodium solution of step B, continuously feeds dry N 2 Stir at room temperature for 16 hours, impregnate and load, filter and wash to remove excess ethanol and unsupported Rh, and dry the catalyst precursor at 90°C for 3 hours to obtain Rh / N-SiO 2 In the catalyst, the mass percentage of N is abou...

Embodiment 2

[0029] A: Accurately weigh 3.0g of NaY molecular sieve, place it in a 250ml three-necked flask, add 1000mL of toluene, and continuously feed dry N 2 , stirred magnetically at room temperature for 50 minutes, added 4 mL of 3-aminopropyltriethoxysilane dropwise to a constant pressure funnel, raised the temperature to 50°C, stirred for 24 hours, filtered and washed, and dried in vacuum at 80°C for 12 hours.

[0030] B: In a 250mL three-necked flask, the rhodium precursor Rh(acac)(CO) 20.05g was dissolved in 40mL of absolute ethanol, magnetically stirred for 60min, and configured as a 4.8mmol / L rhodium solution.

[0031] C. Take 1.0 g of the carrier N-NaY obtained in step A and add it to the rhodium solution in step B, and continue to feed dry N-NaY 2 Stir at room temperature for 16 hours, impregnate and load, filter and wash to remove excess ethanol and unsupported Rh, and dry the catalyst precursor at 90°C for 3 hours to obtain the supported catalyst Rh / N-NaY, wherein the mass ...

Embodiment 3

[0034] A. Accurately weigh 1.5g SiO 2 , placed in a 250ml three-necked flask, added 50mL of toluene, and continuously fed dry N 2 , stirred magnetically at room temperature for 30 minutes, added 2 mL of γ-aminoethylaminopropyltrimethoxysilane dropwise to a constant-pressure funnel, raised the temperature to 110°C, stirred for 48 hours, filtered and washed, and vacuum-dried at 50°C for 12 hours to obtain amino-modified N-SiO 2 ; Wherein the mass percentage of N is 4.22%, and the mass percentage of Rh is 3.03%;

[0035] B. In a 250mL three-necked flask, 0.1g rhodium precursor Rh(acac)(CO) 2 Dissolve in 60ml of ethanol solution, stir magnetically for 30min, and prepare 6.4mmol / L rhodium solution.

[0036] C. Take 1.0 g of the carrier N-NaY obtained in step A and add it to the rhodium solution in step B, and continue to feed dry N-NaY 2 Stirring at room temperature for 28 hours to impregnate and load, filter and wash to remove excess ethanol and unloaded Rh, and dry the cataly...

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Abstract

The invention provides a rhodium-based catalyst for glycollic aldehyde synthesis and a preparation method of the rhodium-based catalyst. The method adopted by the invention comprises the steps of firstly, carrying out organic functional group modification on the surface of a carrier, then dipping and adsorbing in a rhodium precursor solution, washing and drying to obtain the high-dispersion and high-load rhodium-based immobilized catalyst. Compared with a solid catalyst prepared by a common impregnation method, the catalyst provided by the invention is higher in conversion rate and selectivitywhen being used for hydroformylation reaction of formaldehyde, and compared with a traditional homogeneous formaldehyde hydroformylation method, the yield of the glycolaldehyde product generated integrally is basically the same, so that the problems that the homogeneous catalyst is difficult to separate from the product and precious metal is difficult to recover are solved, and the problems of low formaldehyde conversion rate and low yield of a common supported rhodium catalyst are also solved.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a supported rhodium-based catalyst for synthesizing glycolaldehyde through a formaldehyde hydroformylation reaction route and its preparation. Background technique [0002] Glycolaldehyde is an important raw material for organic synthesis. As the smallest sugar molecule, glycolaldehyde can react with acrolein to generate ribose, which is of great significance to the synthesis of RNA in vivo. Glycol aldehyde is an intermediate of ethylene glycol, which can be hydrogenated as a raw material for preparing ethylene glycol to obtain ethylene glycol. Glycolaldehyde can also be used in the synthesis of pesticides and drugs, protein modifiers, reducing agents and antibacterial agents, and has a very considerable market value. [0003] Synthesis of glycolaldehyde by hydroformylation of formaldehyde is a well-known technical route for converting carbon-1 raw materials to ca...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/20B01J31/18B01J31/02B01J29/08B01J37/02C07C45/50C07C47/19
CPCB01J29/084B01J31/0274B01J31/0275B01J31/1805B01J31/20B01J31/2213B01J37/0207B01J2231/321B01J2531/0238B01J2531/822C07C45/505C07C47/19
Inventor 姚元根陈婕乔路阳周张锋吴小满郭夏芯宗珊珊
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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