Synthesis method of saturated aldehyde

A synthesis method and unsaturated technology, applied in the field of catalytic synthesis, can solve problems such as catalyst instability, loss of active phase, and potential safety hazards, and achieve the effect of being suitable for storage and transportation, high activity, and ensuring safety

Pending Publication Date: 2021-04-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although Raney nickel and amorphous nickel have relatively excellent catalytic selectivity, they are prone to loss and agglomeration of the active phase during the catalytic hydrogenation process, and the catalyst itself is unstable in the air, which poses a greater safety hazard.

Method used

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  • Synthesis method of saturated aldehyde
  • Synthesis method of saturated aldehyde
  • Synthesis method of saturated aldehyde

Examples

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preparation example Construction

[0033] The invention provides a method for synthesizing saturated aldehydes, comprising: using carbon-coated nickel nanocomposites as catalysts to catalyze α, β-unsaturated aldehydes for hydrogenation reduction reaction in a hydrogen atmosphere to obtain saturated aldehydes; wherein, The nanocomposite has a core-shell structure with a shell of graphitized carbon layers containing alkali metals and oxygen and a core of nickel nanoparticles comprising a face centered cubic lattice structure and / or a hexagonal compact lattice structure.

[0034] In some embodiments, the α,β-unsaturated aldehyde may be selected from one or more of cinnamaldehyde, furfural, 3-methyl-2-butenal and acrolein. Among them, the α, β-unsaturated aldehyde referred to in the present invention refers to the carbon atom directly connected with the aldehyde functional group is called "α" position, and the one separated by one carbon atom is called "β" position. Saturated bond (double bond), so it is called α,...

preparation example 1

[0066] This preparation example illustrates the preparation of carbon-coated nickel nanocomposites

[0067] 1) Weigh 4.38g (15mmol) of ethylenediaminetetraacetic acid and 1.85g (20mmol) of nickel hydroxide into 150mL of deionized water, stir at 75°C to obtain a homogeneous solution, continue to heat and evaporate to dryness, and grind the solid to obtain Precursor.

[0068] 2) Put the precursor obtained in step 1) in the porcelain boat, then place the porcelain boat in the constant temperature zone of the tube furnace, feed nitrogen with a flow rate of 80mL / min, and raise the temperature to 600°C at a rate of 3°C / min , stop heating after 3 hours at constant temperature, and cool to room temperature under a nitrogen atmosphere to obtain a composite material.

[0069] 3) Add 60mL 0.5mol / L H to the composite material obtained in step 2) 2 SO 4 In the solution, after stirring and refluxing at 80°C for 6h, the solution was suction-filtered, washed with deionized water until neut...

preparation example 2

[0072] This preparation example is used to illustrate the preparation of another carbon-coated nickel nanocomposite

[0073] 1) Weigh 10 mmol of nickel hydroxide and 10 mmol of citric acid into 150 mL of deionized water, stir at 80°C to obtain a homogeneous solution, continue to heat and evaporate to dryness, and grind the solid to obtain a precursor.

[0074] 2) Put the precursor obtained in step 1) in the porcelain boat, then place the porcelain boat in the constant temperature zone of the tube furnace, feed nitrogen gas at a flow rate of 150mL / min, and raise the temperature to 575°C at a rate of 2.5°C / min , stop heating after constant temperature for 2h, and cool to room temperature under nitrogen atmosphere to obtain a composite material.

[0075] 3) Add the composite material obtained in step 2) into 50mL 1mol / L H 2 SO 4 In the solution, the solution was stirred and refluxed at 90° C. for 4 hours, then the solution was suction-filtered, washed with deionized water until...

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Abstract

The present invention provides a synthesis method of saturated aldehyde, which comprises that a carbon-coated nickel nanometer composite material is adopted as a catalyst, and alpha, beta-unsaturated aldehyde is catalyzed under a hydrogen atmosphere to carry out a hydrogenation reduction reaction so as to obtain saturated aldehyde, wherein the nano composite material contains a core-shell structure with a shell layer and an inner core, the shell layer is a graphitized carbon layer, the inner core is nickel nano particles, and the inner core of the nickel nano particles comprises a face-centered cubic lattice structure and/or a hexagonal compact lattice structure. The carbon-coated nickel nano composite material is used as the catalyst, C=C bonds can be selectively hydrogenated to synthesize corresponding saturated aldehyde from alpha, beta-unsaturated aldehyde, the reaction selectivity is high, the condition is mild, the product is conveniently separated from the catalyst, and compared with an industrial traditional Raney nickel catalyst, the catalytic system has better safety and stability.

Description

technical field [0001] The invention belongs to the technical field of catalytic synthesis, in particular to a method for synthesizing saturated aldehydes. Background technique [0002] The α,β-unsaturated aldehyde structure contains conjugated C=C bonds and C=O bonds. Selective hydrogenation of C=O bonds can synthesize unsaturated alcohols, while selective hydrogenation of C=C bonds can synthesize corresponding saturated aldehydes. These two types of substances have important uses in industries such as medicine, pesticides, and spices. For example, 3-phenylpropanal can be used as an intermediate of HIV treatment drugs. The catalytic hydrogenation of α,β-unsaturated aldehydes to prepare corresponding saturated aldehydes has better atom economy, which is of great significance for theoretical research and industrial applications. [0003] Catalysts for catalytic hydrogenation mainly include supported noble metals (Pt, Rh, Ir, Ru, Au), Raney nickel and amorphous alloys. Amo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/62C07C49/213B01J23/755B01J27/24B01J35/10
CPCC07C45/62B01J27/24B01J23/755B01J35/1019B01J35/1038B01J35/0086B01J35/0033C07C49/213
Inventor 吴耿煌荣峻峰达志坚宗明生于鹏纪洪波
Owner CHINA PETROLEUM & CHEM CORP
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