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A kind of method that solid catalyst catalyzes n-butyraldehyde one-step synthetic isooctylaldehyde

A technology of solid catalyst and n-butyraldehyde, which is applied in the field of green chemistry, can solve problems such as low conversion rate of n-butyraldehyde, decline, and poor catalyst stability, and achieve the effects of broad industrialization prospects, shortened process flow, and high selectivity

Active Publication Date: 2022-04-19
HEBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Although the highest selectivity of isooctylaldehyde can reach more than 90%, the conversion rate of n-butyraldehyde is low, and the highest is only close to 80% (occurring at the beginning of the reaction), and the catalyst stability is relatively poor, and it reacts in a fixed bed. After running for 300 minutes, the conversion rate of n-butyraldehyde has dropped below 30%.

Method used

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  • A kind of method that solid catalyst catalyzes n-butyraldehyde one-step synthetic isooctylaldehyde
  • A kind of method that solid catalyst catalyzes n-butyraldehyde one-step synthetic isooctylaldehyde

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Pd / Fe 2 o 3 The preparation process of @C multifunctional catalyst: (1) weigh 32.32g (0.08mol) Fe(NO 3 ) 3 9H 2 O, 2.52g (0.012mol) trimesic acid, 0.035g (0.2mmol) PdCl 2 Mix well with 200mL absolute ethanol; (2) Add the prepared mixed solution into a polytetrafluoroethylene-lined crystallization kettle, raise the temperature to 160°C and keep it for 12 hours; (3) After the reaction, centrifuge and separate dried, and the resulting solid was 2 Calcined at 450°C for 5 hours in the atmosphere to prepare PdO / Fe 2 o 3 @C; (4) PdO / Fe 2 o 3 @C on H 2 Reduction at 300°C for 4 hours in the atmosphere to finally produce Pd / Fe 2 o 3 @C multifunctional catalyst, wherein, the mass fraction of metal Pd is 0.25%, Fe 2 o 3 The mass fraction of is 85%, and the rest is C.

Embodiment 2

[0041] Pd / ZnO-Al 2 o 3 Preparation process of @C multifunctional catalyst: (1) Preparation of ZnO-Al by co-precipitation method 2 o 3 Carrier (Zn / Al molar ratio is 3:1); (2) weigh 4.75g ZnO-Al 2 o 3 Carrier, 0.025g PdCl 2And 0.85g glucose, join in the mixed solution of ethanol and water (10mL, the volume ratio of ethanol and water is 1:1); (3) remove water and ethanol by rotary evaporation at 80 ℃, gained solid is in N 2 Calcined at 500°C for 4 hours in the atmosphere to obtain PdO / ZnO-Al 2 o 3 @C; (4) put the roasted sample in H 2 Pd / ZnO-Al can be prepared by reducing at 350°C for 4 hours in the atmosphere 2 o 3 @C multifunctional catalyst, wherein the mass fraction of metal Pd is 0.3%, ZnO-Al 2 o 3 The mass fraction of is 93.3%, and the rest is C.

[0042] The multifunctional catalysts used in the following reaction examples are all prepared by catalyst preparation example 1, example 2, or similar methods.

Embodiment 3

[0044] Add 30g of n-butyraldehyde and Pd / Fe equivalent to 10% of the quality of n-butyraldehyde in the 100mL autoclave 2 o 3 @C Catalyst, use N first 2 Displacing the air, followed by H 2 Replacement, at a reaction temperature of 160°C, filled with H 2 Maintain the pressure at 2.0MPa, and magnetically stir for 6h. After the reaction, the product liquid was analyzed by gas chromatography, the conversion rate of n-butyraldehyde was 94.3%, and the selectivity of isooctylaldehyde was 96.0%.

[0045] Examples 4-10 are in accordance with the operation steps of Reaction Example 3, and the reaction conditions and results are shown in the summary table.

[0046]

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Abstract

The invention relates to a method for one-step synthesis of isooctylaldehyde from n-butyraldehyde catalyzed by a solid catalyst. The method comprises the following steps: adding a solid catalyst and n-butyraldehyde into an autoclave or a fixed-bed reactor, filling with hydrogen, and reacting at 120-200° C. to obtain isooctaldehyde; the solid catalyst is Pd / solid acid -Basic@C catalyst, wherein, the mass fraction of metal Pd in ​​the catalyst is 0.1-0.5%, the mass fraction of solid acid-base in the catalyst is 80-95%, and the rest is C. The invention has the advantages of short process flow, low equipment and operating costs, and environmental friendliness; at the same time, the designed and prepared Pd / solid acid-base@C catalyst has the characteristics of high activity, stability and selectivity.

Description

technical field [0001] The invention belongs to the technical field of green chemistry, and relates to a process for one-step synthesis of isooctylaldehyde from n-butyraldehyde with a solid catalyst, specifically the preparation of Pd / solid acid-alkali@C multifunctional catalyst and its application in the catalysis of n-butyraldehyde A process for synthesizing isooctylaldehyde from aldehydes in one step. Background technique [0002] Isooctylaldehyde (2-ethylhexanal) is an important chemical intermediate, which can be oxidized to generate isooctanoic acid, and can also be further hydrogenated to produce plasticizer dioctyl phthalate (DOP). isooctyl alcohol. At the same time, isooctylaldehyde is also a flavor additive used in the synthesis of soaps and detergents. [0003] At present, the industrial production of isooctyl aldehyde is mainly carried out by propylene oxo synthesis (also known as hydroformylation reaction or hydroformylation reaction). The synthesis of isooct...

Claims

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Application Information

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IPC IPC(8): C07C45/73C07C47/02B01J23/44B01J23/60B01J23/63B01J23/89
CPCC07C45/73B01J23/8906B01J23/60B01J23/44B01J23/63C07C47/02
Inventor 安华良周典根赵新强薛伟王延吉
Owner HEBEI UNIV OF TECH
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