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Method for preparing n-octanal

A technology of n-octyl aldehyde and octatrienal, which is applied in the direction of carbon-based compound preparation, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problem that it is difficult to improve the conversion rate of crotonaldehyde, so as to improve the reaction conversion rate and The effect of selectivity, novel synthetic route and low price

Active Publication Date: 2022-06-03
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above two catalysts are difficult to improve the conversion rate of crotonaldehyde in the aldol condensation reaction.

Method used

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  • Method for preparing n-octanal
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  • Method for preparing n-octanal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Preparation of catalyst A: carbon nanotubes, silver nitrate, cadmium nitrate, and lead nitrate were mixed in water according to a mass ratio of 100:1:1:1, immersed at 25°C for 24 hours, and then calcined at 500°C for 8 hours in a nitrogen atmosphere. Then, the obtained mixture is uniformly mixed with sodium hydroxide, and the mass ratio of sodium hydroxide to carbon nanotubes is 1:10 to obtain catalyst A.

Embodiment 2-5

[0054] Embodiment 2-5 (abbreviated as S2-S5) and comparative example 1-4 (abbreviated as D1-D4)

[0055] The preparation process parameters of condensation catalyst B-I are shown in Table 1. The composition of the condensation catalyst is shown in Table 2.

[0056] Table 1 Condensation catalyst B-I preparation process parameters

[0057] catalyst carrier Active ingredient m 1 :m 2 :m 3 :m 4 :m 5

Immersion temperature / time Roasting temperature / time S2 B Graphene Zinc oxide 100:5:1:1:0.5 30℃ / 48h 400℃ / 4h S3 C carbon nanocloth Calcium Oxide 100:20:1:1:0.8 40℃ / 12h 600℃ / 6h S4 D activated carbon Calcium hydroxide 100:10:0.8:0.5:1 30℃ / 24h 500℃ / 4h S5 E carbon nanotubes sodium oxide 100:15:1:0.8:1 30℃ / 36h 600℃ / 5h D1 F carbon nanotubes sodium hydroxide 100:10:0:1:1 25℃ / 24h 500℃ / 8h D2 G carbon nanotubes sodium hydroxide 100:10:1:0:1 25℃ / 24h 500℃ / 8h D3 H carbon nanotubes sodium...

Embodiment 6-10

[0061] Example 6-10 (S6-S10 for short) and Comparative Example 5-8 (D5-D8 for short)

[0062] Using crotonaldehyde as raw material, 2,4,6-octatrienal was prepared by gas-phase condensation reaction. The reactor for the gas phase condensation reaction is in the form of a fixed bed. The gas-phase condensation reaction of crotonaldehyde is carried out under a certain catalyst concentration, certain temperature and residence time to obtain 2,4,6-octatrienal. The technical parameters of the condensation reaction are shown in Table 3. The condensation reaction results are shown in Table 4.

[0063] Table 3 Condensation reaction process parameters

[0064] Condensation catalyst Condensation reaction temperature / residence time Condensation catalyst dosage / wt% S6 A 250℃ / 1h 0.1 S7 B 180℃ / 2h 1.0 S8 C 360℃ / 0.5h 0.05 S9 D 300℃ / 3h 0.1 S10 E 250℃ / 2h 2.0 D5 F 250℃ / 1h 0.1 D6 G 250℃ / 1h 0.1 D7 H 250℃ / 1h 0.1 D8 I 250℃...

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Abstract

The invention provides a method for preparing n-octanal. Comprising the following steps: (1) carrying out gas phase condensation reaction on crotonaldehyde to obtain 2, 4, 6-octyltrienal; and (2) carrying out hydrogenation reaction on the 2, 4, 6-octyltrienal to obtain the n-caprylic aldehyde. The step (1) is carried out under the action of a modified basic catalyst, and the modified basic catalyst comprises an active component, a cocatalyst silver, cadmium oxide, lead oxide and a carrier. In the step (2), under the action of the modified palladium-carbon catalyst, the catalyst comprises the following components: palladium, nitrogen, phosphorus, sulfur, boron and a carbon-based carrier. The synthesis route is novel, the cheap and easily available crotonaldehyde is used as the starting raw material, the n-caprylic aldehyde is obtained through two-step reaction, the synthesis route is short, and the method has the potential of replacing an existing traditional process route. The modified basic catalyst is used as the catalyst, so that the selectivity of the condensation reaction is high. And completing high-selectivity hydrogenation of the 2, 4, 6-octyltrienal intermediate by adopting a modified palladium carbon catalyst to obtain an n-octanal product.

Description

technical field [0001] The invention belongs to the fields of fine chemicals and flavors and fragrances, and particularly relates to a method for preparing n-octylaldehyde. Background technique [0002] n-Octalaldehyde is a colorless or slightly yellow liquid with a strong fruity odor. It is used in the fragrance industry to prepare flavors such as rose, carnation, orange blossom, and orange cologne. It can be used in the food industry. Used to produce sweet orange aroma. At present, n-octanol is mostly used in industry to catalyze or oxidative dehydrogenation to prepare n-octaldehyde, and it is also prepared by the reduction of n-octanoic acid under the action of nickel catalyst. [0003] The catalysts used in the oxidative dehydrogenation of n-octanol to prepare n-octaldehyde include potassium chromate, metal oxides, phase transfer catalysts, etc. However, reports at home and abroad all show that the method for preparing n-octylaldehyde by oxidation has low conversion ra...

Claims

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Application Information

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IPC IPC(8): C07C45/62C07C47/02C07C45/74C07C47/21B01J23/66B01J23/44B01J27/24B01J37/02B01J37/08B01J37/14
CPCC07C45/62C07C45/74B01J23/66B01J23/002B01J23/44B01J27/24B01J37/0201B01J37/088B01J37/14B01J37/084B01J2523/00C07C47/21C07C47/02B01J2523/18B01J2523/28B01J2523/44B01J2523/27B01J2523/23B01J2523/12Y02P20/584
Inventor 宋军伟王永军李剑鹏黄文学谢硕王延斌
Owner WANHUA CHEM GRP CO LTD
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