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Process method for one-step synthesis of long-chain alcohol by catalyzing aldehydes with solid catalyst

A technology for catalyzing aldehydes and solid catalysts with catalysts, applied in the field of green chemistry, can solve the problems of catalysts that cannot be reused, large waste water discharge, environmental pollution, etc. short process effect

Active Publication Date: 2014-04-09
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the aldol condensation reaction, liquid alkali (dilute NaOH solution) is often used as a catalyst in the industry. Although a high conversion rate of raw materials and product yield can be obtained, the catalyst cannot be reused, the equipment is severely corroded, and the amount of waste water is discharged. , serious environmental pollution

Method used

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  • Process method for one-step synthesis of long-chain alcohol by catalyzing aldehydes with solid catalyst
  • Process method for one-step synthesis of long-chain alcohol by catalyzing aldehydes with solid catalyst
  • Process method for one-step synthesis of long-chain alcohol by catalyzing aldehydes with solid catalyst

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0021] Taking the preparation of Ni-Ce-HY catalyst as an example, the preparation process

[0022] The solid acid HY was calcined in a muffle furnace at 500°C for 4h for later use. First, weigh the metal component precursor Ni(NO 3 ) 2 ·6H 2 O2.664g and auxiliary precursor Ce(NO 3 ) 3 ·6H 2 O0.543g was made into 15mL aqueous solution, and the prepared salt solution was immersed in 10g of heat-treated solid acid HY; after aging for 24h, it was dried at 110°C for 10h, then roasted in a muffle furnace at 450°C for 4h, and finally, 5wt.%Ni-Ce-HY catalyst can be obtained by reducing at 450℃ for 4h in the hydrogen atmosphere of the reduction furnace, in which the mass fraction of Ni is 5%, and the mass fraction of additives is 2%.

Embodiment 1

[0024] Add 30g of n-valeraldehyde and a Ni-Ce-HY catalyst equivalent to 10% of the mass of n-valeraldehyde into a 100mL autoclave, first use N 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, and the conversion rate of n-valeraldehyde was 89.2%, and the yield of decanol was 75.0%. At the same time, a small amount of n-valeraldehyde was directly hydrogenated to generate n-pentanol, and the yield of n-pentanol was 11.8%.

[0025] Examples 2-17 According to the operation steps of Example 1, the reaction conditions and results are shown in the summary table.

[0026]

[0027]

[0028] Examples 18-38 According to the operation steps of Example 1, n-butyraldehyde was selected as the raw material aldehyde, and the reaction conditions and results are shown in the summary table.

[0029]...

Embodiment 39

[0032] In a 100mL autoclave, put 32g n-butyraldehyde, and then add 15wt.%Cu-Cr-MgO catalyst with 10% n-butyraldehyde mass, first use N 2 Purge three times with H 2 Purge three times. flushed with H at 200 °C 2 Maintain the reaction pressure at 4.5MPa, and magnetically stir for 8h. After the reaction was finished, it was filtered under reduced pressure, and the filtrate was analyzed by gas chromatography. The conversion rate of n-butyraldehyde was 100%, and the yield of 2-ethylhexanol was 78.1%. The reacted catalyst was washed three times with absolute ethanol, and dried at 110° C. for 8 h. Roasted in a muffle furnace at 500°C for 4h, and then heated with H 2 Reduction at 200°C for 4h. Then under the same reaction conditions, the repeated use effect of the catalyst was investigated, and the results are shown in the table below. With the increase of the number of reactions, the activity of the catalyst decreased slightly, and the yield of 2-ethylhexanol decreased by 5.4% a...

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Abstract

The invention relates to a process method for one-step synthesis of long-chain alcohol by catalyzing aldehydes with a solid catalyst. The method comprises the following steps of adding the solid catalyst and a raw material aldehyde into an autoclave, wherein an addition amount of the catalyst is 1-25% by mass that of the raw material aldehyde; reacting for 4-20 h at a temperature of 80-240 DEG C and under a hydrogen pressure of 0.5-8 MPa; and finally obtaining the long-chain alcohol. The raw material aldehyde is n-butyl aldehyde or n-valeraldehyde; the long-chain alcohol is octanol or decanol; the solid catalyst is a metal-solid acid (alkali) catalyst and comprises a metal, an auxiliary agent and a solid acid (alkali), wherein a mass percentage of the metal is the catalyst is 0.5-40%; the mass percentage of the auxiliary agent is 0-10%; and the balance being the solid acid (alkali). The provided environment-friendly novel process for the one-step synthesis of the long-chain alcohol by catalyzing the aldehydes with the solid catalyst can greatly shorten a process flow for synthesizing the long-chain alcohol and reduces equipment cost and operation cost.

Description

technical field [0001] The invention relates to the technical field of green chemistry, in particular to a process method for synthesizing octanol and decanol in one step from n-butyraldehyde and n-valeraldehyde respectively with a solid catalyst, and simultaneously obtaining n-butanol and n-pentanol. Background technique [0002] Octanol (2-ethylhexanol) is an important organic chemical raw material. As an important plasticizer alcohol, it is used to synthesize octyl acrylate, dioctyl sebacate, dioctyl phthalate (DOP ) and other plasticizers. In addition, octanol is widely used as a solvent and petroleum additive with excellent performance. [0003] Decyl alcohol (2-propylheptanol) is also an important plasticizer alcohol. Compared with DOP, polyvinyl chloride products produced with diisodecyl phthalate (DIDP) plasticizer synthesized from decyl alcohol have better electrical insulation, low volatility, and are safer for humans and the environment. Has become an ideal sub...

Claims

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Application Information

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IPC IPC(8): C07C31/125C07C29/141C07C29/17
CPCC07C29/141C07C29/17C07C45/74C07C31/125C07C31/12C07C47/21
Inventor 赵新强梁宁安华良王延吉
Owner HEBEI UNIV OF TECH
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