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Preparation method for 6-amino-1-hexanol

A technology of hexanol and amino group, applied in the field of preparation of 6-amino-1-hexanol, can solve problems such as harsh reaction conditions, and achieve the effects of improving surface activity, good catalytic activity and lowering reaction temperature

Inactive Publication Date: 2018-12-11
SUZHOU GAIDE FINE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst used in this method is cheap and has high catalytic efficiency, but the reaction conditions are relatively harsh.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method of 6-amino-1-hexanol, comprising the following steps:

[0024] (1) Mix and grind nickel powder and absolute ethanol until the solvent evaporates, then disperse it in deionized water, add sodium ethylenediamine tetraacetate, stir and disperse evenly, and obtain a dispersion; wherein, nickel powder, deionized The dosage ratio of ionized water and sodium edetate is 1g: 15mL: 0.01g;

[0025] (2) dissolving cerium nitrate in deionized water and stirring and mixing to make a mass concentration of 5% cerium nitrate solution, then it is added dropwise to the dispersion made in step (1) with sodium hydroxide solution, 1500 Stir the reaction for 0.5h under the state of rpm, filter after the reaction, and dry the precipitate to obtain a catalyst precursor; wherein, the mass ratio of cerium nitrate and nickel is 0.3:2;

[0026] (3) placing the catalyst precursor prepared above in a muffle furnace at 800° C. for 1 hour, cooling to room temperature with the furn...

Embodiment 2

[0029] A preparation method of 6-amino-1-hexanol, comprising the following steps:

[0030] (1) Mix and grind nickel powder and absolute ethanol until the solvent evaporates, then disperse it in deionized water, add sodium ethylenediamine tetraacetate, stir and disperse evenly, and obtain a dispersion; wherein, nickel powder, deionized The dosage ratio of ionized water and sodium edetate is 1g: 20mL: 0.05g;

[0031] (2) dissolving cerium nitrate in deionized water and stirring and mixing uniformly to obtain a cerium nitrate solution with a mass concentration of 5-15%, and then adding it dropwise to the dispersion obtained in step (1) simultaneously with the sodium hydroxide solution , stirred and reacted for 3.5 hours at 5000 rpm, filtered after the reaction, and dried the precipitate to obtain a catalyst precursor; wherein, the mass ratio of cerium nitrate to nickel was 0.3:6;

[0032] (3) placing the catalyst precursor prepared above in a muffle furnace at 950° C. for 2 hour...

Embodiment 3

[0035] A preparation method of 6-amino-1-hexanol, comprising the following steps:

[0036] (1) Mix and grind nickel powder and absolute ethanol until the solvent evaporates, then disperse it in deionized water, add sodium ethylenediamine tetraacetate, stir and disperse evenly, and obtain a dispersion; wherein, nickel powder, deionized The dosage ratio of ionized water and sodium edetate is 1g: 15mL: 0.02g;

[0037] (2) dissolving cerium nitrate in deionized water and stirring and mixing to obtain a mass concentration of 10% cerium nitrate solution, and then adding it dropwise to the dispersion obtained in step (1) simultaneously with sodium hydroxide solution, 2000 Stir the reaction for 1 h under the state of rpm, filter after the reaction, and dry the precipitate to obtain a catalyst precursor; wherein, the mass ratio of cerium nitrate and nickel is 0.3:3;

[0038] (3) Place the catalyst precursor prepared above in a muffle furnace at 850° C. for 1.2 hours. After the treatme...

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PUM

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Abstract

The invention discloses a preparation method for 6-amino-1-hexanol. The preparation method specifically comprises the following steps: mixing nickel powder and absolute ethyl alcohol, and grinding until a solvent is completely evaporated, dispersing in deionized water, adding sodium ethylene diamine tetracetate, uniformly stirring and dispersing, and preparing dispersion liquid; enabling cerous nitrate to be dissolved in the deionized water, uniformly stirring and mixing to prepare cerous nitrate solution, and dropwise adding the cerous nitrate solution and sodium hydroxide solution to the dispersion liquid simultaneously, stirring and reacting, filtering after ending a reaction, and drying a precipitate, to obtain a catalyst precursor; enabling the catalyst precursor to be placed in a muffle furnace and treating for 1-2 h in 800-950 DEG C, after ending treatment, cooling to a room temperature along with the furnace, grinding, and preparing a cerium-containing nickel catalyst; and using 1,6-hexanediol as a raw material, feeding an ammonia gas and a hydrogen gas, reacting for 1-2 h under catalysis of the prepared cerium-containing nickel catalyst, and preparing the 6-amino-1-hexanol. The method is simple in operation, and a product yield reaches 93.5% or more.

Description

Technical field: [0001] The invention relates to the field of preparation of pharmaceutical intermediates, in particular to a preparation method of 6-amino-1-hexanol. Background technique: [0002] 6-Amino-1-hexanol is a chemical intermediate, white needle crystal at room temperature, melting point 58-60°C, boiling point 130.5-131.5°C (10.2mmHg). It contains amino groups and hydroxyl groups, has the general properties of alcohols and amines, and is widely used in the preparation of special chemicals, medicines and pesticides. [0003] The patent (201610114746.4) discloses a preparation method of 6-amino-1-hexanol using calcium carbonate as a catalyst. Using calcium carbonate as a reaction catalyst, 1,6-hexanediol, ammonia and hydrogen are mixed at a temperature of 270-290 ℃, pressure 150-180MPa, mixed heating and pressurized reaction for 1.5-2h. The catalyst used in this method is cheap and has high catalytic efficiency, but the reaction conditions are relatively harsh. ...

Claims

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Application Information

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IPC IPC(8): C07C215/08C07C213/02B01J23/83
CPCB01J23/83C07C213/02C07C215/08
Inventor 李晓明
Owner SUZHOU GAIDE FINE MATERIALS CO LTD
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