Molybdenum carbide catalyst for producing nerol and geraniol by citral hydrogenation

A catalyst, nerol technology, applied in physical/chemical process catalysts, tungsten/molybdenum carbides, carbides, etc., can solve the problem of high cost of noble metal hydrogenation catalysts, achieve low cost, high product quality, and expanded applications range effect

Active Publication Date: 2018-04-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] One of the technical problems to be solved in the present invention is the high cost of commonly used noble metal hydrogenation catalysts, providing molybdenum carbide catalysts for the hydrogenation of citral to nerol and geraniol

Method used

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  • Molybdenum carbide catalyst for producing nerol and geraniol by citral hydrogenation
  • Molybdenum carbide catalyst for producing nerol and geraniol by citral hydrogenation
  • Molybdenum carbide catalyst for producing nerol and geraniol by citral hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] 1. Catalyst preparation

[0066] Take molybdenum atomic concentration as 0.07mol / L (NH 4 ) 6 Mo 7 o 24 4H 2 0.15 L of O aqueous solution, 0.18 mol of aniline was added to the solution, and 2 mol / L of HCl solution was added dropwise under stirring until pH=2.0 to obtain material I;

[0067] Put material I at 60°C for 12 hours to obtain material II, filter, wash the filter cake with water three times with 200 mL of water each time, then wash the filter cake with absolute ethanol three times with 100 mL of ethanol each time, and finally dry the filter cake in vacuum at 60°C After 12 hours, material III was obtained.

[0068] Material III is pre-calcined and roasted under a nitrogen atmosphere: the temperature is raised from 20°C to 300°C at a rate of 5°C / min, and then raised from 300°C to 700°C at a rate of 1°C / min, and kept at 700°C 2 hours. After cooling down to room temperature and cooling for 48 hours under nitrogen protection, the desired molybdenum carbide cat...

Embodiment 2

[0078] 1. Catalyst preparation

[0079] Take molybdenum atomic concentration as 0.07mol / L (NH 4 ) 6 Mo 7 o 24 4H 2 0.15 L of O aqueous solution, 0.18 mol of 1,6-hexanediamine was added to the solution, and 2 mol / L of HCl solution was added dropwise under stirring until pH = 2.0 to obtain material I;

[0080] Put material I at 60°C for 12 hours to obtain material II, filter, wash the filter cake with water three times with 200 mL of water each time, then wash the filter cake with absolute ethanol three times with 100 mL of ethanol each time, and finally dry the filter cake in vacuum at 60°C After 12 hours, material III was obtained.

[0081] Suspend 3.39g of material III in 100mL of water, add 1.45g of APS, drop in 2mol / L HCl solution to pH=2.5 under stirring, filter, wash the filter cake with water three times with 200mL of water each time, and finally dry the filter cake in vacuum at 60°C 12 hours, got material IIIB

[0082] Material IIIB is pre-calcined and roasted in a...

Embodiment 3

[0090] 1. Catalyst preparation

[0091] Take molybdenum atomic concentration as 0.07mol / L (NH 4 ) 6 Mo 7 o 24 4H 2 O aqueous solution was 0.15 L, and 0.18 mol of tetraethylenepentamine was added to the solution, and 2 mol / L of HCl solution was added dropwise under stirring until pH=2.0 to obtain material I.

[0092] Put material I at 60°C for 12 hours to obtain material II, filter, wash the filter cake with water three times with 200 mL of water each time, then wash the filter cake with absolute ethanol three times with 100 mL of ethanol each time, and finally dry the filter cake in vacuum at 60°C After 12 hours, material III was obtained.

[0093] Material III is pre-calcined and roasted under a nitrogen atmosphere: the temperature is raised from 20°C to 300°C at a rate of 5°C / min, and then raised from 300°C to 700°C at a rate of 1°C / min, and kept at 700°C 2 hours. After cooling down to room temperature and cooling for 48 hours under the protection of nitrogen, the des...

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Abstract

The invention discloses a molybdenum carbide catalyst for producing nerol and geraniol by citral hydrogenation. The XRD diffraction spectrogram of the molybdenum carbide catalyst has one characteristic of the following four groups of characteristics according to the difference of 2theta: 36-38 degrees, 41-43 degrees, 61-63 degrees and 73-75 degrees; 34-35 degrees, 37-38 degrees, 39-40 degrees, 51-53 degrees, 61-63 degrees, 69-71 degrees, 72-73 degrees, 74-75 degrees and 75-76 degrees; 36-39 degrees, 42-44 degrees, 62-65 degrees and 74-77 degrees; and 25-27 degrees, 34-35 degrees, 36-37 degrees, 37-39 degrees, 39-41 degrees, 51-53 degrees, 53-54 degrees, 61-63 degrees, 68-70 degrees, 71-73 degrees, 73.5-75 degrees and 75-77 degrees.

Description

technical field [0001] The invention relates to a molybdenum carbide catalyst used for hydrogenation of citral to prepare nerol and geraniol and application thereof. Background technique [0002] Citral (citral) is an important α, β-unsaturated aldehyde with two geometric isomers: geranial (trans, citral A) and neral (cis, citral B), The citral contained in citronella oil is mainly citral B. The unsaturated alcohols of its selective hydrogenation products are nerol and geraniol (cis / trans-3,7-dimethyl-2,6-octadien-l-ol), which are two valuable spices and pharmaceutical intermediates. It has wide application value in flavor, medicine and other industries (Li Qiugui, Liu Yingxin, Wang Guilin, etc. Research progress of citral selective hydrogenation catalysts for nerol / geraniol synthesis[J]. Modern Chemical Industry, 2007( S2):32-36.), so in recent years, the selective catalytic hydrogenation of citral to the synthesis of nerol and geraniol has been widely concerned and explo...

Claims

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Application Information

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IPC IPC(8): B01J27/22C01B32/949C07C29/141C07C33/02
CPCC07C29/141B01J27/22C07C33/02
Inventor 甘泉马宇春刘仲能刘旭
Owner CHINA PETROLEUM & CHEM CORP
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