Method for preparing linalool from dehydrolinalool through selective hydrogenation

A dehydrolinalool and selective technology, applied in hydrogenation preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of increasing residence time and increasing the complexity of production equipment operation process , Increase the complexity of production equipment and operating processes, etc., to achieve the effect of improving the space-time yield

Inactive Publication Date: 2012-04-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the fixed-bed catalyst bed formed by such a material and a carrier with such a structural shape obviously cannot obtain an ideal catalyst load, which directly affects the space-time yield. For the technical solution disclosed in the above-mentioned Chinese patent 96110670.0, the space-time yield is only 0.31hr -1
Increasing the reaction residence time seems to be able to properly compensate for this defect. For example, the technical solution disclosed in the above-mentioned Chinese patent 00131057.7 adopts a two-stage series connection method to complete the entire hydrogenation process, and the space-time yield reaches 1.01hr. -1 However, this obviously leads to a great increase in the complexity of the production equipment and operation process
In addition, adding a certain amount of CO to hydrogen to inhibit the occurrence of deep hydrogenation and ensure the long-term stability of catalyst performance also has obvious defects, which further increases the complexity of production equipment and operating processes.

Method used

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  • Method for preparing linalool from dehydrolinalool through selective hydrogenation
  • Method for preparing linalool from dehydrolinalool through selective hydrogenation
  • Method for preparing linalool from dehydrolinalool through selective hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1~10

[0036] The carrier slurry is prepared from aluminum hydroxide powder, then shaped and granulated, and then roasted at 500-1100°C for 2-5 hours to obtain a particle size range of 3-5mm and a BET specific surface area range of 50- 150m 2 / g spherical Al 2 o 3 carrier.

[0037] Take the required ratio of palladium chloride, lead nitrate and bismuth nitrate to prepare impregnation solution, and then impregnate Al 2 o 3 The carrier is placed in the impregnation solution and stirred evenly. Standing and aging for 10-15 hours, drying and roasting to obtain the catalyst precursor. The firing temperature is controlled at 400-600° C., and the firing time is controlled at 2-3 hours.

[0038] The catalyst precursor is impregnated with an equal volume of sodium ethylenediamine tetraacetate (EDTA) aqueous solution, and the concentration of EDTA in the aqueous solution is controlled at 0.3-3.0 wt.%. Subsequently, the catalyst precursor with adsorbed EDTA was dried, and directly loaded...

Embodiment 11~26

[0045] Obtain a fixed-bed reactor according to Examples 1-10. Under the condition of continuously feeding hydrogen, the reactor is lowered to the temperature required for the reaction, and the hydrogen pressure is adjusted. C2-C4 aliphatic alcohol is used as a solvent, the solvent and dehydrolinalool are mixed according to the required ratio (solvent ratio), and then the liquid phase passes through the catalyst bed, and the continuous hydrogenation reaction is carried out to prepare linalool while maintaining suitable reaction conditions.

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Abstract

The invention discloses a method for preparing linalool from dehydrolinalool through selective hydrogenation. The method is characterized in that dehydrolinalool and a solvent are mixed and the liquid mixture passes through a fixed bed catalyst layer in a hydrogen atmosphere and undergoes a hydrogenation reaction, wherein the solvent is C2-C4 fatty alcohol; a solvent ratio is 1: (0.5 to 1.2); a liquid hourly space velocity is in a range of 2.0 to 2.5h*r<-1>; catalyst carriers are Al2O3 particles; a particle size is in a range of 3 to 5 millimeters; and active components comprise Pd, Pb and Bi. The method comprises the following steps that the active components of Pd, Pb and Bi are loaded on the catalyst carriers through immersion and high-temperature calcination to form catalyst precursors; sodium ethylene diamine tetracetate is adsorbed on the catalyst precursors through an immersion method; and catalyst finished products are obtained through reduction activation treatment in a hydrogen atmosphere. The method for preparing linalool from dehydrolinalool through selective hydrogenation has the advantages that preparation is convenient; a preparation cost is low; other deep hydrogenation side reaction inhibition processes are avoided; a conversion rate and product selectivity reach ideal levels; and a space-time yield is obviously improved.

Description

technical field [0001] The invention relates to a method for selectively hydrogenating acetylenic bond-containing compounds to prepare corresponding ethylenic bond-containing compounds, in particular to the use of Al as a carrier 2 o 3 , the active component includes the supported fixed-bed catalyst of metal Pd, Pb and Bi, the method for preparing linalool by the selective hydrogenation of dehydrolinalool. Background technique [0002] Linalool has high economic value, and it can be used as a raw material for the preparation of high-grade spices or essences, and is also an important intermediate for the synthesis of vitamin E and vitamin A. The preparation of linalool from the separated products of petroleum C5 fractions via 6-methyl-5-hepten-2-one and dehydrolinalool is an important process route for artificially synthesizing linalool at present. The main and side reactions of dehydrolinalool through selective hydrogenation to linalool are shown in the following formulas ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/644C07C33/02C07C29/17
Inventor 朱志庆吕自红郭世卓谢家明杜宇
Owner CHINA PETROLEUM & CHEM CORP
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