Ruthenium-modified Ir/C catalyst and preparation method thereof, as well as application to citral hydrogenization

A catalyst, citral technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve the problem that reactivity, selectivity and stability cannot be balanced at the same time, The preparation process is complicated, the product is difficult to separate, etc., and the effect of reducing the cost of precious metals, high reactivity, and mild process conditions is achieved.

Active Publication Date: 2017-06-13
JIANGXI HANS PRECIOUS METALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation method of this technical solution has problems such as complex preparation process, relatively harsh operating conditions, and difficult separation of products, especially its reactivity, selectivity and stability cannot be taken into account at the same time.

Method used

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  • Ruthenium-modified Ir/C catalyst and preparation method thereof, as well as application to citral hydrogenization
  • Ruthenium-modified Ir/C catalyst and preparation method thereof, as well as application to citral hydrogenization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Step (a), the treatment of activated carbon, activated carbon with 5%HNO 3 The solution was stirred at 80°C for 4h, then washed with deionized water until neutral;

[0038] Step (b), according to the active component iridium loading 5.0%, prepare iridium solution;

[0039] Step poly (c), get the activated carbon 5g of step (a), adopt equal volume impregnation method to impregnate the iridium solution prepared. Stand in a water bath at 40°C for 8 hours, and dry at 100°C for 4 hours to obtain the Ir / C catalyst precursor;

[0040] Step (d), use 5wt% sodium hydroxide aqueous solution to adjust the pH value of the precursor to 10, and leave it to age for 8 hours;

[0041] Step polymerization (f), at 100°C, put into the autoclave, under the pressure of 2MPa, reduce for 2h, cool, filter, and wash with deionized water until there is no chloride ion, then the Ir / C catalyst can be obtained.

Embodiment 2

[0043] Step (a), the treatment of activated carbon, activated carbon with 5%HNO 3 The solution was stirred at 80°C for 4h, then washed with deionized water until neutral;

[0044] Step (b), according to the active component iridium loading 4.0%, ruthenium loading 1.0%, prepare iridium solution and ruthenium solution respectively;

[0045] Step poly (c), get the activated carbon 5g of step (a), adopt equal volume impregnation method to impregnate the prepared iridium solution and ruthenium solution. Stand still in a water bath at 40°C for 8 hours, and dry at 100°C for 4 hours to obtain the Ir-Ru / C catalyst precursor;

[0046] Step (d), use 5wt% sodium hydroxide aqueous solution to adjust the pH value of the precursor to 10, and leave it to age for 8 hours;

[0047]Step (f), reduce the above solution with sodium borohydride solution, the amount is more than 100% of the theoretical amount, reduce for 2h, cool, filter, and wash with deionized water to get 4%Ir-1%Ru / C catalyst....

Embodiment 3

[0049] Step (a), the treatment of activated carbon, activated carbon with 5%HNO 3 The solution was stirred at 80°C for 4h, then washed with deionized water until neutral;

[0050] Step polymerization (b), according to active component iridium load 3.0%, ruthenium load 2.0%, prepare iridium solution, ruthenium solution;

[0051] Step poly (c), get the activated carbon 5g of step (a), adopt equal volume impregnation method to impregnate the prepared iridium solution and ruthenium solution. Stand still in a water bath at 40°C for 8 hours, and dry at 100°C for 4 hours to obtain the Ir-Ru / C catalyst precursor;

[0052] Step (d), use 5wt% sodium hydroxide aqueous solution to adjust the pH value of the precursor to 10, and leave it to age for 8 hours;

[0053] Step (f), reduce the above solution with sodium borohydride solution, the amount is more than 100% of the theoretical amount, reduce for 2h, cool, filter, and wash with deionized water to get 3%Ir-2%Ru / C catalyst.

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Abstract

The invention discloses preparation of a ruthenium-modified Ir/C catalyst and application of the ruthenium-modified Ir/C catalyst to citral hydrogenization. The catalyst comprises an active carbon carrier, and an active component comprises Ir nano particles and Ru nano particles, wherein the carrying capacity of the Ir nano particles is 1.0 to 5.0 percent, and the carrying capacity of the Ru nano particles is 0 to 4.0 percent. The invention further discloses a preparation method of the ruthenium-modified Ir/C catalyst. The preparation method comprises the following steps: firstly, treating active carbon through nitric acid, then carrying the active component including iridium and auxiliary ruthenium to obtain a catalyst precursor, and carrying out drying and reducing. As Ru replaces part of Ir, the catalyst disclosed by the invention is lower in cost, and also has higher catalysis activity and selectivity; furthermore, the catalyst can be used indiscriminately for multiple times, so that the production cost is reduced. When the catalyst is applied to citral hydrogenization to synthesize nerol, the raw material conversion rate is 100 percent, and the nerol/geraniol selectivity is up to 98.0 percent; the reaction process is mild in condition, and can completely meet the industrial production requirement.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation and catalytic hydrogenation, and in particular relates to a ruthenium-modified Ir / C catalyst, its preparation method and its application in citral hydrogenation. Background technique [0002] Citral is a typical α,β-unsaturated aldehyde, which has important application value in industries such as spices and pharmaceutical intermediates. Its selective hydrogenation product unsaturated alcohols (nerol and geraniol) are two kinds of Precious spices and pharmaceutical intermediates are widely used in the formulation of high-end flavors in diet, food, and daily chemicals. [0003] The citral molecule contains isolated C=C double bonds, C=O bonds and carbonyl-conjugated C=C double bonds that can be hydrogenated. Hydrogen is only added to the C=O double bond but not to the C=C double bond. For nerol or geraniol, the bond energy of the C=C bond is less than the C=O bond in thermodynamics, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46C07C29/141C07C33/02
CPCB01J23/468B01J35/006C07C29/141C07C33/02
Inventor 卢新宁郁丰善何治鸿相亚波赵栋云李永敏程龙高艳妮谢永荣华德润李剑李阳明
Owner JIANGXI HANS PRECIOUS METALS CO LTD
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