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P-nitrotoluene hydrogenated ruthenium-lanthanum double metal catalyst and preparation method thereof

A bimetallic catalyst and p-nitrotoluene technology, which is applied in the preparation of amino compounds, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problem of uneven radial distribution of active component content, loss of active component, low stability, etc. problem, to achieve the effect of high selectivity, good stability and simple synthesis method

Inactive Publication Date: 2017-07-18
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Abstract
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AI Technical Summary

Problems solved by technology

The excess reducing agent self-decomposes, which prevents the reduction of metal ions deposited in the deep pores of the carrier, resulting in a decrease in the content of active components and uneven radial distribution
[0005] CN101439285A discloses a kind of preparation method that is used for carrying out catalytic hydrogenation to nitro compound and prepares the catalyst of corresponding amino compound, the nickel / diatomite catalyst active component content that this method prepares is too high, although it has certain effect in reducing tar Effective, but the loss of active components is not high, the stability is not high
[0006] Sasson et al. studied the reduction of nitrobenzene and found that the aromatic ring can be reduced with formic acid and palladium-carbon system. Under the protection of nitrogen, the methanol solution of 2 mmol of p-nitrotoluene, Pd / C 50 mg and 0.5 ml of formic acid was at room temperature Stir for 70 h, the obtained precipitate is extracted with ester, and the final product is separated by capillary column chromatography to obtain 48% p-methylcyclohexylamine, and the product yield is too low (Sasson, Tetrahedron lett, 1992, 49:7477)

Method used

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  • P-nitrotoluene hydrogenated ruthenium-lanthanum double metal catalyst and preparation method thereof
  • P-nitrotoluene hydrogenated ruthenium-lanthanum double metal catalyst and preparation method thereof
  • P-nitrotoluene hydrogenated ruthenium-lanthanum double metal catalyst and preparation method thereof

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Experimental program
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preparation example Construction

[0026] The preparation method of p-nitrotoluene hydrogenation ruthenium-lanthanum double metal catalyst, its steps are:

[0027] (1) Prepare a solution with a concentration of 0.3-3.0 mol / L of the soluble compound of the active component Ru with distilled water, add a carrier to the prepared solution, and immerse under strong stirring for 1-5 h to obtain a solution;

[0028] (2) The soluble compound of auxiliary agent lanthanum is formulated into B solution with a concentration of 0.3~3.0 mol / L;

[0029] (3) Add the prepared B solution directly to the A solution to obtain the C mixed solution, and continue aging for 2-10 h after adding;

[0030] (4) The precipitating agent is made into D solution with a concentration of 0.5~3.0 mol / L;

[0031] (5) Add the prepared solution D to the mixed solution C dropwise. During the dropping process, the reaction temperature is kept at 40-80 °C, and the aging is continued for 5-20 h after the addition;

[0032] (6) Filter and wash the sam...

Embodiment 1

[0041]Example 1: Weigh 0.3 g of ruthenium chloride hexahydrate and dissolve it in 70 ml of distilled water. After it is completely dissolved, add 5.7 g of HY molecular sieves and soak it at 70°C for 1 h, then dissolve 0.01 g of lanthanum oxide in 15 ml of distilled water Add the above mixed solution to continue stirring and impregnating for 9 h, then add 0.05mol / L urea aqueous solution dropwise, continue aging for 14 h, filter and wash, then dry at 100 °C for 10 h, and then dry at 120 °C for 10 h Grind the dried catalyst to 200 mesh, and reductively activate the obtained catalyst. The conditions are: reduce with hydrogen (hydrogen pressure: 0.1-2.0 MPa) at 500 °C for 3 h, and then drop to room temperature under the protection of high-purity nitrogen. The obtained catalyst sample was recorded as 1# catalyst, and 0.5 g of catalyst 1# was taken for activity evaluation.

Embodiment 2

[0042] Example 2: Weigh 0.3 g of ruthenium oxide and dissolve it in 70 ml of distilled water. After it is completely dissolved, add 5.7 g of NaY molecular sieve, soak it at 60°C for 2 h, then dissolve 0.02 g of lanthanum chloride in 20 ml of distilled water, Add to the above mixed solution and continue to stir and impregnate for 5 h, then add dropwise 0.04 mol / L potassium carbonate aqueous solution, continue to age for 17 h, filter and wash, then dry at 95°C for 12 h, and then dry at 110°C for 12 h , the dried catalyst was ground to 200 mesh, and the obtained catalyst was reductively activated under the following conditions: reducing with hydrogen (hydrogen pressure: 0.1-2.0 MPa) at 480 °C for 3 h, and then cooling down to room temperature under the protection of high-purity nitrogen. The obtained catalyst sample was recorded as 2# catalyst, and 0.5 g of catalyst 2# was taken for activity evaluation.

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Abstract

The invention relates to a p-nitrotoluene hydrogenated ruthenium-lanthanum double metal catalyst and a preparation method thereof. The catalyst comprises an active ingredient ruthenium, an auxiliary agent lanthanum and a carrier. The catalyst is shown by x%Ru-y%La / carrier, in which x% represents percentage by mass of Ru in the catalyst, y% represents percentage by mass of La in the catalyst, and the catalyst comprises the following components in percentages by mass: 0.5-5% of Ru, 0.2-2% of La and the balance of carrier. The precursor of the catalyst is prepared by means of an impregnating-precipitating method and is reduced in a hydrogen-containing atmosphere to obtain the p-nitrotoluene hydrogenated ruthenium-lanthanum double metal catalyst. In a reaction of preparing p-methyl-cyclohexylamine by p-nitrotoluene hydrogenation, p-methyl-cyclohexylamine will be strongly adsorbed on the catalyst so as to generate a lot of tar to inhibit the reaction; and by adding lanthanum, the problem that the catalyst strongly adsorb p-methyl-cyclohexylamine is solved well, and the generating amount of tar is reduced.

Description

technical field [0001] The invention relates to a hydrogenation catalyst and a preparation method thereof, in particular to a hydrogenation catalyst for p-nitrotoluene. Background technique [0002] P-methylcyclohexylamine is mainly used in the fields of medicine, automobiles, papermaking and catalysis, such as for the synthesis of some drugs that improve human immunity. Secondly, as an intermediate, it is also an inhibitor of spermidine It can be used in the preparation of zeolite catalyst in the catalytic industry; as a good binder component, it can also be used in the retreading of automobile tires and the repair of factory conveyor belts; it can also be used in bleaching pulp and waste paper in the paper industry. In addition, p-methylcyclohexylamine is an intermediate for the production of a new generation of sulfonyl hypoglycemic drug glimepiride, and with widespread attention and attention at home and abroad, it will have broad prospects. At present, there are two ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/12B01J29/74B01J29/44C07C209/36C07C211/35
CPCB01J29/126B01J29/44B01J29/74B01J2229/18C07C209/36C07C211/35
Inventor 李贵贤李红伟季东
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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