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
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[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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