Molybdenum, nickel, phosphorus soaking solution and preparation thereof

A technology of impregnating solution and solution, which is applied in the field of impregnating solution used in hydroprocessing catalysts and its preparation, which can solve the problems of metal deposition, strong interaction, loss of carrier specific surface area, etc., and achieve high catalyst activity, stable solution properties, and strong force Appropriate effect

Active Publication Date: 2008-10-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN 93109141.1 pointed out that when the solution used contains ammonia solution of molybdenum and cobalt (nickel) at the same time, the impregnating solution is alkaline, if it is to be impregnated once to make a catalyst, it needs to be made into a very high concentration of molybdenum-cobalt (nickel)-ammonia solution , this solution is unstable and brings difficulties to the impregnation operation
[0005] Hydrotreating catalysts mostly use γ-Al 2 o 3 As a carrier, its isoelectric point is 7-9, and the pH value of commonly used Mo, Ni, and P impregnating solutions is mostly <2, which is much lower than the isoelectric point of the carrier, which makes the active components in the impregnating solution interact with the carrier. The effect is too strong, which is not conducive to the uniform dispersion of active metals, and the pH value is too small will also cause the specific surface area of ​​the carrier to be lost during the impregnation process
However, if the pH value of the acidic impregnation solution is too high, metals will be deposited on the surface of the carrier during impregnation, and the active components in the catalyst will not be uniformly dispersed, which will affect the performance of the catalyst.

Method used

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  • Molybdenum, nickel, phosphorus soaking solution and preparation thereof

Examples

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Embodiment 1

[0014] This example introduces the preparation method of Mo, Ni, P original solution. In this example, only Mo, Ni, and P original solutions with one concentration and ratio are prepared. According to the method described, Mo, Ni, and P original solutions with other ratios and concentrations can be prepared as required, so as to prepare the desired target solution.

[0015] Get a certain amount of molybdenum oxide and basic nickel carbonate into a multi-necked flask, add a certain amount of deionized water, stir until the substance in the bottle is slurry, then slowly add a certain amount of phosphoric acid (weight concentration 85%) After the initial reaction, heat slowly, and keep the solution temperature at 90-110° C. for 1-3 hours (choose the holding time according to the transparency of the solution). After the heating was stopped, the obtained solution was filtered while it was hot, and after some insoluble impurities were filtered out, a clear dark green original soluti...

Embodiment 2

[0019] This example introduces the addition of ammonia solution of EDTA to the original solution to prepare target solutions with different pH values.

[0020] First prepare the ammonia solution of EDTA, weigh 100g EDTA and put it into a round bottom flask, add 50ml water and 70g concentrated ammonia water respectively (concentrated ammonia water contains NH 3 The mass percent concentration is about 26% to 28%), stirring and dissolving at room temperature.

[0021] Put a certain volume of original solution of Mo, Ni, and P into a beaker, and slowly add the ammonia solution of EDTA dropwise under the condition of constant stirring, pay attention to the dropping speed not too fast, so as not to generate stable insoluble matter. Measure the pH value of the solution in time with a pH meter, stop dropping the EDTA solution when the required pH value is reached, and continue stirring until the flocs in the solution are completely dissolved. Finally, an appropriate amount of water w...

Embodiment 3

[0025] In this embodiment, the ammonia solution of NTA is added to the original solution to prepare target solutions with different pH values.

[0026] Preparation of ammonia solution of NTA: Weigh 100g NTA and put it into a round bottom flask, add 50ml water and 100g concentrated ammonia water respectively (concentrated ammonia water contains NH 3 The mass percent concentration is about 26% to 28%), stirring and dissolving at room temperature.

[0027] The method of adding the NTA solution in the original solution is as in Example 2, and Table 3 provides the preparation parameters of two groups of pH Mo, Ni, and P solutions. The concentration of each substance (metal concentration is calculated as oxide) in the target solution 4 is: MoO 3 is 64.9g / 100ml, NiO is 10.9g / 100ml, and P is 1.8g / 100ml; the concentration of each substance in the target solution 5 (the metal concentration is calculated as oxide) is: MoO 3 30.2g / 100ml, NiO 5.1g / 100ml, P 0.8g / 100ml

[0028] Table 3 Ex...

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Abstract

The present invention relates to a dipping solution containing molybdenum (Mo), nickel (Ni) and phosphor (P) and a preparation method thereof. The concentration for each matter in the solution is: 10 to 90g/100ml of MoO3, 1 to 18g/100ml of NiO and 0.5 to 5g/100ml of P. The solution is mainly characterized by changing the pH value of the solution between 2 to 6 by adding nitrogen compound into an acid dipping solution. The dipping solution provided by the present invention with a high pH value and good stability, can be used for the preparation of various hydrogenation catalysts, weaken the coactions between active components and a carrier and reduce the loss of the specific surface of the catalyst caused by high acidity of the dipping solution.

Description

technical field [0001] The invention relates to an impregnating solution and a preparation method thereof, in particular to an impregnating solution used for hydrogenation catalysts and its preparation. Background technique [0002] Most supported catalysts are prepared by impregnation method, such as various hydrogenation catalysts. When the hydrogenation catalyst is prepared by the impregnation method, the pH value of the impregnation solution has a great influence on the structure, dispersibility and degree of dispersion of the active metal (such as Mo) on the surface of the catalyst and its interaction with the carrier (such as Al 2 o 3 ) have a great influence on the interaction. The increase of the pH value can reduce the loss of the specific surface area of ​​the carrier during the impregnation process and increase the specific surface area of ​​the catalyst. [0003] In general, there are two types of impregnating solutions for hydrogenation catalysts: one is the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/19B01J37/02
Inventor 杨占林彭绍忠姜虹刘雪玲
Owner CHINA PETROLEUM & CHEM CORP
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