Method of preparing catalyst for dehydration of paraffinic hydrocarbons

FIELD: chemistry.

SUBSTANCE: described is method of catalyst preparation, which consists in impregnation of product of thermochemical activation of hydrargillite by active components under microwave radiation with operating frequency 2.46 GHz and power 180-900 Wt for 3-30 min with the following drying in electromagnetic field of ultrahigh-frequency range and incineration at temperature from 600 to 800°C.

EFFECT: increase of method productivity, high mechanical strength and thermal stability of catalyst, increase of catalytic properties.

2 tbl, 4 ex

 

The invention relates to the field of oil refining and catalytic chemistry, in particular to a method of synthesis of a catalyst for the dehydrogenation of light paraffin hydrocarbons, preferably isobutane and isopentane, for production of isobutylene and isoamylenes - monomers of synthetic rubbers.

Known impregnation method for the synthesis of the catalyst in the dehydrogenation of paraffins, which is impregnated alumina carrier with the desired properties of the solution of active components and promoters and subsequent heat treatment (drying and calcining of the catalyst). Stage drying is conducted in a traditional way in the laboratory on a sand bath or in an oven, in industry - in apparatus with stirrer, equipped with a steam jacket [Karimov O. H. investigation of the drying process alimohammadi catalyst in the electromagnetic field of the microwave range / Karimov O. H., Damini P. P., Kasyanov L. H., Karimov, E. H., Vakhitova P. P. // Oil and gas business: electronic scientific journal. No. 4, 2013. - 291-301 http://www.ogbus.ru/authors/KarimovOKh/KarimovOKh_l.pdf].

The disadvantage of drying by convective method are the high energy costs associated with the creation of heat in the reaction zone, and the duration of the stage of drying.

A method of obtaining oxide catalysts, which consists in mixing two or more salts of predshestvennikami catalyst, melting the mixture until a homogeneous melt, cooling the melt to room temperature, the decomposition of the molten salt to the oxide under the action of microwave radiation and subsequent calcination [RF Patent №2301705 C1, B01J 37/34, B01J 35/12, B01J 23/10, B01J 23/70, publ. 27.06.2007].

Known chemical method of obtaining alimohammadi catalyst for dehydrogenation of hydrocarbons. This method includes a heat treatment of the raw materials taken in the form of powders of aluminum and chromium carbonyl in air flow low-temperature microwave plasma, and the reagents are served in the flow of air plasma and the reactor separately in the form of an aerosol carrier gas argon [RF Patent №2347613 C1, B01J 37/34, B01J 21/04, B01J 23/26, B82B 3/00, publ. 27.02.2009]. Or to get alimohammadi catalyst in a stream of microwave plasma fused oxides of aluminum and chromium [RF Patent №231.8597 from 10.03.2008].

The disadvantage of these methods is the technical complexity of the process, including, including additional stages of oxidative processing reagents fused catalyst, evaporation of the excess reagent, drying and calcination of the catalyst.

There is a method of preparation of the catalyst for dehydrogenation of paraffin hydrocarbons by impregnation [RF Patent 2432203 C1, B01J 23/26, B01J 21/04, B01J 23/02, B01J 23/745, B01J 21/10, C07C 5/333, publ. 27.10.201]. The process of preparation of the catalyst involves the impregnation product thermochemical activation hydrargillite solutions of chromium compounds, alkali metal, iron, calcium, magnesium, drying and calcination at a temperature of 650-800°C. Mainly impregnation takes place simultaneously all the components of the catalyst capacity at a temperature of 20-50°C.

The disadvantage of this method is the duration of the stages of impregnation and drying is carried out at 120°C, which is up to 4 hours, which leads to high energy costs.

The closest technical solution to the present method of preparation of the catalyst is a method based upon the use of electromagnetic radiation in the microwave range at the stage of drying alimohammadi catalyst [Karimov O. H., Damini P. P., Kasyanov L. H., Karimov, E. H. the Use of microwave radiation in the preparation of metal oxide catalysts // Fundamental research. - 2013. No. 4. - S. 801-805]. The catalyst was impregnated with a solution of active ingredients, dried under the action of electromagnetic radiation in order to intensify the drying process.

The disadvantage of this method is the duration of the stage of impregnation of the catalyst due to diffusion processes on the catalyst surface. The duration of the impregnation, providing uniform distribution with the joining of chromium and potassium, may take up to 1 hour.

Problem to be solved in the invention is to develop a method of producing a catalyst for dehydrogenation of paraffin hydrocarbons, which improves the physico-chemical and catalytic properties of the catalyst and increases the productivity of its preparation impregnation method by intensifying stage of impregnation of the carrier with a solution of active components.

To solve the problem in the preparation method of catalyst for dehydrogenation of paraffin hydrocarbons by impregnation product thermochemical activation hydrargillite solutions of chromium compounds and alkali metal, followed by drying electromagnetic radiation and calcination of the catalyst according to the invention stage impregnation carried out under the action of electromagnetic radiation at the operating frequency of 2.45 GHz and power 180-900 W within 3-30 minutes

Product thermochemical activation hydrargillite, which is a carrier for the catalyst and the precursor of aluminium oxide, obtained by dehydration under conditions of pulsed heating hydrargillite Al(OH)3. The product has high reactivity, and is easily hydrated in the presence of water or vapor environment with the formation of aluminum hydroxide patterns AlOOH. This connection has a high reaction capable of the flesh, as a result of which it becomes possible the impregnation of the carrier based on the product of thermochemical activation hydrargillite compounds active catalyst components. In the impregnation compounds of chromium and alkali metal not only evenly distributed in the alumina, but also chemically bound with the compound of aluminium. The use of microwave effects on heterogeneous catalysts in the process of their preparation allows in some cases to obtain catalysts with a more uniform particle distribution. So, processing of the electromagnetic field of the dried catalyst for the synthesis of ethylene oxide allows to obtain a fine distribution of silver ions on the catalyst surface [Patent US 8017546 13.09.2011].

In the process of impregnation of the carrier in the electromagnetic field of the media is heated to 110°C, which accelerates the diffusion of active components on the catalyst surface. Drying of the catalyst is conducted in the electromagnetic field of the microwave range. Preferably the use of microwave radiation with a frequency of 2.45 GHz. The radiation power is 10-2000 W, preferably 180-900 W, the duration of radiation up to 30 minutes to complete removal of the aqueous solvent from the catalyst.

In the preparation of the catalyst in the electromagnetic field of the microwave range maximum is W hen operations of impregnation and drying of the catalyst is reduced from 4 hours to 1 hour. It was also established that lomography the catalyst prepared by this method have high catalytic performance (activity and selectivity), mechanical strength and thermal stability.

The resulting catalyst was tested in a laboratory reactor at 50 cm3in the process of dehydrogenation of isopentane at a temperature of 550°C, at a space velocity of isopentane 1 hour-1(liquid). The catalytic cycle consists of the reaction phase, in which the hydrocarbons are served within 30 minutes; phase purging with nitrogen for 10 minutes to release the catalyst from the adsorption of the reaction products of dehydrogenation; regeneration phase, when in the regenerator the gas is fed to the regeneration air for 30 minutes at a temperature of 650°C.

In the analysis of catalysts using the following methods.

Thermal stability of the catalyst test using Express methods by annealing at 800°C for 4 hours. The abrasion resistance is determined by the fraction of total mass loss during abrasion of the catalyst particles. The method is based on the destruction of the catalyst particles in the fluidized layer and measuring the mass of particles carried by the air flow, the speed of which is stabilised.

The invention is illustrated by the following examples.

Example 1 (the prototype)./p>

For the preparation of the catalyst compound of aluminum (product of thermochemical activation hydrargillite) in the form of microspherical powder impregnated with constant stirring a solution containing chromic anhydride and potassium lye. All components taken in such quantities, to ensure that after calcination the catalyst composition, wt.% (in terms of oxides: chromium oxide (in terms of Cr2O3) 13,0; the oxide of the alkali metal 2; aluminium oxide - rest. The impregnation is carried out at room temperature for 1 hour, followed by drying in an electromagnetic field with a frequency of 2.45 GHz, power irradiation 900 watts for 3 minutes. The dried catalyst is calcined at a temperature of 660°C for 6 hours. Physico-chemical and catalytic properties of the catalyst are presented in table 1. Comparative results of thermal stability of the catalysts are presented in table 2.

Example 2.

The catalyst is prepared analogously to example 1, with the difference that the impregnation solution active components are under the influence of electromagnetic field frequency of 2.45 GHz, the radiation power of 180 watts for 5 minutes. Physico-chemical and catalytic properties of the catalyst are presented in table 1. Comparative results of thermal stability of the catalysts are presented in table 2.

Example 3.

Catalysis is tor is prepared analogously to example 1, with the difference that the impregnation solution active components are under the influence of electromagnetic field frequency of 2.45 GHz, the radiation power of 180 watts for 10 minutes. The dried catalyst was calcined at 700°C for 6 hours. Physico-chemical and catalytic properties of the catalyst are presented in table 1. Comparative results of thermal stability of the catalysts are presented in table 2.

Example 4.

The catalyst is prepared analogously to example 3, with the difference that the impregnation solution active components are under the influence of electromagnetic fields 22 minutes. Physico-chemical and catalytic properties of the catalyst are presented in table 1. Comparative results of thermal stability of the catalysts are presented in table 2.

91,2
Table 1
Physico-chemical and catalytic properties
IndicesExample 1Example 2Example 3Example 4
Abrasion, %90,192,0to 92.1
The content in the catalyst Cr+6, wt.%the 4.75,24,84,3
Activity* catalyst in the process44,648,143,040,1
dehydrogenation of isopentane, %
Selectivity* catalyst in dehydrogenation of isopentane, %82,187,180,682,5
* Catalytic performance output unsaturated hydrocarbon, C5.

Table 2
The results of Express-methods for determining thermal stability of the catalysts
A sample of catalystThe content of Cr6+, wt.%Loss of Cr6+after the rosalki, %
SourceAfter calcination 800°C, 4 h
Example 14,83,025,9
Example 25,24,324,8
Example 34,83,723,0
Example 44,33,425,2

A method of producing a catalyst for dehydrogenation of paraffin hydrocarbons by impregnation product thermochemical activation hydrargillite solutions of chromium compounds and alkali metal, followed by drying electromagnetic radiation and calcination of the catalyst, characterized in that the stage of impregnation carried out under the action of electromagnetic radiation at the operating frequency of 2.45 GHz and power 180-900 W within 3-30 minutes



 

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1 tbl, 2 dwg, 3 ex

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