The method of preparation of the catalyst for conversion of hydrocarbons

 

(57) Abstract:

The invention relates to the production of catalysts for conversion of hydrocarbons. The method of preparation of the catalyst for conversion of hydrocarbons includes the preparation of a carrier by mixing alumina, aluminum hydroxide, technical aluminate calcium, graphite, introduction aqueous plasticizing burnable additives, molding, the crop has wilted in the air, the heat media in the environment of water vapor, high temperature annealing, subsequent impregnation of the support with solutions of nitrates of Nickel and aluminum, drying and heat treatment of the catalyst mass, and heat treatment of the carrier are in an autoclave at a pressure of water vapor of 1 to 2 ATM and 150 - 170C for 1.0 to 1.5 hours, subsequent drying is carried out at the following mode: the temperature in the drying zone lift with a speed of 40 - 60oC to 120oC and at this temperature the media stand at 1.5 - 2.0 h, and the impregnation of the calcined carrier implement solutions of nitrates of Nickel and aluminum, taken in the mass ratio (4,0 - 5,0) : 1 in terms of Nickel oxide and aluminum oxide. At the same time as plasticizing burnable supplements use the sodium carboxymethyl cellulose is the doctrine of the catalyst, to improve the specifications and appearance of final product, ensuring high activity of the catalyst during long-term operation. 1 C.p. f-crystals.

The invention relates to the production of catalysts for conversion of hydrocarbons, in particular, for process steam, steam-air and propakistani the conversion of natural gas to receive the process gas used in the production of ammonia, methanol, organic acids, and can be used in chemical, petrochemical and other industries.

There is a method of preparation of the catalyst for conversion of hydrocarbons by mixing aluminum oxide, pre-dispersible in water, with calcium aluminates, adding plasticizing burnable additive is a mixture of glycerin and polyvinyl alcohol, molding the resulting mass, drying, calcination, impregnation of the carrier with a solution of Nickel nitrate, drying and calcination of a catalyst mass [SU 1502078 A1, class B 01 J 37/04, publ. 23.08.89].

There is a method of preparation of the catalyst for conversion of hydrocarbons, including the preparation of a carrier by mixing the calcium aluminate containing from 0.2 - 10 wt.% titanium dioxide with HYDR it in an oxidizing atmosphere at a temperature of 1100 - 1600oC, impregnation of the carrier with solutions of Nickel and aluminum, drying, heat treatment [EP 0279389 A1, class C 01 3/40, publ. 24.08.88].

Used for preparation of media aluminate calcium corresponds rentgenograficheski hibonite - CaO 6Al2O3.

Also known preparation method of catalyst for steam reforming of lower hydrocarbons by impregnation with a solution of Nickel carrier containing aluminum oxide and from 0.5 to 25% of calcium oxide, at least part of the calcium oxide is associated with the aluminum oxide in the form of so-called kalyanamitra cement, which consists of calcium oxide as CaO aluminate 6Al2O3and CaO 2Al2O3, followed by drying, calcination [DE 19720599 A1, class B 01 J 23/78, publ. 20.11.97].

The closest known solution to the technical essence and the achieved effect is a method for preparing a catalyst for the conversion of hydrocarbons comprising preparing a carrier by mixing alumina, aluminum hydroxide, technical aluminate calcium, graphite, introduction aqueous plasticizing burnable additives, which are used polyvinyl alcohol, the molding, the crop has wilted media on the air , wysokotemperaturowe the calcination of the carrier at a temperature of 1450 - 1550oC, the carrier impregnated with solutions of nitrates of Nickel and aluminum, followed by drying and calcination of the catalyst mass [SU, 1780208 A1, class B 01 J 23/78, publ. 10.11.95].

The disadvantages of this method include the duration of the preparation of the catalyst, since such stage as the crop has wilted media on the air, is carried out for 24 h, the heat media in the environment of water vapor should be performed within 4 h in Addition, the carrier obtained in a known manner, partially cracks, leading to increased waste and scrap during production of the catalyst.

The present invention is to simplify the technology and obtaining a catalyst with high activity and mechanical strength and persistence of these characteristics during long-term operation of the catalyst.

To solve this problem, a method for preparation of the catalyst for conversion of hydrocarbons, including the preparation of a carrier by mixing alumina, aluminum hydroxide, technical aluminate calcium, graphite, introduction aqueous plasticizing burnable additives, molding, the crop has wilted n is mperature 150 - 170oC for 1.0 -1.5 h, followed by drying under the following mode: the temperature in the drying zone lift with a speed of 40 to 60oC in 1 h to 120oC and at this temperature, the carrier can withstand 1.5 - 2.0 hours, followed by high temperature annealing and subsequent impregnation of the support with solutions of nitrates of Nickel and aluminum, taken in the mass ratio (4.0 - 5.0): 1, in terms of Nickel oxide and aluminum oxide, drying and heat treatment of the catalyst mass.

As the plasticizing burnable supplements use the sodium carboxymethyl cellulose and high-temperature calcination of the carrier is carried out at a temperature of 1450 - 1500oC.

Example. Nickel-containing catalyst for the conversion of hydrocarbons obtained by impregnation of the carrier with an aqueous solution of nitrates of Nickel and aluminum with subsequent impregnation and calcining.

For preparation of the media take the source components in the following quantities (kg): ground alumina 64; aluminum hydroxide 99; technical aluminate calcium 85.2; graphite - 16.5, place them in a plow mixer and mix for 10-15 minutes, the resulting mixture is humidified in the Z-shaped mixer for 10-15 minutes with a solution of sodium carboxymethyl cellulose, gave the hydrothermal processing of media in the autoclave in an environment of water vapor pressure of 1-2 ATM, the temperature of 150-170oC for 1-1.5 hours Drying medium is carried out in a shaft of electric furnaces in the following mode: the temperature raising speed of 40-60oC to 120oC and at this temperature, the carrier can withstand 1.5-2.0 hours the Dried carrier is calcined in a tunnel kiln at a temperature of 1450-1500oC, where due to the processes of sintering is formed physical structure of the media.

To obtain the catalyst of a given amount of Nickel oxide calcined and cooled medium is subjected to (3 - 4)-fold impregnation in the scrubber with a solution of nitrate salts of Nickel and aluminum at a mass ratio (4 - 5):1 in terms of Nickel oxide and aluminum oxide and installation impregnation-calcination with subsequent drying-calcining at a temperature of 400 - 450oC after each impregnation to decompose the nitrates.

The result is 300 kg of finished catalyst for the conversion of hydrocarbons.

According to the invention is the simplification of the technology is due to the fact that the sodium carboxymethyl cellulose is better than the polyvinyl alcohol is dissolved in water, which in turn leads to a more homogeneous mass; conducting heat treatment of the media in avtak the operation of technical calcium aluminate, it allows to increase the content of fine products of hydration in the composition of the medium and to reduce the temperature of the annealing medium 20 - 30oC.

Carrying out drying in the above mode virtually eliminates cracking of media tablets and improves technical characteristics and appearance of final product.

Used the ratio of nitrates of Nickel and aluminum impregnation of the carrier maintains the crystallinity of the active component - Nickel at a level of not more than 400 , which in turn provides a high catalyst activity during long-term operation.

1. The preparation method of catalyst for the conversion of hydrocarbons comprising preparing a carrier by mixing alumina, aluminum hydroxide, technical aluminate calcium, graphite, introduction aqueous plasticizing burnable additives, molding, the crop has wilted in the air, the heat media in the environment of water vapor, high temperature annealing, subsequent impregnation of the support with solutions of nitrates of Nickel and aluminum, drying and heat treatment of the catalyst mass, characterized in that the heat carrier is carried out in the autoclave at the IU: the temperature in the drying zone lift with speed 40 - 60 deg/h to 120oC and at this temperature the media stand at 1.5 - 2.0 h, the impregnation of the calcined carrier implement solutions of nitrates of Nickel and aluminum, taken in the mass ratio (4,0 - 5,0) : 1 in terms of Nickel oxide and aluminum oxide.

2. The method according to p. 1, characterized in that the plasticizing burnable supplements use the sodium carboxymethyl cellulose and high-temperature calcination of the carrier is carried out at 1450 - 1500oC.

 

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