Method of preparation of catalyst postinoculation

 

(57) Abstract:

The invention relates to a method of preparing phosphoroclastic catalysts for processes of oligomerization of low molecular weight olefins and alkylation of benzene by propylene and can be used in the refining and petrochemical industries. The objective of the invention is to increase the strength and thermo-mechanical stability of the granules postinoculation catalyst. The technical result is achieved by the known method of preparation of the catalyst, comprising mixing the acid with the carrier, drying and grinding the resulting silicophosphates complex, its moisturizing and granulation, followed by drying, the granules of the catalyst is subjected to ultra-high frequency electromagnetic wave impact at temperatures from 400 to 600C. table 1.

The invention relates to a method of preparing phosphoroclastic catalysts for processes of oligomerization of low molecular weight olefins and alkylation of benzene by propylene and can be used in the refining and petrochemical industries.

There is a method of cooking postinoculation catalyst on the basis of the value is the existing silicophosphates its hydration, the molding extrusion and drying the resulting catalyst [Higher olefins. Production and use. / Under. Ed. M. And Dalina - Leningrad: Khimiya, 1984, S. 125-126] . The disadvantage of this method is the low mechanical strength of the pellets of the obtained catalyst.

The closest technical solution to the claimed invention (the prototype) is a method for preparing postinoculation catalyst based on silica-containing media and phosphoric acid, comprising mixing the acid with the carrier, drying, grinding formed silicophosphates complex, tableting with the addition of graphite or talc, processing water vapor and drying. The method allows to obtain granules with high mechanical strength [A. S. 1245338 (USSR) M. Rakhimov, J. F. Galimov, B. L. Rosenbaum, N. E. Putilin. The method of preparation postinoculation catalyst. Publ in B. And 1986, N 27]. The disadvantage of this method is not sufficiently high strength of the granules of catalyst and low thermo-mechanical stability. It is known that at higher temperatures there is a decrease in mechanical strength of the granules phosphoroclastic catalysts. The stability of the strength of their pellets to the temperature effect is estimated as the ratio nacinajuscih properties postinoculation catalyst. Colloid journal, 1987, T. XI, issue 2, S. 333-336].

The present invention solves the problem of increasing strength and thermo-mechanical stability of the granules postinoculation catalyst by creating in their structure silicophosphates high thermomechanical stability.

The technical result is achieved by the known method of preparation of the catalyst, comprising mixing the acid with the carrier, drying and grinding the resulting silicophosphates complex, its moisturizing and granulation, followed by drying, according to the invention, the granules of the catalyst is subjected to microwave (MW) electromagnetic wave impact at temperatures from 400 to 600oC. Preparation of the catalyst of the proposed method allows you to instantly enter in the volume of granules of high energy density and to avoid local overheating. This phenomenon leads to increased strength and thermo-mechanical stability of the granules of the catalyst due to the formation of the structure of silicophosphates with high thermo-mechanical stability.

The method is as follows.

Phosphoric acid in a concentration of 80 wt.% on phosphoric anhydride mixture is statnogo complex, its moisturizing, granulation and drying, the catalyst is subjected to microwave electromagnetic wave impact at temperatures from 400 to 600oC.

The effect of increasing the strength and thermo-mechanical stability of the granules catalysts was confirmed by the following examples.

Example 1. Commodity phosphoric acid is evaporated to a concentration of 80 wt. % phosphoric anhydride and mixed at 175oC prestaged diatomaceous earth mass ratio of 2.8:1. Received silicophosphates complex is dried until the content of free acid of 17.7 wt.% and after grinding, sieving, wet granularit and dried in a muffle furnace until the content of free acid 15...20 and chemically bound water 6...8 wt.%

Example 2. Commodity phosphoric acid is evaporated to a concentration of 80 wt. % phosphoric anhydride and mixed at 175oC prestaged diatomaceous earth mass ratio of 2.8:1. Received silicophosphates complex is dried until the content of free acid of 17.7 wt.% and after grinding, sieving, wet granularit and dried in a muffle furnace until the content of free acid 15...20 and chemically bound water 6...8 wt.%. Next, the resulting granules are subjected to microwave electric is alistore the same, as in example 2, except that the pellets of the catalyst is subjected to microwave electromagnetic wave exposure at a temperature of 300oC.

Example 4. Conditions of preparation of the catalyst are the same as in example 2, except that the pellets of the catalyst is subjected to microwave electromagnetic wave exposure at a temperature of 350oC.

Example 5. Conditions of preparation of the catalyst are the same as in example 2, except that the pellets of the catalyst is subjected to microwave electromagnetic wave exposure at a temperature of 400oC.

Example 6. Conditions of preparation of the catalyst are the same as in example 2, except that the pellets of the catalyst is subjected to microwave electromagnetic wave exposure at a temperature of 450oC.

Example 7. Conditions of preparation of the catalyst are the same as in example 2, except that the pellets of the catalyst is subjected to microwave electromagnetic wave exposure at a temperature of 500oC.

Example 8. Conditions of preparation of the catalyst are the same as in example 2, except that the pellets of the catalyst is subjected to microwave electromagnetic wave exposure at a temperature of 550ooC.

Example 10. Conditions of preparation of the catalyst are the same as in example 2, except that the pellets of the catalyst is subjected to microwave electromagnetic wave exposure at a temperature of 650oC.

Example 11. Conditions of preparation of the catalyst are the same as in example 2, except that the pellets of the catalyst is subjected to electromagnetic wave exposure at a temperature of 700oC.

Example 12. Ready industrial catalyst-84-3 is subjected to microwave electromagnetic wave exposure at a temperature of 520oC.

Example 13. Ready industrial catalyst Phosphoric acid on the diatomite" (FCD) is subjected to microwave electromagnetic exposure at a temperature of 520oC.

Example 14. Ready industrial phosphonacetyl catalyst company "UOP" subjected to microwave electromagnetic wave exposure at a temperature of 520oC.

Samples of the catalyst prepared according to examples 1-14 were tested for catalytic activity in the reaction of oligomerization of concentrated isobutylene and identified the mechanical strength and thermo-mechanical stability of the granules by the method described above. Received the samples of catalysts With-84-3, FCD and firms "UOP".

As follows from table 1, the microwave electromagnetic wave effects on catalysts at temperatures from 400 to 600oC (samples in examples 5-9 and 12-14) allows to increase the strength and thermo-mechanical stability of the granules without reducing their activity.

At temperatures of exposure below 400oC increase strength and thermo-mechanical stability of the granules does not occur, and at temperatures influence over 600oC increased strength and thermo-mechanical stability of the granules is accompanied by a decrease in the catalyst activity.

With the purpose of comparative evaluation of stability of the durability of the pellets in an industrial reactor of industrial samples of the catalyst-84-3 and the catalyst prepared by the proposed method (example 12) were loaded into a perforated container and installed in a separate tube reactor industrial installations oligomerization butane-butylene fraction. Reactor spent 91 days, the process temperature was varied in the range of 160...200oC, a pressure of 5.6...6.3 MPa.

The analysis extracted from the reactor samples showed that the residual strength of the catalyst-84-3 is 2.7 N/Gran., that is just 0, which has been equal to 26.8 N/Gran., what is 4.9% from its original value or more than six times greater than the residual strength of the catalyst-84-3.

Thus, comparative tests of the catalysts prepared with known and proposed methods in an industrial reactor confirmed the increased stability of the strength of the granules of the catalyst obtained by the proposed method.

The present invention can be used on installations oligomerization of low molecular weight olefins and alkylation of benzene with propylene.

The method of preparation postinoculation catalyst, comprising mixing the acid with the carrier, drying and grinding the resulting silicophosphates complex, its moisturizing and granulation, followed by drying, characterized in that the catalyst is subjected to ultra-high frequency electromagnetic wave impact at temperatures from 400 to 600oC.

 

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