RU1803409C - Method of active component of catalyst synthesis in exhaust gases scrubbing process from nitrogen oxides - Google Patents

Abstract

The inventive treatment of bromine tetra-4-carboxyphthalocyanine with bromine in chlorosulfonic acid in the presence of iodine at 75-80 ° C for 7-8 hours, followed by cooling of the reaction mixture, establishing a neutral medium by washing the reaction mixture with water after treatment its hydrochloric acid, followed by treatment with alkali and acid. 22 examples. 2 tab.

Description

The invention relates to a method for producing a new active component of a catalyst for the purification of exhaust gases from nitrogen oxides, which can be used in the chemical industry, ferrous metallurgy and other industries for industries requiring the purification of a large amount of gases with a temperature below 200 ° C during etching metals with nitric acid in galvanic shops, in a number of processes in instrument making, in the production of phosphors, etc. - where the emissions of nitrogen oxides are periodic and the gases are often dusty, contain droplets, diluted with atmospheric oxygen.

The aim of the invention is to increase the catalytic activity of the target product.

The goal is achieved in that cobalt tetra-4-carboxyphthalocyanine is brominated with bromine in chlorosulfonic acid in the presence of iodine at 75-80 ° C.

for 7-8 hours, cool, the precipitated precipitate is washed to a neutral medium and the target product is isolated by treating the reaction mass with an alkaline solution, followed by acidification of the aqueous solution and separation of the target product.

Example 1. Obtaining the active component of the catalyst. 1.5 g (0.002 mol) of cobalt tetra-4-carboxypsyphthalocyanine are placed in a three-necked flask, 15 ml of freshly distilled chlorosulfonic acid, 0.7 ml (0.016 mol) of bromine and 0.02 g (0.00015 mol) of iodine are added. With constant stirring, the reaction mixture is heated to 80 ° C and held at this temperature for 8 hours. After cooling, the solution is carefully poured onto ice. The precipitate was centrifuged, washed with hydrochloric acid and water. The resulting product was placed in 200 ml of a 2.5% aqueous solution of potassium hydroxide and heated to 50 ° C with constant stirring. After keeping under these conditions for 0.5 h, the solution is filtered

00 about CJ 4 about

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the active component obtained in example 3.

Example 13. The preparation of the catalyst 4. Analogously to example 10 using the active component obtained in example 4.

PRI me R 14. Preparation of the catalyst 5. Analogously to example 10 using the active component obtained in example 5.

Example 15. Preparation of the catalyst 6. Analogously to example 10 using the active component obtained in example 6.

Example 16. Preparation of the catalyst 7. Analogously to example 10 using the active component obtained in example 7,

Example 17, Preparation of the catalyst 8. Analogously to example 10 using the active ingredient obtained in example 8.

Example 18. Preparation of the catalyst 9. Analogously to example 10 using the active component obtained in example 9.

Example 19. The cleaning process. The purification was carried out in a flow-through glass reactor with a diameter of 10 mm and a catalyst volume of 1 equal to 1 cm3. The composition of the gas mixture before purification: N0 1.0 vol.%; MHZ 1.0 vol.%; 024.0% vol .; N2 94.0% by volume. The gas analysis before and after the contact apparatus was carried out according to method 4. The temperature in the reactor was 50 ° C. The volumetric gas flow rate is 10300. The degree of gas purification from N0 is 99.5%.

Example 20, Purification was carried out as in example 19. The temperature in the reactor was 100 ° C. The volumetric gas flow rate is 12000. The degree of gas purification from N0 99.5%.

Example 21. The purification was carried out as in example 19. The temperature in the reactor was 150 ° C. The volumetric gas flow rate was 13500. The degree of gas purification from N0 99.5%.

Example 22. The purification was carried out as in example 19. The temperature in the reactor was 200 ° C. The volumetric gas flow rate is 14600. The degree of gas purification from N0 99.5%.

The data of Examples 19-22 are summarized in Table 1 and compared with the results of the prototype under similar conditions.

Purification data in the presence of catalysts 2-9, in the preparation of which the active components synthesized according to examples 2-9 were used, are given

in table 2 (the conditions for all catalysts are similar).

A comparison of the catalytic properties shown in Tables 1 and 2 of the catalysts illustrates the undoubted advantage of the catalyst, the active component of which is cobalt tetrabromotetracarboxyphthalocyanine obtained by the inventive method. The catalyst using the obtained active component has a higher activity than the known one, which allows the purification process to be carried out at a gas flow rate of 14,600 and a gas purification rate of 99.5% from nitrogen oxides at 200 ° C, i.e. increases the efficiency of the cleaning process, because a greater volume of gas is subjected to cleaning at the same time; in addition, this leads to a decrease in material consumption and other costs.

The stability coefficient of the catalyst using the active component obtained by the inventive method, as well as using the known active component, is about 0.98-0.99 and maintains its stability for at least 200 hours of operation.

The composition of the gas before purification: N0-1.0 vol.%; MHZ-1, Oob.%; 02-4.0 about. %; N2-94.0 vol. %

After purification, practically all of N0 (up to 99.5%) and LN3 are converted to N2 and.

The proposed method can be used to obtain an active component of a catalyst for the process of purification of exhaust gases from nitrogen oxides having high catalytic activity.

Claims (1)

The claims A method of obtaining an active component of a catalyst for a process for purifying exhaust gases from nitrogen oxides using a cobalt compound and treating the reaction mass with an alkaline solution, followed by acidifying the solution and separating the target product, characterized in that, in order to increase the catalytic activity of the target product, the cobalt compound is used cobalt tetra-4-carboxyphthalocyanine, which is treated with bromine in chlorosulfonic acid in the presence of iodine at 75-80 ° C for 7-8 hours, with the last cooling the reaction mass, establishing a neutral medium by washing the reaction mass with water after treating it with hydrochloric acid, followed by treatment with alkali and acid. Table 1 Table 2