The preparation method of catalyst for the conversion of so2in so3

 

(57) Abstract:

The invention relates to methods of producing sulfuric acid vanadium catalysts. The technical problem of the invention is to increase the stability of the activity of the catalyst at 420oWith in the short-term cooling layer in the reaction medium. The task is solved by the method of preparation of the catalyst involves the deposition of media - hydrocephaly from the system containing dissolved silica in a certain concentration, mixing and/or impregnation of the carrier of the active components containing oxides of vanadium, alkali metals and sulfur, forming, drying and calcining. In this case, the deposition of the carrier is carried out at a concentration of silicon dioxide prior to deposition of 120-270 g/l, and after deposition before mixing with active components media thermoablative not less than 0.5 h at a temperature of not less than 30oC. While the pH of the heat treatment is in the range of 5.2 to 11.5. The deposition of the carrier preferably carried out by pribivaniem acid to the system containing dissolved silica. The deposition can be conducted in two stages, the first concentration of the silicon dioxide support up to 160 g/l, in the second it abruptly increase. Mixing slurries the media is less than 48 hours, its reduction has a positive effect mixing. The heat carrier can be combined with filtering, washing, repulpable. 7 C.p. f-crystals, 1 table.

The invention relates to methods of producing sulfuric acid vanadium catalysts.

A method of obtaining vanadium catalysts, including deposition of media - hydrocephaly (in the text it is wrongly named as silica gel) by simultaneous draining of liquid glass and acid in stationary conditions (at constant pH, temperature, concentration of silicon dioxide and potassium sulfate), introduction to the obtained suspension of powdered media, the mixture obtained is homogenized mass with active components, drying, granulation and heat treatment of the contact mass [A. S. 1785733, BI 1, 1993].

The disadvantage of this method is the low stability of the catalyst activity at low temperatures (at 420o(C) in the short-term cooling layer in the reaction medium.

A method of obtaining vanadium catalysts, including deposition of hydrocephalia for the given values of the concentration of silicon dioxide and pH, mixing the carrier with a solution of active ingredients followed the obtained catalyst low stability of activity (at 420o(C) in the short-term cooling layer in the reaction medium.

The technical problem of the invention is to increase the stability of the activity of the catalyst at 420oWith in the short-term cooling layer in the reaction medium. (This mode reflects the state of the catalyst layer in an industrial reactor during the regular stops associated with preventive repairs).

The task is solved by the method of preparation of the catalyst involves the deposition of media - hydrocephaly from the system containing dissolved silica in a certain concentration, mixing and/or impregnation of the carrier of the active components containing oxides of vanadium, alkali metals and sulfur, forming, drying and calcining.

In this case, the deposition of the carrier is carried out at a concentration of silicon dioxide prior to deposition of 120-270 g/l, and after deposition before mixing with active components media thermoablative not less than 0.5 h at a temperature of not less than 30oC. While the pH of the treatment support in the range of 5.2 to 11.5. The deposition of the carrier preferably carried out by pribivaniem acid to the system containing dissolved silica. The deposition can be conducted in two Mixing slurry of the carrier with solutions of active ingredients is carried out at a temperature of preferably not less than 20oC. the heat treatment Time media is mostly less than 48 hours, its reduction has a positive effect mixing. The heat carrier can be combined with filtering, washing, repulpable. Adjustment of pH during the heat treatment medium hold liquid glass, alkali, acid, water.

The major difference of the proposed method from the prototype is an additional stage heat treatment of the carrier under certain conditions, which is carried out after deposition of the carrier prior to its mixing with the active components. The concentration of the dissolved silicon dioxide should be before the deposition of 120-270 g/L. These conditions allow the catalyst, the technical task of the invention, due to the presence of the following features of the process.

From literature data it is known that in General, when the calcination of the catalyst portion of the vanadium from the active complex is blocked siliceous carrier, goes into acid-insoluble state and becomes inactive.

Under the operating conditions of the active complex catalyst, which is in the molten state can be obednitsa vanadium for scale short-term cooling of the layer is greater, the higher the concentration of active vanadium remaining in the molten state.

Carrying out heat treatment svezheosazhdennoi media in these conditions reduces its ability to block vanadium during the calcining of the catalyst and thus increases the concentration of active vanadium in the melt. This apparently leads to an increase in the stability of the catalyst activity in a negative modes of short-term cooling of the layer.

Carrying out the method of producing the catalyst according to the prototype without heat treatment carrier prior to its mixing with the active components do not provide the specified properties (see table).

Carrying out the method of producing the catalyst according to the model, characterized by the constancy of the pH, the lower is the concentration of SiO2during the precipitation, as well as the addition of dry powder xerogel, also does not provide the specified properties of the catalyst (see table).

Carrying out heat treatment at less than 0.5 h does not improve the stability of active cooling layer. Duration of more than 48 hours is impractical due to the lack of further increasing the stability of the activity.

At lower concentrations of SiO2in the pulp of less than 120 g/l in the deposition of hydrocephalia occurs irreproducibility of results on the durability of the catalyst.

When the concentration of SiO2more than 270 g/l and reduced activity, and stability.

With the increase of pH heat treatment reduced the activity, and stability.

Example 1. For the preparation of carrier - hydrocephaly used standard liquid sodium glass with a density of 1.48 g/cm3and the concentration of SiO2- 30%. Standard glass was diluted with water to a concentration of SiO2120 g/l, the solution was stirred 15 minutes To the diluted solution with stirring was added sulfuric acid with a concentration of 92.5% for 1 min to obtain a pH~ 5,2. The pulp of hydrocephaly was kept under stirring for 1 hour the Slurry was heated to 90oWith and kept under stirring for 3 hours the pH of the pulp after the heat treatment was 7.5. Then the slurry was filtered, the precipitate of hydrocephalia washed with water at the rate of 15 liters per 1 kg of dry Si02. For the preparation of a catalyst mass to wet hydrocephaly with a temperature of ~25oC was added a solution of sulfuric acid and potassium Vanadate based polynoe.

The slurry of the catalyst was evaporated to dryness, the powder was moistened and extrudible, the pellet was dried and progulivali at 500oC for 2 h

The calcined catalyst was analyzed for catalytic activity and the crushing strength along generatrix. The results of the definitions presented in the table as relative values compared with the same test sample obtained in accordance with example 3 of the prototype.

Example 2. The catalyst was prepared in accordance with example 1 except for the following parameters: concentration of SiO2in dilute solution of liquid glass was 190 g/L. pH of the pulp hydrocephaly before heat treatment was diluted to 8.0. After heat treatment, the pH of 11.5. Heat treatment temperature 95oWith time 0.5 hours

Example 3. The catalyst was prepared in accordance with example 1 except for the following parameters: concentration of SiO2in dilute solution of liquid glass was 270 g/l, the pH of the pulp hydrocephaly before heat treatment - 7,0, after heat treatment - 10,0, the temperature of the heat treatment 30oWith time - 48 hours

Example 4. The pulp of hydrocephalia prepared in accordance with example 3 of the prototype in two stages: in the accordance with example 2 of the present technical solution. The heat treatment time media - 2 hours

Example 5. The catalyst was prepared in accordance with example 2. The heat treatment conducted after the filters, cleaning hydrocephaly and repulpable water to form a slurry with a moisture content of 80%.

Example 6. The catalyst was prepared in accordance with example 1. The concentration of SiO2in dilute solution of liquid glass was 115 g/l, the pH of the pulp hydrocephaly before heat treatment - 5,0, after heat treatment to 6.3 heat treatment temperature 25oWith time - 0,4 h

Example 7. The catalyst was prepared in accordance with example 1. The concentration of SiO2in dilute solution of liquid glass was 278 g/l, the pH of the pulp hydrocephaly before heat treatment - 8,2, after heat treatment of 11.4, heat treatment temperature 95oWith time - 6 hours

Example 8. The catalyst was prepared in accordance with example 1. The concentration of SiO2in dilute solution of liquid glass was 190 g/l, the pH of the pulp hydrocephaly before heat treatment - 8,2, after heat treatment - 11,7; heat treatment temperature 100oWith time - 28 hours

1. The preparation method of catalyst for the conversion of SO2in SO3including the deposition of the carrier - hydrobromide media active components, containing oxides of vanadium, alkali metals and sulfur, forming, drying and calcining, characterized in that the deposition of the carrier is carried out at a concentration of silicon dioxide prior to deposition of 120-270 g/l, and after deposition before mixing with active components media thermoablative not less than 0.5 h at a temperature of not less than 30oC, while the pH of the treatment support in the range of 5.2 -11,5.

2. The method according to p. 1, characterized in that the deposition of the carrier preferably carried out by pribivaniem acid to the system containing dissolved silica.

3. The method according to p. 1, characterized in that the deposition of lead in two stages, the first concentration of the silicon dioxide support up to 160 g/l, in the second it abruptly increase.

4. The method according to p. 1, characterized in that the mixing of the slurry of the carrier with solutions of active ingredients is carried out at a temperature of not less than 20oC.

5. The method according to p. 1, characterized in that the heat treatment time media is mostly less than 48 hours

6. The method according to p. 1, characterized in that the heat carrier is combined with filtering, washing, repulpable.

7. The method according to p. 1, characterized in that the heat treatment of the carrier e carrier conducting liquid glass, alkali, acid, water.

 

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