RU2247598C1 - Method for production of sorbent catalyst - Google Patents

Abstract

FIELD: sorption technique for purification of industrial emissions and individual pipe security facilities.

SUBSTANCE: method for production of sorbent catalyst includes preparation of impregnating solution by introducing ammonium carbonate and copper and chromium compounds into ammonia water in ratio ammonia water/ammonium carbonate/copper basic carbonate/chrome anhydride of 1:(0.07-0.15):(0.03-0.06):(0.02-0.04); impregnation with metal-containing carbon solution; aging; and granule thermal treatment.

EFFECT: sorbent catalyst with prolonged protective action in relation to chlorocyanide and decreased cost.

4 cl, 3 ex

Description

The invention relates to the field of sorption technology and can be used in the cleaning of industrial gases or in personal respiratory protection,

A known method of producing a sorbent-catalyst, comprising impregnating activated carbon with a solution of catalytic additives, followed by heat treatment, and as an impregnating solution, an ammonia solution containing 8-16 wt.% Carbon dioxide, 10-25 wt.% Copper cupranate, 2-5 wt. % of chroma, and the ratio of coal-impregnating solution is 1: 0.5-0.9 and heat treatment is carried out in a fluidized bed furnace at 155-190 ° C (see US Pat. Russian Federation No. 2083274, class B 01 J 20 / 20, G 01 B 31/08, publ. 10.07.97).

The disadvantage of this method is the complexity of the preparation of the impregnating solution and the loss of catalyst during high-temperature heat treatment.

The closest to the proposed technical essence and the number of matching features is a method of producing a sorbent-catalyst, comprising impregnating metal-containing granules of activated carbon with an aqueous solution of potassium dichromate and triethylenediamine (TEDA) in the ratio sorbent: potassium dichromate: TEDA 1: (0.04-0, 08): (0.004-0.008), aging is carried out for 1.5-1.8 hours, and the previously metal-containing granules are calcined at 800-850 ° C in an atmosphere of superheated water vapor (see US Pat. RF 2108149, class B 01 J 20/20, G 01 B 51/08, publ. 10.04.98).

The disadvantage of the prototype is the short time of the protective action of chlorocyanine in short layers of the sorbent catalyst.

The technical result (goal) of the invention is to increase the time of the protective action of the sorbent-catalyst on chlorocyanine in short layers.

In modern conditions, the time of the protective action of the sorbent-catalyst in short layers is of great importance. High values of the time of protective action can reduce the weight and size characteristics of respiratory protective equipment and reduce their cost. This is especially important for poorly absorbable substances, an example of which is chlorocyan - a test substance in tests of sorbent-catalysts.

The goal is achieved by the proposed method, including the preparation of an impregnating solution by dissolving chromic anhydride and silver nitrate in copper ammonia, impregnating metal-containing granules of activated carbon, their aging and heat treatment, while the preparation of the impregnating solution is carried out by introducing ammonium carbonate and copper and chromium compounds into ammonia water and the ratio of the components in the impregnating solution is ammonia water: ammonium carbonate: basic carbonic acid: chromic anhydride 1: (0.07-0 , 15) :( 0.03-0.06) :( 0.02-0.04), and, if necessary, 0.10-0.20 wt.% Silver nitrate is added to the impregnation solution with respect to the weight of metal-containing granules of active coal.

The difference of the proposed method from the known one is that the preparation of the impregnating solution is carried out by introducing ammonia carbon dioxide and copper and chromium compounds into ammonia water, and the ratio of the components in the impregnating solution is ammonia water: ammonium carbonate: basic carbonic acid: chromic anhydride 1: (0, 07-0.15) :( 0.03-0.06) :( 0.02-0.04), and if necessary, (0.10-0.20) wt.% Silver nitrate is added to the impregnation solution in relation to to the mass of metal-containing granules of activated carbon.

It is not known from the scientific and technical literature the preparation of an impregnating solution by introducing ammonium carbonate and copper and chromium compounds into ammonia water at a ratio of components in the impregnating solution ammonia water: ammonium carbonate: basic carbonic acid: chromic anhydride 1: (0.07-0.15 ) :( 0.03-0.06) :( 0.02-0.04), if necessary, (0.10-0.20) wt.% Silver nitrate is added to the impregnation solution with respect to the mass of metal-containing granules of activated carbon .

The essence of the proposed method is as follows. To absorb poorly absorbed substances, such as chlorocyanine, it is necessary to create a catalyst that would provide the highest decomposition rate of a toxic substance. As a result of numerous experiments, it was found that the sequence of dissolution of the components in ammonia water by introducing ammonium carbonate, basic copper carbonate, chromic anhydride promotes their good interaction in the solution without precipitation, while the optimal ratio of the components is selected during the experiments.

The addition of silver helps to stabilize the catalytic complex on metal-containing granules of activated carbon.

The method is as follows.

Take metal-containing granules of activated carbon containing copper, chromium, silver, with a total pore volume of 0.6-0.8 cm ³ / year An impregnating solution is prepared by adding the calculated amount of ammonium carbonate, basic carbonic acid and chromic anhydride to ammonia water, while their ratio in the solution is ammonia-based water: ammonium carbonate: basic carbonic acid: chromic anhydride 1: (0.07-0.15) : (0.03-0.06) :( 0.02-0.04).

When preparing the solution, maintain a temperature of 40-60 ° C. Then carry out the impregnation of granules of metal-containing activated carbon impregnating solution with an impregnation coefficient of 0.8-0.9. The granules are aged 1.5-1.8 hours and heat treated in a fluidized bed furnace at a temperature of 150-160 ° C. Then the sorbent catalyst is cooled to room temperature and the time of the protective action of chlorocyanine is estimated.

If necessary, a promoter additive of nitric acid silver is introduced into the impregnation solution in an amount of 0.1-0.2 wt.% With respect to the weight of coal.

Test conditions for the sorbent catalyst:

The concentration of chlorocyanine vapor 5 mg / l

Layer Height 2 cm

Specific volumetric flow rate

vapor mixture 0.5 l / min · cm ²

Relative humidity 75%

obtained by the proposed method, the sorbent catalyst had a protective action time in a short layer (2 cm) of 10-12 minutes

EXAMPLE 1. Take 1 kg of granules of metal-containing activated carbon with a total pore volume of 0.7 cm ³ / g An impregnation solution is prepared by dissolving in 1 liter of ammonia water 70 g of ammonium carbonate, 30 g of basic carbonic acid, 20 g of chromic anhydride, the ratio of ammonia solution: ammonium carbonate: basic carbonic acid: chromic anhydride 1: 0.07: 0.03 : 0.02.

The granules are aged for 1.5 hours and heat treated at 150 ° C, after which they are unloaded and cooled to room temperature. The resulting sorbent catalyst had a chlorocyanine protective action time of 10 minutes.

EXAMPLE 2. The implementation of the process as in example 1, except that prepare an impregnating solution with a ratio of ammonia solution: ammonium carbonate: carbonic base copper: chromic anhydride. 1: 0.11: 0.05: 0.03.

The resulting sorbent catalyst had a chlorocyanine protective action time of 12 minutes.

EXAMPLE 3. The implementation of the process as in example 1, except that preparing an impregnating solution with a ratio of ammonia water: ammonium carbonate: carbonic base copper: chromic anhydride 1: 0.15: 0.06: 0.04.

The resulting sorbent catalyst had a chlorocyanine protective action time of 11 minutes.

The indicator of the protective action of chlorocyan in a short layer of 2 cm in the prototype had 5-7 minutes Thus, the proposed method allows to significantly (1.5-2.4 times) increase the time of the protective action of the sorbent-catalyst for chlorocyanine in comparison with the prototype.

It follows from the foregoing that each of the signs of the claimed combination to a greater or lesser extent affects the achievement of the goal, namely, the increase in the time of the protective action of the sorbent-catalyst on chlorocyanine in short layers, and the entire population is sufficient to characterize the claimed technical solution.

Claims (4)

1. A method of producing a sorbent-catalyst, including the preparation of an impregnating solution, impregnation of a prepared solution of granules of metal-containing coal, aging of the granules and heat treatment, characterized in that the preparation of the impregnating solution is carried out by sequentially adding the calculated amount of ammonium carbonate, carbonic acid basic copper and chromic anhydride to ammonia water . 2. The method according to claim 1, characterized in that activated carbon containing copper, chromium and silver is fed to the impregnation. 3. The method according to any one of the preceding paragraphs, characterized in that the preparation of the impregnating solution is carried out to ensure the ratio of the components of ammonia water: carbonic base copper: chromic anhydride equal to 1: (0.07-0.15) :( 0.03-0 06) :( 0.02-0.04). 4. The method according to any one of the preceding paragraphs, characterized in that nitric acid silver is additionally introduced into the impregnation solution in an amount of 0.1-0.2% by weight of coal.