Iron-chromium catalyst preparation method (options)

FIELD: catalyst preparation methods.

SUBSTANCE: invention relates to methods for preparing carbon monoxide-conversion catalysts used in production of hydrogen, nitrogen-hydrogen mixture, and other hydrogen-containing gases. According to first option, active catalyst component, i.e. iron compound, is precipitated from solution with precipitation reagent, whereupon precipitate is separated from mother liquor and washed to form catalyst mass, which is molded and subjected to heat treatment, re-washed, mixed with chromic anhydride and subjected to final heat treatment: at 280-420°C after molding or at 50-200°C before molding of catalyst mass. According to second option, iron compound is first mixed with promoting additives and cations of promoting additives are precipitated jointly with iron cations, resulting precipitate is separated from mother liquor, washed and subjected to heat treatment, re-washed, mixed with chromic anhydride and subjected to final heat treatment: at 280-420°C after molding or at 50-200°C before molding of catalyst mass. As iron compound in the first and second options, ferrous and ferric sulfates and, as precipitation reagent, carbonate salts or corresponding hydroxides are utilized. Promoting additives are selected from Cu, Mn, and Al or, in the second option, their mixture.

EFFECT: reduced content of sulfur in finished catalyst at the same catalyst activity.

3 cl, 1 tbl, 12 ex

 

The invention relates to a method of preparing gelatobaby catalysts for the conversion of carbon monoxide with hydrogen, nitric mixture or other hydrogen-containing gases and can be used in the manufacture of catalysts for the chemical and petrochemical industries.

There is a method of cooking zhelezohromovyh catalyst, including the precipitation of iron from solution of ferrous sulfate with sodium carbonate, separating the precipitate from the liquid phase, washing, mixing it with chromic anhydride, spraying the resulting catalyst mass, the extract obtained small balls in the air, mixing them with a strong acid (nitric, sulfuric), crushing, drying in a stream of air, glowing and tableting. (Patent of great Britain No. 1109864, 1 E, 1968)

The disadvantages of such a catalyst whose main components - oxide compounds of iron and chromium, are: high sulfur content and relatively low activity.

Also known preparation method zhelezohromovyh catalyst using as initial components ferrous iron sulfate, chromic anhydride, water-soluble salt of the promoter - copper or aluminum, including deposition of iron cation ammonium carbonate, separating the precipitate from the liquid phase, washing him, mixing with the promoters, proc is the Lebanon at a temperature of 300 to 400° With subsequent mixing of the powder with a solution of chromium trioxide, drying the mass, grinding, molding into pellets, calcining at a temperature of 450°C. (Patent RF №2059430, 01 J 23/885, 01 3/16, 1996)

The disadvantages of this method are: high sulfur content in the catalyst, as well as the difficulties arising in the pelletizing calcined catalyst mass, representing rigid abrasive powder.

In addition, there is a method of cooking zhelezohromovyh catalyst comprising a mixture of iron compounds with a solution of chromic acid, which is introduced as promoting additives salt of manganese and at least one compound of alkaline-earth metal selected from the group comprising magnesium, calcium and at least one compound of rare earth metal selected from the group CE, La, Nd, Pr, and optionally, a compound of copper, as well as compounds of iron using iron oxide or iron oxide containing additional magnetite - Fe3O4and/or chromite iron. (Patent RF №2170615, 01 J 37/04, 23/78, 23/83, 2001)

The disadvantages of the method are:

high sulfur content in the finished catalyst

- in addition, the introduction of promoting additives in an aqueous solution of chromic acid, followed by mixing it with a solid-oxide compounds of iron may limit the soon the be the interaction of the latter with the promoting additives and thus, to achieve the desired level of catalyst activity.

Closest to the proposed invention to the technical essence and the achieved result is a cooking method zhelezohromovyh catalyst comprising a mixture of an aqueous salt solution of ferrous sulfate (ferrous) iron with a solution of chromic acid (chromium trioxide), adding one or more salts of the promoters or their aqueous solutions, mainly sulphates of copper and/or aluminum, joint deposition of a mixture of cations of metals of iron, chromium and one or more promoters by simultaneous draining of the mixture of solution and an aqueous solution of water-soluble salts of carbonic acid, preferably sodium carbonate, in an alkaline environment with a pH of not less than 7.1, sediment stabilization, separation its from the liquid phase, and a one-time or repeating washing, followed by drying and forming the catalyst mass by tabletting or molded on the screw press. (Declarative patent of Ukraine # 38510, 01 J 23/74, 23/86, 2001)

The disadvantages of this known method are:

high sulfur content in the finished catalyst is 0.05 wt.%,

- difficulties in washing and filtering the precipitate, obtained by joint precipitation of the catalyst components containing hydroxide connection is in the ferric and chromium, representing an amorphous substance, which is well adsorb impurities (sulfur, sodium) and poorly laundered,

- reducing economic indicators of production of the catalyst due to the additional cost of sulfuric acid (up to 400-500 kg per ton of catalyst), required for the transfer of chromium from hexavalent to the trivalent state by mixing chromium trioxide with a solution of ferrous sulphate of iron, and also because of the larger flow of clean water for washing the precipitated mass and an increase in the duration of its washing.

The objective of the invention is to reduce the sulfur content in the finished catalyst, while maintaining its increased activity.

To solve the problem in the first method of preparation zhelezohromovyh catalyst, by mixing the compounds of iron and chromium, including deposition of the active component of the catalyst compounds of iron from solution precipitating reagent, separating the precipitate from the mother liquor, washing the precipitate, heat treatment and forming the catalyst mass, according to the invention as compounds of iron use of divalent or trivalent iron sulfate, and as a precipitating reagent use soluble salts of carbonic acid or their hydroxides first precipitated iron cations and the precipitate in the Le of separation from the mother liquor and washing subjected to heat treatment, additionally washed, mixed with chromic anhydride and conduct a final heat treatment at 280-420°after forming the catalyst mass or 50-200°before forming the catalyst mass.

According to the second method of preparation zhelezohromovyh catalyst, by mixing compounds of iron, chromium and promoting additives, including deposition of the active component of the catalyst compounds of iron and of promoting additives from the solution precipitating reagent, separating the precipitate from the mother liquor, washing the precipitate, heat treatment and forming the catalyst mass, as compounds of iron use of divalent or trivalent iron sulfate, and as a precipitating reagent use soluble salts of carbonic acid or their hydroxides, first mix the compound of iron with promoting additives, co-precipitation of cations promoting additives with cations of iron, the precipitate after separation from the mother solution and washing subjected to heat treatment, optionally washed, mixed with chromic anhydride and conduct a final heat treatment at 280-420°after forming the catalyst mass or 50-200°before forming the catalyst mass.

As of promoting additives IP is result connection elements, selected, for example, from the series: Cu, Mn, Al or a mixture.

Distinctive features of the methods of the present invention consist in the fact that in the first and second embodiments as compounds of iron use of divalent or trivalent iron sulfate, and as a precipitating reagent use soluble salts of carbonic acid or their hydroxides. In the first method initially precipitated iron cations and the precipitate, after separation from the mother liquor and washing subjected to heat treatment, optionally washed, mixed with chromic anhydride and conduct the final heat treatment. And the second way is first mixed compound of iron with promoting additives, co-precipitation of cations promoting additives with cations of iron, the precipitate after separation from the mother liquor and washing subjected to heat treatment, optionally washed, mixed with chromic anhydride and conduct the final heat treatment. And the final heat treatment is carried out at a temperature of 280-420°after forming the catalyst mass or at a temperature of 50-200°before forming the catalyst mass for both variants of the method.

As of promoting additives are used compounds of elements selected from, for example, range: Cu, Mn, l, or a mixture of - only for the 2nd version of the method.

Intermediate stage heat treatment involves the drying and heat treatment at 130-380°C. as hydroxides use hydroxides of alkali metals and ammonium hydroxide, and as soluble salts of carbonic acid use salts of alkali metals and ammonium.

The present invention meets the condition of patentability - novelty", as in the prior art failed to find technical solutions, the essential features which would coincide with all the features available in the independent claims.

Also the present invention meets the condition of patentability - "inventive step", since the prior art has failed to find technical solutions, the hallmarks of which was provided by the same basic technical problems, the solution of which the invention is directed.

The invention is illustrated by the following examples.

Example 1.

In the apparatus with stirrer pour 6.5 m3solution of ferrous sulfate iron concentration of 248 g/l In the second apparatus with a stirrer to prepare a solution of sodium carbonate (soda) with a concentration of 11-12 wt.%. In the reactor precipitator pour 2-3 m3condensate and slowly add a solution of sodium carbonate of soda), bringing the pH to 7.5 to 7.7, and then begin simultaneous flow in the reactor precipitator prepared solutions - sulphate of iron and soda with a rate of 10-15 l/min, maintaining the precipitator pH level of 7.5-7,8 feed speed sulfate solution. The temperature during the precipitation of support within 30-35°C. after the deposition of the formed slurry is 8 hours for aging the precipitate (in the precipitator or thickener). Settled precipitate was separated by decantation from the mother liquor and spend two consecutive washing reformirovannoy suspension on vacuum filters. The filtered mass is dried, calcined at a temperature of 380°and optionally washed to a specified content of sodium. The washed wet weight in the amount of 485 kg loaded into the mixer and add 34 kg of chromium trioxide (CrO3). The resulting mixture was thoroughly mixed, dried to a predetermined moisture content and ekstragiruyut into pellets with a diameter of 5-7 mm Pellets pre provalivajut, dried to a moisture content of 1-2 wt.% and calcined at a temperature of 400-420°and then, separated from the dust and stuff, stariway in special drums. Chemical composition and quality of the obtained catalyst are shown in the table below.

Example 2.

In the apparatus with stirrer pour 5.5 m3solution of divalent chamois is acidic iron concentration of 242 g/l, add 30 kg solid of copper sulfate (CuSO45H2O) and stirred. In the second apparatus with stirrer preparing soda solution with a concentration of 10-13%. In the reactor precipitator pour 2-3 m3condensate and gradually add the soda solution, bringing the pH to 7.5 and 7.6, and then begin simultaneous flow in the precipitator of the solutions prepared with a rate of 10-15 l/min, maintaining the precipitator pH level of 7.5-7.8 for the supply of the solution sulfate salts of iron and copper and the temperature 30-35°C. after the deposition of the formed slurry is not less than 4 hours for aging (in the precipitator or thickener). Settled precipitate was separated by decantation from the liquid phase, the suspension twice washed on a vacuum filter, dried and calcined at a temperature of 350°C. the resulting powder was sent to repulper, and then press the filter for final cleaning. The washed mass with a known moisture content is loaded into the mixer, to which is added the calculated amount of chromic anhydride (prepared catalyst was 8.3 wt.% Cr2About3). The resulting mixture is stirred until a smooth paste and at a certain humidity ekstragiruyut into pellets of 5 mm diameter, which are dried, and then calcined at a temperature of 380°C.

The calcined catalyst disqualified from dust and stuff, then is loaded into a special drum is to send the consumer.

Example 3.

The catalyst is prepared as in example 2, but in the apparatus with stirrer contribute additionally to 39.3 kg manganese sulfate (MnSO47H2O) and the annealing of the finished catalyst after drying is carried out at a temperature of 280°C.

Example 4.

The beginning of the preparation of the catalyst as in example 2. Dried residue optionally subjected to heat treatment at a temperature of 130°With and washed to a specified content of sodium. The washed precipitate is sent to the mixer, add the calculated amount of solid chromium trioxide (8 wt%), mixed and calcined at a temperature of 200°C. the Obtained catalyst mass is mixed with graphite and pressed into tablets.

Example 5.

The beginning of the preparation of the catalyst as in example 2. Dried sludge is subjected to heat treatment at a temperature of 170°With and washed to a specified content of sodium. The washed mass is mixed with chromic anhydride, dried at a temperature of 50°C, mixed with graphite and pressed into tablets.

Example 6.

For the preparation of the catalyst charge of 0.87 liters of a solution of the oxide iron sulfate with a concentration of 250 g/l and added to a solution of 7.82 g of copper sulfate (CuSO45H2O). Simultaneously prepare 1.1 l 11% solution of soda.

A 2-liter vessel with stirrer and heated (precipitator) pour in the 0.2-0.3 distillirovannoi water, heated to 35°C, poured dropwise a solution of soda, bringing the pH to the precipitator to 7.5 and 7.6. Then in the precipitator at the same time begin to enter the prepared solutions of sulphate of iron with copper and soda, heated to 35-40°S, with a speed of 10-12 ml/min Flow soda solution to regulate pH in the precipitator at the level of 7.5 to 7.8. After deposition of the resulting suspension is left for 15 hours for aging sludge settled sludge is separated from the mother liquor by decantation and then washed to the lack of sulfur in the wash water. The washed precipitate is subjected to heat treatment at a temperature of 350°and then additional washing. The washed precipitate is mixed with 10.6 g of chromic anhydride and the resulting mixture is thoroughly mixed, dried to a moisture content of 23 to 25% and formed into pellets, which are subjected to a heat treatment at a temperature of 350°C.

Example 7.

For the preparation of the catalyst charge of 0.67 liters of a solution of ferrous sulfate iron concentration of 250 g/l and enter into solution 6,37 g of solid salt MnSO47H2O. Simultaneously prepare 1.1 l 11% solution of soda.

A 2-liter precipitator pour in 0.2-0.3 l of distilled water, heated to 35°C, poured dropwise a solution of soda, bringing the pH to the precipitator to 7.5 and 7.6. Then in the precipitator at the same time begin to apply the prepared solution, warmed to 35-40°C. Astor sulfate iron manganese served with a speed of 9-10 ml/min, and the feed rate of ash regulate pH in the precipitator to 7.7. The precipitated suspension is left for 10 hours for aging. The remaining precipitate is decanted from the mother liquor, washed, conduct heat treatment at a temperature of 340°and optionally washed. The washed mass is mixed with 10.6 g of chromic anhydride. The resulting mixture is stirred, dried to a moisture content of 22-25% and ekstragiruyut into granules, which are subjected to a heat treatment at a temperature of 370°C.

Example 8.

For the preparation of the catalyst charge of 0.67 liters of a solution of divalent iron sulfate with a concentration of 250 g/l and injected into a solution of 10.1 grams of salt is aluminum sulfate. Simultaneously prepare 1.2 l 11% solution of soda.

A 2-liter precipitator pour in 0.2-0.3 l of distilled water. Further preparation as in example 7.

Example 9.

For the preparation of the catalyst charge of 0.67 liters of a solution of ferrous sulfate iron concentration of 250 g/l and enter into the solution of 7.82 g of copper sulfate. Prepare 1 liter of solution of 10% sodium hydroxide. Further preparation as in example 7.

Example 10.

In the apparatus with stirrer pour 6.5 m3solution of ferrous sulfate iron concentration of 242 g/l, add 30 kg of solid sulphate of copper - CuSO45H2O and stirred. In the second apparatus with a stirrer to prepare a solution of carbon dioxide Ammon who I am (NH4)2CO3with a concentration close to 20 wt.%. Further preparation as in example 1.

Example 11.

In the apparatus with stirrer pour 6.5 m3solution of ferrous sulfate iron concentration of 242 g/l In the second apparatus 25% ammonia water - NH4OH. Further preparation of the catalyst is carried out as in example 1.

Example 12.

For the preparation of the catalyst is taken to 0.67 liters of a solution of divalent iron sulfate with a concentration of 250 g/l, which introduced of 7.82 g of copper sulfate. Prepare 1 liter of a 10% solution of potash - K2CO3. Further preparation as in example 9.

Characteristics of the samples of the catalysts prepared according to examples 1-12 in comparison with the prototype presented in the table.

To assess the quality of the prepared catalyst samples used the following indicators:

- chemical composition, including loss on ignition (SPT),

- bulk density,

- mechanical strength - the force of destruction when the load on the forming granules

activity is the rate constant at temperature 350°C.

From the data presented in the table shows that the proposed method of cooking zhelezohromovyh catalyst can be obtained from sulfur-containing raw materials (iron sulfate) as a catalyst with low content of ser is at the level excluding the operation of desulphurization when putting it into operation without deterioration of other consumer indicators.

In contrast to the prototype of the production technology of the catalyst according to the proposed method eliminates the use of sulfuric acid (about 500 kg per ton of catalyst), and also increases the performance of the filtration equipment (vacuum filters, filter presses).

Table
№p/pThe quality indicators catalystSamples of the catalysts according to examples 1-12 and prototype
123456789101112The placeholder
1.Content, wt.%
1.1Fe2O389,3of 87.385,077,179,4of 87.087,1 85,586,789,087,189,277,5
1.2Cr2O38,08,38,18,17,88,17,98,38,88,38,57,88,4
1.3CuO-2,42,22,02,22,5--2,4-2,22,32,6
1.4MnO2--1,5---2,0------
1.5Al2About3-------3,0-----
1.6SPT2,72,03,212,810,62,43,03,22,12,72,22,911,5
1.7S, ppm971009512010010013012010512010092800
2.Bulk density, kg/DM31,261,221,251,351,321,31,301,271,221,311,261,271,25
3.Mechanical strength, MPa3,23,02,73,22,92,52,73,23,13,53,33,62,8
4.Activity, cm3CO/GS1,302,42,62,72,62,41,71,62,72,52,52,72,5

1. The method of preparation zhelezohromovyh catalyst by mixing the compounds of iron and chromium, including deposition of the active component of the catalyst compounds of iron from solution precipitating reagent, separating the precipitate from Mato the aqueous solution, the sediment washing, heat treatment and forming the catalyst mass, characterized in that compounds of iron use of divalent or trivalent iron sulfate, and as a precipitating reagent use soluble salts of carbonic acid or their hydroxides first precipitated iron cations and the precipitate, after separation from the mother liquor and washing subjected to heat treatment, optionally washed, mixed with chromic anhydride and conduct a final heat treatment at 280-420°after forming the catalyst mass or 50-200°before forming the catalyst mass.

2. The method of preparation zhelezohromovyh catalyst by mixing the compounds of iron, chromium and promoting additives, including deposition of the active component of the catalyst compounds of iron and of promoting additives from the solution precipitating reagent, separating the precipitate from the mother liquor, washing the precipitate, heat treatment and forming the catalyst mass, characterized in that compounds of iron use of divalent or trivalent iron sulfate, and as a precipitating reagent use soluble salts of carbonic acid or their hydroxides, first mix the compound of iron with promoting additives co-precipitation of cations promoting additives with cations of iron, the precipitate after separation from the mother liquor and washing subjected to heat treatment, optionally washed, mixed with chromic anhydride and conduct a final heat treatment at 280-420°after forming the catalyst mass or 50-200°before forming the catalyst mass.

3. The method according to claim 2, characterized in that as promoting additives are used compounds of elements selected from, for example, range: Cu, Mn, Al or a mixture.



 

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