Method of producing large spherical carbon carrier for catalysts

FIELD: chemistry.

SUBSTANCE: invention relates to the technology of making carbon carriers for different types of catalysts and sorbents. Description is given of a method of making large spherical carbon carrier for catalysts, which involves heating a moving bed of palletised black to 800-900°C, feeding a stream of gaseous or vaporous hydrocarbons in the moving bed, packing the carbon black by thermal decomposition of hydrocarbons on the surface of its particles with formation of pyrocarbon until attaining 0.5-0.7 g/cm3 packed density of carbon black, cooling the mass of the material and its screening with separation of the fraction of granules, which are subjected to repeated pyrolytic packing with subsequent activation of the obtained product. This method is distinguished by that, gaseous or vaporous hydrocarbons are fed into the layer of carbon black at the first and second stages with different bulk speed: at the first stage with speed of 65-72 hour-1, and at the second stage at temperature 650-750°C and speed 52-58 hour-1. Granules with size 3.5-6.0 mm undergo packing at the second stage. Material is activated until attaining void space of 0.3-0.7 cm3/g. At the second stage packing using pyrocarbon is done until attaining weight of granules of 0.88-0.95 g/cm3.

EFFECT: obtaining a carrier with strong and composition homogenous granules.

2 cl, 2 ex

 

The invention relates to the technology for carbon carriers of various catalysts and sorbents.

A method of obtaining carbon granular material, comprising heating a moving layer of pre-classified into fractions by size 0,2-1,0 mm 1,0-3,0 mm 3,0-6,0 mm granulated carbon black in a rotating horizontal reactor, the flow in the moving layer of soot gaseous or vaporous hydrocarbons and their subsequent thermal decomposition of deposition of pyrocarbon on soot. When this process occurs in the temperature 900-1030°C, 800-900°C and 750-800°C for each of these fractions, respectively. In the production of carrier catalysts used fraction of 0.2-1.0 mm for suspension of processes and 2-3 mm for stationary processes in the layer (patent RF №2106375, CL SS 1/60, op. 10.03.1998).

The disadvantage of this method of obtaining carbon granular material is uneven compaction of the pellet fraction 3,0-6,0 mm on all cross-section, as at a temperature of 750-800°C in one stage, the depth of penetration of hydrocarbons in the pores and interparticle space of the material does not exceed 1.5 to 2.0 mm. In these conditions, the granules of carbon black treated with pyrocarbon at half volume and then when you activate the pellet is destroyed.

A method of obtaining carbon carrier for catalysts, cat is which includes heating a moving layer of granulated carbon black, used as the substrate, with a specific surface area of 10 to 30 m2/g and the amount of adsorption of dibutyl phthalate 95-115 ml/100 g, and the flow in the moving layer of soot gaseous or vaporous hydrocarbons which decompose on the surface of soot particles with the formation of a layer of pyrocarbon. This process of carburizing granulated carbon black lead in two stages. In the first stage soot compacted to achieve a bulk density of 0.5-0.7 g/cm3after which the process is stopped, the soot is cooled and subjected to sieving with the release fraction of granules with a size of 1.6-3.5 mm, which is then heated and compacted by pyrocarbon. When reaching the bulk density of the material, 0.9-1.1 g/cm3carry out the activation process. Activation of the material is produced at a temperature of 800-900°C by contact with water vapor or its mixture with the combustion products of the fuel. The process is conducted to obtain a product having a total pore volume, equal to 0.2-1.7 cm3/g (RF patent №2268774, CL B01J 37/08, op. 27.01.2006, prototype)

The disadvantage of this method of obtaining carbon carrier for catalysts is conducting pyrolytic seal of soot in the second stage under the same conditions as the first. This limits the possibility of a uniform volumetric compaction of soot with a granule size of 3.5-6.0 mm to the bulk density higher than 0, g/cm 3necessary to ensure the required strength of the granules after activation.

The aim of the present invention to provide a durable and uniform in properties of the carbon granules media (3,5-6,0 mm Material with these properties is used as a carrier in the preparation of catalysts for chemical processes, which are carried out in a reactor with a fixed bed of catalyst and low hydraulic resistance of the layer.

The proposed method for krupnoporistogo carbon carrier for catalysts includes heating a moving layer of granulated carbon black to a temperature of 800-900°C, feed him in a gaseous or vaporous hydrocarbons with a bulk velocity 65-72 h-1the seal carbon black by thermal decomposition of hydrocarbons on the surface of its particles with the formation of pyrocarbon to achieve a bulk density of carbon black 0.5-0.7 g/cm3cooling of the mass of material and sieving emitting krupnoperistye granules (3,5-6,0 mm Selected fraction of the large granules are subjected to re-pyrolytic condensation at a temperature of 650-750°C and space velocity of the hydrocarbon layer of soot 52-58 h-1to achieve a bulk density from 0.88 to 0.95 g/cm3with subsequent activation of the resulting carbon-carbon material until the value with marnoso pore size of 0.3-0.7 cm 3/year

Distinctive features of the present invention are different speeds of the feed hydrocarbons in a layer of soot on the first and second stages of propatria: the first with a bulk velocity 65-72 h-1and on the second -

52-58 h-1while the process of propatria in the second stage is conducted at a temperature of 650-750°C. And pyrolytic seal is subjected granules 3.5-6.0 mm, and the activation material is produced until the value of the total pore volume of 0.3-0.7 cm3/year

Another hallmark is the process of sealing the pyrocarbon in the second stage to achieve a bulk density from 0.88 to 0.95 g/cm3.

Offered for bid is a set of essential features of the invention allows to obtain a durable and uniform properties of granules (3,5-6,0 mm

The complexity of a uniform volumetric compaction of carbon black pyrocarbon when the granule size of 3.6-6.0 mm is that at high temperatures the layer of granules and high speed feeding of raw materials in the layer decomposition of hydrocarbons on the surface of soot particles in the pellet and the deposition of pyrocarbon happen at high speed. When this first occurs nauglerozhivaniya interparticle space in a surface layer of granules and adjacent soot particles with the formation of dense pyrocarbon the cover, impeding the access of hydrocarbons to the center of the pellets. This circumstance is exacerbated by the carburizing granules that are larger than 3 mm So uniform pyrolytic seal large granules (>3 mm) in the whole volume can be achieved at relatively low temperature layer pellets and feed rate of the hydrocarbon layer. However, this greatly increases the time of the carburizing process and reduce the productivity of the equipment. Therefore, the proposed method at different stages provides optimal for each stage of the process conditions. In the first stage, the process is conducted at 800-900°C and a feed rate of the hydrocarbon 65-72 h-1to the bulk density of 0.5-0.7 g/cm3i.e. before the formation of the "skin" of pyrocarbon. Then after classification in the second stage, the temperature of the layer of granules is reduced to 650-750°C and a flow rate of hydrocarbons to reduce 52-58 h-1.

This provides a reduction in the time seal of soot in the first stage and uniform deposition of pyrocarbon throughout the volume of the granules by reducing the speed of deposition of pyrocarbon on the diameter of the granules in the second stage of the process.

Reducing the feed rate of the hydrocarbon in the first stage below 65 h-1leads to lower productivity and higher to enter the 72 hour -1- to decrease the degree of conversion of hydrocarbons and deposition of pyrocarbon on the pellets of carbon black.

Reducing the temperature of the layer of granules of material in the second stage less than 650°C leads to lower productivity, and higher than 750°C to uneven deposition of pyrocarbon in the volume of the granules. The temperature conditions of the process determine the optimal feed rate of the hydrocarbon in the stratum granulosum of soot.

Decreasing space velocity of the hydrocarbon in the stratum granulosum in the second stage less than 52 hours-1increases the time of carburizing and, accordingly, reduce productivity, and increase the space velocity of the hydrocarbon over 58 h-1may contribute to incomplete decomposition of hydrocarbons on the surface of the particles.

The lower limit of the grain size of 3.5 mm, subjected to pyrolytic condensation in the second stage of the process, due to a limitation of the hydraulic resistance of the layer of granules of catalyst in chemical reactors, and the upper limit is 6.0 mm, limited by the penetration depth of the hydrocarbons in the granules.

The lower limit value of the total pore volume of 0.3 cm3/g - is needed to develop specific surface of the material, and the upper limit is 0.7 cm3/g is limited by the required strength of the granules.

The bottom paragraph is published by third parties the value of the bulk density of the granules is 0.88 g/cm3to which the lead seal in the second stage, due to the need to obtain granules with high strength carrier, and its upper limit is 0.95 g/cm3that limited the performance of the process, since a further increase in bulk density of the material increases production time.

The effectiveness of the proposed method and the necessity of its implementation to achieve the goal is illustrated by the following examples.

Example 1 (the prototype). In a preheated 400 With horizontal rotating reactor load 200 kg of granulated carbon black with a grain size of 1.0-6.0 mm and a specific surface area of 50 m2/, Then the reactor is heated to 850°C and in the layer continuously stir the carbon black pellets with a bulk velocity 69 h-1serves propane-butane mixture containing 50% propane and 50% butane. After pyrolytic seal soot for 20 hours until the value of the bulk density of the soot 0.6 g/cm3, carburizing stop, the material is cooled and classified into different fractions. For further work are selected fraction with grain sizes of 3.5 to 6.0 mm, Then the material is loaded into the heated reactor is again heated to 850°C. Then, in the layer continuously stir the material with the same bulk velocity serves propane-butane mixture of the same composition that lane on the stage,. After carburizing material for 15 hours to achieve a bulk density of 1.0 g/cm3feeding hydrocarbons stop, but instead for 15 hours serves a steam-air mixture. Activation of the material is conducted to obtain material with a total pore volume equal to 0.55 cm3/year

Properties of the obtained product:

bulk density0.40 g/cm3
the specific surface520,0 m2/g
the total pore volume0,55 cm3/g
the crushing strength60,0 kg/cm
the coefficient of variation0,63
(in terms of crushing strength)

The coefficient of variation, which represents a relative measure of dispersion, expressed in percent, was calculated by the standard method.

Example 2 (present invention). The process of carbonization of carbon black in the first stage are as in example 1, but in the second stage and lower the processing temperatures up to 700°C, and the volumetric feed rate of the propane-butane mixture is about

55 h-1. The carburizing process in the second stage is carried out to achieve a bulk weight of the product of 0.90 g/see Activation material is conducted to obtain material with a total pore volume equal to 0.50 cm3/year

Properties of the obtained product:

bulk density0.52 g/cm3
the specific surface480 m2/g
the total pore volume0,50 cm3/g
the crushing strength120,0 kg/cm
the coefficient of variation0,52
(in terms of crushing strength)

Thus, the analysis of the above data shows that the organization of the process of obtaining krupnoporistogo carbon carrier for catalysts with the use of the invention allows to obtain a product with a more solid and homogeneous granules. These properties allow it to be used as an effective carrier for catalysts used in various chemical processes, such as hydrogenation of fatty acids, the dehydrochlorination of methanol and others.

1. The method of obtaining krupnoporistogo carbon carrier for catalysts comprising heating a moving layer of granulated carbon black to a temperature of 800-900°C, the flow in the stream of gaseous or vaporous hydrocarbons, seal carbon black by thermal decomposition of hydrocarbons on the surface of its particles with the formation of pyrocarbon to achieve a bulk density of carbon black 0.5-0.7 g/cm3cooling of the mass of material and sieving emitting fraction of granules, which are subjected to a re-pyrolytic condensation with subsequent activation of the obtained product, characterized in that the gaseous or vaporous hydrocarbons are served in a layer of soot on the first and second stages with different bulk velocity: at the first stage - speed 65-72 h-1and on the second stage at a temperature of 650-750°C at the rate 52-58 h-1and pyrolytic condensation in the second stage is subjected granules 3.5-6.0 mm, and the activation material lead until the value of the total pore volume of 0.3-0.7 cm3/year

2. The method according to claim 1, characterized in that in the second stage seal pyrocarbon are to achieve a bulk density of pellets from 0.88 to 0.95 g/cm3.



 

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15 cl, 1 ex, 1 tbl, 1 dwg

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1 tbl, 6 ex

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21 cl, 4 tbl, 14 cl

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10 cl, 3 dwg, 2 tbl

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11 cl, 3 tbl, 16 ex

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5 cl, 1 tbl, 3 dwg, 2 ex

FIELD: chemistry.

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5 cl, 2 tbl, 31 ex

FIELD: chemistry.

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EFFECT: material with enhanced adsorption surface.

1 tbl, 21 ex

FIELD: metallurgy.

SUBSTANCE: alloy contains (wt %): from 2.5 till 5.0% Al, from 10 till 25% Cr and from 0.05 till 0.8% Si, and also admixtures from >0.01 till 0.1% Y and/or from >0.01 till 0.1% Hf, and/ or from >0.01 till 0.2% Zr, and/ or from >0.01 till 0.2% of misch metal with high content of cerium (Ce, La, Nd), and also attached foreign material and it is used for manufacturing details of diesel or two-cycle engine. Those details are: foil - carrier of metallic catalyst of discharge gases neutralisation, heater element or resistance material for electrical heating of purification system of discharge gas.

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8 cl, 2 dwg, 1 tbl

FIELD: chemistry.

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86 cl, 1 dwg, 2 tbl, 10 ex

FIELD: chemistry.

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EFFECT: elaboration of the catalyst synthesis method on the base of the noble metals sulphides in water media without using of highly inflammable and highly toxic compounds.

12 cl, 4 ex

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