Carbon catalyst support preparation method

FIELD: carbon materials.

SUBSTANCE: invention relates to porous carbon materials and, more specifically, to carbon catalyst supports and sorbents. Preparation of catalyst support is accomplished by treating carbon black with hydrocarbon gas at heating and stirring until mass of carbon material increases by 2-2.5 times, after which resulting compacted material is oxidized, said hydrocarbon gas being gas originated from liquid hydrocarbon electrocracking and said treatment being carried out at 400-650°C.

EFFECT: simplified technology.

1 tbl, 6 ex

 

The invention relates to the field of porous carbon materials that are used in Hydrotreating processes, hydrogenation of hydrocarbons and the synthesis of hydrocarbons by the Fischer-Tropsch.

Intensive development of the research and development of new high-performance processes of catalysis and adsorption requires expanding the range of porous media, including carbon carriers having a high absorptive capacity.

Known carbon carriers [USSR Author's certificate 1352707 A1, B01J 37/10, 35/10, 21/18. Publ. 10.07.1996]obtained the seal of soot by pyrocarbon formed by the decomposition of hydrocarbons, and subsequent treatment of formed material vapor mixture.

The disadvantage of these methods is the low stability with respect to physico-mechanical effect.

The closest technical solution achieved the effect is [USSR Author's certificate 1453682 A1, 01J 37/08, 21/18, 32/00. Publ. 10.09.1996]. According to him, the carbon material obtained by processing carbon black propane-butane gas mixture under stirring and the temperature 750-1200°before the formation of compacted carbon material with subsequent processing of the vapor mixture.

The disadvantage of this method is the high temperature decomposition of the hydrocarbon gas.

Technical is the definition of the invention is to reduce the temperature of decomposition of the hydrocarbon gas, that will reduce the cost of obtaining carbon media.

This technical result is achieved that the sealing soot is carried out at temperatures amounts to 400-650°C due To the decomposition applied to the mixture with her gas electrocoating liquid hydrocarbons whose composition, vol.%: H2- 60-80, CH4- 1-5, With2H6- 0,15-0,5, C2H4- 1-16, With3H6- 0,2-1, C2H2- 10-24. More detailed information about the decomposition of hydrocarbons in an electric arc and the composition of the produced gas is given in [editor Dragunov AS Chemical reactions of organic products in electric discharges. M.: Nauka, 1966, 199 S.]. Compacted to increase the weight of the sample in 2-2,5 times the material was then subjected to oxidation.

Examples illustrating the invention.

Example 1.

In a quartz reactor with a diameter of 20 mm load ˜0.5 g of carbon black with specific adsorption surface 100 m2/greater purge with inert gas and heated to a temperature of 650°C. Upon reaching this temperature, with continuous stirring, the reactor serves gas electrocoating liquid hydrocarbons with a flow rate of 150 ml/min. and the gas Flow is to increase the sample mass 2 times due to thermal decomposition of the hydrocarbon gas. The resulting material is subjected to oxidation. Okislyayutsya until while the weight loss (oxidation) will not be 50%. Output process indicators presented in the table.

Example 2.

In a quartz reactor with a diameter of 20 mm load ˜0.5 g of carbon black with specific adsorption surface 100 m2/year / Reactor purge with inert gas and heated to a temperature of 500°C. Upon reaching this temperature, with continuous stirring, the reactor serves gas electrocoating liquid hydrocarbons with a flow rate of 150 ml/min. and the gas Flow is to increase the weight of the sample is 2.2 times due to thermal decomposition of the hydrocarbon gas. Oxidation continues until the degree of oxidation will not be 50%. Output process indicators presented in the table.

Example 3.

In a quartz reactor with a diameter of 20 mm load ˜0.5 g of carbon black with specific adsorption surface 100 m2/year / Reactor purge with inert gas and heated to a temperature of 400°C. Upon reaching this temperature, with continuous stirring, the reactor serves gas electrocoating liquid hydrocarbons with a flow rate of 150 ml/min. and the gas Flow is to increase the sample mass 2.5 times due to thermal decomposition of hydrocarbon gas. The resulting material is subjected to oxidation. Oxidation continues until the degree of oxidation will not be 50%. The weekend show is whether the process is presented in the table.

Example 4.

The carbon carrier was obtained by the method of example 1. Differences: temperature seals soot - 300°C. Output process indicators presented in the table.

Example 5.

The carbon carrier was obtained by the method of example 2. Differences: temperature seals soot - 700°C. Output process indicators presented in the table.

Example 6.

The carbon carrier was obtained by the method of example 1. Differences: as the hydrocarbon gas used was a mixture containing 50 vol.% propane and 50% vol. butane. Output process indicators presented in the table.

The stability of the obtained media to physico-mechanical stress was determined by its ability to adsorb methyl orange from aqueous solution. Physico-mechanical impact of the media were subjected to the example of the prototype. The results are presented table.

Table

Output indicators under seal in obtaining carbon media
Carbon materialThe seal of the source materialSorption activity, mg/g
The conversion of acetylene, %The output of carbon, g/lTo physico-mechanical effects After physico-mechanical effectsThe loss of sorption activity, %
The placeholder--˜100not determined-
For example 11000,271401353,6
For example 21000,231321255,3
For example 3890,151251158,0
In example 4100,051201099,2
For example, 51000,271401362,9
In example 6-0,171291188,5

From the presented data shows that the use of gas electrocoating liquid hydrocarbons can significantly lower the temperature of the densification process of soot while maintaining stability of the sample to the physico-mechanical effect.

The method of obtaining carbon catalyst carrier by processing of soot in hydrocarbon gas while heating and stirring to increase the weight of the material in 2÷2,5 the Aza with subsequent oxidation of the resulting material, characterized in that the hydrocarbon gas use gas electrocleaning liquid hydrocarbons and the treatment is carried out at a temperature amounts to 400-650°C.



 

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1 ex

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SUBSTANCE: claimed method includes silicate reaction with acidifying agent to produce silicium dioxide slurry separation and drying of said slurry, wherein reaction is carried out according to the next steps: i) providing base aqueous solution with pH from 2 to 5, preferably from 2.5 to 5; ii) simultaneous addition silicate and acidifying agent to said base solution maintaining solution pH from 2 to 5, preferably from 2.5 to 5; iii) addition silicate only without acidifying agent to produce pH from 7 to 10, preferably from 7.5 to 9.5; (iv) simultaneous addition silicate and acidifying agent to reaction medium to maintain pH from 7 to 10, preferably from 7.5 to 9.5; (v) addition acidifying agent only without silicate to produce reaction medium pH below 6. Obtained high structured silicium dioxides have the next characteristics: CTAB specific surface (SCTAB) is 40-525 m2/g; BET specific surface (SBET) is 45-550 m2/g; width Ld ((d84-d16)/d50) of particle size distribution measured by XDC grading analysis after ultrasound grinding is at least 0.92; and such pore distribution that V(d95-d50)/V(d5-d100) is at least 0.66.

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FIELD: production of carbon carrier for catalysts.

SUBSTANCE: proposed method includes heating of moving layer of granulated furnace black used as backing, delivery of gaseous or vaporous hydrocarbons into soot layer followed by their thermal decomposition on soot surface forming layer of pyrocarbon at forming of layer of pyrocarbon and activation of material compacted by pyrocarbon at temperature of 800-900°C and unloading of finished product. Granulated furnace black at specific surface of 10-30 m2/g and adsorption rate of 95-115 ml/100 g is used as backing for compacting with pyrocarbon. Then, product is subjected to activation for obtaining total volume of pores of 0.2-1.7 cm3/g. Black is compacted by pyrocarbon at two stages: at first stage, granulated black is compacted to bulk density of 0.5-0.7 g/cm3, after which material is cooled down and screened at separation of fraction of granules of 1.6-3.5 mm; at second stage, this fraction is subjected to repeated pyrolytic compacting to bulk density of granules of 0.9-1.1 g/cm3.

EFFECT: enhanced economical efficiency; increased productivity of process.

3 ex

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