Catalyst, method of its preparation and method of purifying butenes of butadiene admixtures

FIELD: chemistry.

SUBSTANCE: this invention relates to heterogeneous catalysis, namely to catalyst and method of purifying butenes of butadiene admixtures. This invention covers the catalyst intended for purifying butenes of harmful admixtures of diene hydrocarbons by selective hydrogenation that contains filamentous carbon bound with nickel alloy and carrier, i.e. aluminium oxide. It differs from known compositions in that it contains filamentous carbon bound with particles of nickel alloy with indium as a promoting addition with its content in (Ni-In)/C catalyst makes 35-80 wt % with nickel-to-indium atomic fraction ratio making 19 to 52. Content of (Ni-In)/C in catalyst makes 96 - 97 wt %, the rest making aluminium oxide. Invention covers also the method of preparing the catalyst intended for purifying butenes of harmful admixtures of diene hydrocarbons by selective hydrogenation that consists in mechanical activation of the mix of nickel oxide, aluminium hydroxide and compound containing promoting additive in centrifugal planetary mill, reducing and cocking up in methane at not less than 550°C and atmospheric pressure. It differs from known methods in that indium acetate is used as promoting additive to produce catalyst that filamentous carbon bound with particles of nickel alloy with indium as a promoting addition with its content in (Ni-In)/C catalyst makes 35-80 wt % with nickel-to-indium atomic fraction ratio making 19 to 52. Content of (Ni-In)/C in catalyst makes 96 - 97 wt %, the rest making aluminium oxide. This invention covers the catalyst intended for purifying butenes of harmful admixtures of diene hydrocarbons by selective hydrogenation in the presence of above described catalyst.

EFFECT: selective hydrogenation of butadiene to butenes at lower hydrogenation of butenes to butane.

5 cl, 2 tbl, 4 ex

 

The invention relates to the field of heterogeneous catalysis, namely the catalyst and the purification method of butenes from impurities butadiene, and may find application in the treatment process of raw materials from harmful impurities diene hydrocarbon processes for the production of plastic and rubber.

Modern production of high-molecular compounds requires a high degree of purification of the monomers from harmful impurities - diene hydrocarbons. The presence of the latter dramatically reduces the rate of polymerization, causes an increase in the formation of low molecular weight rubber (plastic), and also affects the quality of the rubber on the basic parameters.

One way to clean from unwanted impurities diene hydrocarbons is selective catalytic hydrogenation.

Currently offered many varieties of selective hydrogenation catalysts based on metals of group VIII of the Periodic system [Purification of monomers from acetylene hydrocarbons by selective hydrogenation. M: Tsniiteneftehim, 1988; Catalysts and processes for the selective hydrogenation in the petrochemical and chemical industries. M: Tsniiteneftehim, 1993]. However, industrial use of Hydrotreating processes received only Nickel on kieselguhr and palladium on aluminium oxide. The most effective process is the purification of monomers palladium catalysts, deposited on alumina. However, in addition to the high cost of such catalysts are not without other significant deficiencies. For example, it is impossible to obtain bimetallic catalysts with Pd content less than 3 wt.% conventional methods of impregnation. Methods for their preparation, including the use of ORGANOMETALLIC compounds or steam condensation of two metals on the media (in one or two stages), are too complex to be used in traditional industrial production. When using giph-108 have to work with low volume speed (1000 h-1), and because of the low activity to process at high temperatures (up to 165°C) in spite of the high content of the hydrogenating component of the catalyst. Industrial catalyst MA-15 temperature process below, however, adverse reactions occur with the formation of oligomers, which leads to decreased activity and requires periodic regeneration. The oligomerization reaction are accelerated with increasing temperature, an important role in this process belongs to polimerizuet ability of the surface of the carrier - Al2O3characterized by high acidity. In addition, not only the stability but also the possibility of regeneration of used catalysts are often not satisfactory. Thus, the catalyst Pd(S)Al 2O3loses sulfide sulfur as hydrogenation process and catalyst regeneration.

As a prototype of the present invention proposes a catalyst for selective hydrogenation of diene hydrocarbon composition of 10.5 wt.% Nifor 0.9Cua 0.1/C and the method of its preparation. The catalyst produced by the catalytic decomposition of hydrocarbons at temperatures of 550-700°C Nickelodeon alloy catalyst obtained by reduction in hydrogen flow megachilinae a mixture of oxides of Nickel, copper and aluminum. The active component particles are nickelodeo alloy size of about 10 nm on the surface of which there is no crystallographic faces, responsible for the reaction complete hydrogenation to alkanes [You, Web, Rasulov, Nasyreva. New metallovedenie catalysts. I. the Method of preparation, scope // Kinetics and catalysis. 1998. T. No. 3. S-415; You, Web, Rasulov, Nasyreva, Whitenose, Lampreave, Vieru, Ipproved, Binogradov. New metallovedenie catalysts. II. Causes selective effect of Nickel catalysts in hydrogenation reactions // Kinetics and catalysis. 1998. T. No. 3. S-421].

The invention solves the problem of creating a cheap, highly effective catalyst for the selective hydrogenation of butadiene in the environment Moneo is Efimov. The catalyst should provide sufficient depth of hydrogenation of butadiene to butenes in the least degree of hydrogenation of the latter to Bhutan, to be inert to the polymerization of olefins and to reduce costs not contain precious metals.

The task is solved by a catalyst for purification of butenes from harmful impurities diene hydrocarbons by selective hydrogenation containing filamentous carbon associated with particles of Nickel alloy with indium, and the carrier is alumina.

The content of Nickel alloy with indium in (Ni-In)/C catalyst is 35-80 wt.% with respect to the atomic fraction of Nickel/India from 19 to 52.

Content (Ni-In)/C catalyst is 96-97%by weight, the rest of the media is aluminum oxide.

The problem is solved by the method of preparation of the catalyst for purification of butenes from harmful impurities diene hydrocarbons by selective hydrogenation, which consists in megachilini mixture of Nickel oxide, aluminum hydroxide and the compounds containing the promoting additive in a centrifugal planetary mill with subsequent reconstruction and coking in methane at temperatures below 550°C and atmospheric pressure, as the promoting additives use of the Indies, by the above-described catalyst. As compounds containing the promoting additive, use of salt India, for example, the R acetate or nitrate.

The size of the original alloy particles obtained by reduction megachilinae mixture: Nickel oxide, acetate or nitrate India and hydroxide of aluminum, not more than 50 nm.

The task is also solved by a method of purification of butenes from impurities diene hydrocarbons by selective hydrogenation in the presence of a catalyst containing filamentous carbon associated with particles of Nickel alloy with indium as the promoting additive, the content of which in (Ni-In)/C catalyst is 35-80 wt.% with respect to the atomic fraction of Nickel and India from 19 to 52, the content (Ni-In)/C catalyst is 96-97%by weight, the rest of the media is aluminum oxide.

The process is carried out at a temperature of 70-120°C and atmospheric pressure.

The content of diene hydrocarbons in the butenes is 0.1 to 1.0 vol.%.

The distinctive features of such catalysts are particulate alloys associated with carbon fibers, as well as lack of floatable particles leaving the surface crystallographic faces, responsible for the reactions of complete hydrogenation to the corresponding alkanes.

Distinctive features of the catalyst for selective hydrogenation of butadiene in the environment of butenes are: the active component, which represents the particle Ni-In alloy associated with carbon fibers, the ratio of the atomic fraction of Nickel and India is t 19 to 52, the number of filamentous carbon produced per 1 g of the alloy, 1,8-3,3,

The invention is illustrated by the following examples.

Example 1.

A mixture of 3.6 g of Nickel oxide, 0.6 g of aluminum hydroxide (0.24 g monobasic acetate India is subjected to mechanochemical activation in a centrifugal planetary mill for 30 minutes a Sample of 1 g of the sample restore and subjected to coking in methane at 600°C. discharged From the reactor a portion of the sample 2.85 g, containing 3.2 wt.% Al2O3the rest - metallogeny the catalyst composition of 35 wt.% Ni0,981In0,019/C.

Example 2.

Similar to example 1, except that the sample yielding acetate India - of 0.45 was Obtained metallogeny the catalyst has a composition of 3.1 wt.% Al2O3the rest - metallogeny catalyst composition 41,2 wt.% Ni0,964Inbeing 0.036/C.

Example 3.

Similar to example 1, except that the sample yielding acetate India - 0,6, Received metallogeny the catalyst has a composition of 3.0 wt.% Al2O3the rest - metallogeny the catalyst composition of 35 wt.% Ni0,952In0,048/C.

Example 4.

Similar to example 1, except as a source of India use nitrate India, the hinge of which is 0.1 was Obtained metallogeny the catalyst has a composition of 3.5 wt.% Al2O3the rest - metallogeny ka is Aligator composition of 76.9 wt.% Ni 0,964Inbeing 0.036/C.

Thus, as seen from the above examples and tables, the catalyst provides sufficient depth of hydrogenation of butadiene to butenes in the least degree of hydrogenation of the latter to butane, inert to the polymerization of olefins.

Table 1
The degree of purification of butane-butenova fraction of impurities butadiene from the composition of the catalyst and the reaction temperature
The reaction temperature, °CThe content of the butadieneThe content of Bhutan
The initial mixture0,53%11,3%
Example 1 - 35% Ni0,952In0,048/C
900,006%23,0%
105-25,1%
Example 2 - 41,2% Ni0,964Inbeing 0.036/C
650,007%10,8%
70- 11,2%
100-13,9%
Example 3 - 35% Ni0,981In0,019/C
650,009%10,7%
75-11,3%
100-13,6%
Example 4 - 76,9% Ni0,981In0,019/C
1100,002%10,32
120-11,21
(Prototype) of 10.5 wt.% Nifor 0.9Cua 0.1/C
900,008%11,93
95-19,04

Table 2
The test results metallogidridnyh catalysts in the purification of n-butenes from impurities butadiene
The active ingredient The minimum temperature up to 10 ppm, °CThe initial temperature of appearance of C4H10, °C
41,2% Ni0,964Inbeing 0.03670100
10,5% Ni0,952Cu0,0489595

1. The catalyst for purification of butenes from harmful impurities diene hydrocarbons by selective hydrogenation containing filamentous carbon associated with the Nickel alloy, and the carrier is alumina, characterized in that it contains filamentous carbon associated with particles of Nickel alloy with indium as the promoting additive, the content of which in (Ni-In)/C catalyst is 35-80 wt.% with respect to the atomic fraction of Nickel / India from 19 to 52, the content (Ni-In)/C catalyst is 96-97%by weight, the rest of the media is aluminum oxide.

2. The method of preparation of the catalyst for purification of butenes from harmful impurities diene hydrocarbons by selective hydrogenation, which consists in megachilini mixture of Nickel oxide, aluminum hydroxide and the compounds containing the promoting additive in a centrifugal planetary mill with subsequent reconstruction and coking in methane at temperatures below 550°C and atmospheric pressure, the ex is different, however, as the promoting additives used acetate India, you get a catalyst, which contains filamentous carbon associated with particles of Nickel alloy with indium as the promoting additive, the content of which in (Ni-In)/C catalyst is 35-80 wt.% with respect to the atomic fraction of Nickel / India from 19 to 52, the content (Ni-In)/C catalyst is 96-97%by weight, the rest of the media is aluminum oxide.

3. The purification method of butenes from impurities diene hydrocarbons by selective hydrogenation in the presence of a catalyst containing filamentous carbon associated with the Nickel alloy with promoting additive, and the carrier is alumina, characterized in that the use of catalyst containing filamentous carbon associated with particles of Nickel alloy with indium as the promoting additive, the content of which in (Ni-In)/C catalyst is 35-80 wt.% with respect to the atomic fraction of Nickel / India from 19 to 52, the content (Ni-In)/C catalyst is 96-97%by weight, the rest of the media is aluminum oxide.

4. The method according to claim 3, characterized in that the process is carried out at a temperature of 70-120°C and atmospheric pressure.

5. The method according to claim 3, characterized in that the content of diene hydrocarbons in the butenes is 0.1 to 1.0 vol.%.



 

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17 cl, 6 ex, 2 av ex, 19 dwg

FIELD: chemistry.

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2 cl, 2 ex, 1 tbl

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26 cl, 8 tbl, 17 ex

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15 cl, 2 tbl, 5 ex

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20 cl, 24 ex, 5 tbl

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23 cl, 26 tbl, 52 ex

FIELD: chemistry.

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18 cl, 5 tbl

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7 cl, 3 ex, 2 tbl

FIELD: process engineering.

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EFFECT: higher catalytic activity at lower temperature and high selectivity in production of ethylene and polyethylene.

10 cl, 7 tbl, 20 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method for synthesis of caprolactam from alkylcyanovalerate which involves bringing alkylcyanovalerate into contact with hydrogen in gaseous state in the presence of a hydrogenation catalyst and a ring formation catalyst, and treatment after condensation of a gaseous stream containing the formed lactam in order to separate ammonium which may be present, the formed alcohol and/or the caprolactam solvent and extraction of caprolactam, where the hydrogenation catalyst includes a metal element or a mixture of metal elements selected from a group containing an active metal element in form of iron, ruthenium, rhodium, iridium, palladium, cobalt, nickel, chromium, osmium and platinum or several metals from this list, and the ring formation catalyst is porous aluminium oxide.

EFFECT: obtaining caprolactam without intermediate separation of alkylaminocaproate.

10 cl, 5 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to organic synthesis and specifically to synthesis of olefin and diene hydrocarbons through dehydrogenation of paraffin hydrocarbons. The invention describes a method for synthesis of C3-C5 olefins through dehydrogenation of paraffin hydrocarbons in the presence of a catalyst which contains chromium oxide, an alkali metal oxide, oxides of transition metals and a support. The raw material of the process is a mixture of C1-C5 paraffin hydrocarbons, where the said mixture may contain two to seven components.

EFFECT: higher overall conversion of C3-C5 paraffins to olefins, higher overall olefin selectivity of the process.

5 cl, 5 ex, 5 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to catalysts for preparing petroleum fractions with low content of sulphur and nitrogen, methods of preparing such catalysts and processes for hydrofining hydrocarbon material. The invention describes a catalyst for hydrofining hydrocarbon material, having pore volume of 0.3-0.7 ml/g, specific surface area of 200-350 m2/g and average pore diametre of 9-13 nm, and containing a boron compound and a bimetallic complex compound [M(H2O)x(L)y]2[Mo4O11(C6H5O7)2], where: M=Co2+ and/or Ni2+; L is a partially deprotonated form of citric acid C6H8O7; x=0 or 2; y=0 or 1; - 30-45 wt %, a boron compound in amount of 1.06-3.95 wt %, Al2O3 -51.05-68.94 wt %, which corresponds to the following content in a catalyst annealed at 550°C, wt %: MoO3 - 14.0-23.0; CoO and/or NiO - 3.6-6.0; B2O3 -0.6-2.6 Al2O3 - the rest. The catalyst is prepared through saturation of aluminium oxide with a pre-synthesised solution of a bimetallic complex compound [M(H2O)x(L)y]2[Mo4O11(C6H5O7)2] and a boron compound, wherein concentration of the bimetallic compound in the solution provides 40-45 wt % bimetallic complex compound in the ready catalyst. The process of hydrofining hydrocarbon material is carried out at temperature 320-400°C, pressure 0.5-10 MPa, weight flow rate of material of 0.5-5 h-1, volume ratio hydrogen/material equal to 100-1000 m3/m3 in the presence of the catalyst described above.

EFFECT: maximum catalyst activity in target reactions taking place when hydrofining hydrocarbon material, which ensures obtaining petroleum products with low residual content of sulphur.

8 cl, 8 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to catalytic chemistry, specifically to catalysts for oxidation of hydrocarbons in an oxygen-containing gas and methods of preparing said catalysts. The invention describes a catalyst for oxidising hydrocarbons, which contains an active component - manganese oxide and a support in form of granular zirconium oxide with the following content of components, wt %: manganese oxide (MnO2) 5.0-20.0; zirconium oxide (ZrO2) 80.0-95.0. Described also is a catalyst which contains manganese oxide and a granular support made from powdered aluminium oxide in a mixture with crystalline mesoporous aluminium silicate with molar ratio Si/Al equal to 10-60:1, with the following ratio of components, wt %: manganese oxide (MnO2) 5.0-20.0; aluminium oxide (Al2O3) 40.0-85.0; crystalline mesoporous aluminium silicate (AlxSiyOz, where x=0.017-0.1, y=1, z=2.026-2.15) 10.0-40.0. The invention describes a method of preparing catalysts (versions) described above, involving preparation of a support - zirconium oxide or granular mixture of powdered aluminium oxide and crystalline mesoporous aluminium silicate and depositing onto the support manganese oxide, obtained through calcination at 500-600°C of the support saturated with aqueous manganese hydroxide solution after drying in an a temperature interval from 60 to 110°C.

EFFECT: higher catalytic activity and life of the catalyst.

6 cl, 1 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to chemical industry and catalysts used in reactions for gas-phase fluorination of halogenated hydrocarbons. The invention describes a catalyst for fluorination of halogenated hydrocarbons using hydrogen fluoride gas which contains chromium (III) oxide, an aluminium (III) compound whose content is 2-15 wt % in terms of Al2O3, wherein the mixed chromium (III) oxide and aluminium (III) oxide have specific surface area of 130-300 m2/g, pore volume of not less than 0.3 cm3/g and monomodal pore size distribution in the interval 70-300 A, and a metal Me compound selected from a group comprising iron, nickel, cobalt, zinc, copper, magnesium or any of their mixture in amount of 0.1-1.5 wt % in terms of oxide, and the catalyst is in form of cylindrical granules with diametre of 3-10 mm. The invention describes a method of preparing catalysts and a method of fluorinating halogenated hydrocarbons with hydrogen fluoride gas in the presence of the catalyst described above at pressure of 0.1-0.5 MPa, temperature of 260-380°C and molar ratio HF: halohydrocarbon equal to 4:1-40:1.

EFFECT: higher low-temperature activity of the catalyst.

18 cl, 14 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention describes a method of preparing a support for a catalyst for isomerisation of light gasoline cuts, involving mixing aluminium and zirconium hydroxides, extraction, drying and calcination, wherein a hydrate of ortho-tungstic acid is also used during mixture and hydroxides of titanium and/or manganese may or may not be added, and the mixture is stirred at 60-100°C for 2-4 hours. Described also is a support for a catalyst for isomerisation of light gasoline cuts made using the method described above, where the said support contains aluminium and zirconium oxides as well as tungsten oxide and optionally titanium oxide and/or manganese oxide and is a composition of oxides: aAl2O3·bZrO2·cWO3·dMO2, where M - Ti, and/or Mn; a=0.05-0.3; b=0.6-0.9; c=0.005-0.15; d=0 or d=0.001-0.015; a+b+c+d=1.

EFFECT: support made using the method described above has high strength ratio for a catalyst for isomerisation of light gasoline cuts, low content of dust and crumbs resulting in low loss, as well as high activity of the catalyst for isomerisation of light gasoline cuts prepared using said support.

3 cl, 2 tbl, 20 ex

FIELD: oil and gas industry.

SUBSTANCE: invention refers to technology of active alumina stabilised nickel-containing catalysts for redox processes. There is described a method for manufacturing impregnation nickel catalysts for redox processes, e.g. for hydrocarbon conversion, involving carrier impregnation with nickel and aluminium nitrates, drying and ignition; before impregnation, the carrier is heated to temperature exceeding a steam condensation point of the impregnation solution, and the impregnating solution has temperature below a boiling point.

EFFECT: reduced number of impregnation cycles and improving catalyst activity.

2 cl, 2 ex, 1 tbl

FIELD: oil and gas industry.

SUBSTANCE: invention refers to a method and a catalyst-catalytic composition for selective olefin-containing naphtha desulphurisation. There is disclosed a desulphurising catalytic laminate comprising a core and an outer layer attached to the core and containing refractory inorganic oxide with at least one dispersed metal component chosen of the group including cobalt, nickel, molybdenum and tungsten. There is disclosed a desulphurisation method involving contacting of olefin-containing naphtha with said catalytic laminate in a desulphurisation zone and medium to produce low sulphur naphtha flow.

EFFECT: higher desulphurising selectivity of the catalyst with maintaining of high olefin content in the prepared desulphurised naphtha.

11 cl, 1 dwg, 1 ex

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