Catalyst of hydrogenation of arenes and the method of its preparation

FIELD: chemical industry; petrochemical industry; other industries; methods of production of the catalysts of hydrogenation of arenes.

SUBSTANCE: the invention is pertaining to the field of the catalytic chemistry, in particular, to production of the catalysts used for dearomatization of the diesel fractions. The invention presents the catalyst for hydrogenation of the arenas containing platinum the carrier, which aluminum oxide containing of no more than 500 ppm of impurities in the mixture with the crystalline mesosculiferous aluminosilicate with the molar ratio of Si/Al equal to 10-60 at the following contents of the ingredients (in mass %): platinum (Pt) - 0.15-0.60; aluminum oxide (AI2O3) - 59.85-94.4; crystalline mesoosculiferous aluminosilicate (AlxSiyOz) - 5-40, where х = 0.017 - 0.1; y = 1; z = 2.026 - 2.15. The invention also presents the method of preparation of the catalyst of hydrogenation of the arenes providing for production of the carrier, deposition of platinum on the carrier by the method of the competitive impregnation from the combined solution of the carrier from the joint solution of the chloroplatinic acid, acetic acid and hydrochloric acid the subsequent drying, and burning, differing that the carrier is produced by mixing of the powdery aluminum oxide containing of no more than 500 ppm of the impurities, and the crystalline mesoosculiferous aluminosilicate AlxSiyOz, (where х = 0.017 - 0.1; y = 1; z = 2.026 - 2.15), with the molar ratio molar ratio of Si/Al equal to 10-60, humidification of the produced mixture and the jellification by the 1.5 - 5 % solution of the nitric acid. The technical result of the invention is the increased hydrogenating activity of the catalyst.

EFFECT: the invention ensures the increased hydrogenating activity of the catalyst.

3 cl, 2 tbl, 4 ex

 

The technical field to which the invention relates.

The invention relates to catalytic chemistry, in particular to catalysts dearomatization diesel fractions, and more particularly to a catalyst for the hydrogenation of hydrocarbons and method of its preparation, which can be used in the oil industry.

The level of technology

A known catalyst for the hydrogenation of arenes containing the VIII group metals (Pt, Pd)deposited on γ-AL2About3(J.-R.Chang. S.-L.Chang, Catalytic Properties of γ-Alumina-Supported Pt Catalysts for Tetralin Hydrogenation, Journal of Catalysis (1998), CH, No. 1, SS-51). Known catalysts, including Pt deposited on the tungsten and zirconium, or zeolite BETA (M.A.Arribas and others, Activity, selectivity values and Sulfur Resistance of Pt/WOx-ZrO2and Pt/Beta Catalysts for the Simultaneous for Hydroisomerization of n-Heptane and Hydrogenation of Benzene, Journal of Catalysis (2000), CH, No. 2, SS-319).

The disadvantage of these catalysts is the low hydrogenation activity.

Closest to the proposed invention is a catalyst for the hydrogenation of arenes containing Pd,Pt, deposited on mesoporous silicate with a molar ratio Si/Al equal to 20 (M.Jacquin and others, Cetane improvement of diesel with a novel bimetallic catalyst, Journal of Catalysis (2004), CH, No. 2, SS-459).

The disadvantage of this catalyst is not sufficiently high hydrogenating activity at low temperatures the degree of hydrogenation of arenes under pressure the Sri hydrogen 6,0 MPa is 60-89% and up to 95% Rel. only at 280°C.

Closest to the proposed in the invention method is a method of preparation of the catalyst for reforming of gasoline fractions, including the stage of impregnation of calcined Al2About3solutions of hexachloroplatinic, hydrochloric acid or acetic acid and ammonium perrhenate, drying, annealing with simultaneous recovery of platinum (patent RF 2245190, 2004).

The invention

The objective of the invention is to develop a highly active catalyst for the hydrogenation of arenes that are included with diesel and oil fractions, and the method of its preparation.

Technical result achieved when implementing the claimed invention is to increase the hydrogenation activity of the catalyst.

The technical result is achieved by the fact that the catalyst for the hydrogenation of arenes contains platinum on a carrier comprising alumina, aderrasi not more than 500 ppm of impurities in a mixture with crystalline mesoporous aluminum silicate with a molar ratio Si/Al equal to 10-60, with the following content, wt.%:

tr>
platinum (Pt)0,15-0,60
aluminum oxide (Al2About3)59,85-94,4
crystalline mesoporous aluminosilicate (AlxSiyOz),
where x=0,017-0,1, y=1, z=2,026-2,155-40

The claimed invention allows to significantly increase the degree of hydrogenation of arenes by using the ratio of components and aluminum oxide of high purity.

The technical result is also achieved by the fact that the preparation method of catalyst for the hydrogenation of arenes includes receiving media, drawing on media platinum by the method of competitive impregnation of the joint solution of hexachloroplatinic, acetic and hydrochloric acids, subsequent drying and calcination, and the carrier is produced by mixing a powder of aluminum oxide containing not more than 500 ppm of impurities and crystalline mesoporous aluminosilicate AlxSiyOz(where x=0,017-0,1, y=1, z=2,026-2,15) with a molar ratio Si/Al equal to 10-60, moistening the mixture and gelation of 1.5-5%solution of nitric acid.

Preferably, the gelation moistened mixture to carry out at a temperature of 5-10°and With stirring.

The technical result of the invention is significantly higher hydrogenation activity of the catalysts prepared by the proposed method.

In the particular case of carrying out the invention, the content of impurities in the aluminum oxide is preferably not more than 500 ppm.

Technical is the second result of the invention is significantly higher hydrogenation activity of the catalysts, prepared by the proposed method. Thus, the degree of hydrogenation of arenes, including monocyclic, on the catalysts prepared by this method, when the hydrogen pressure of 3.0 MPa, is maintained at a high level 93-99% Rel. in the whole temperature range 220-340°and may even exceed 99% Rel. at 280°C.

Information confirming the possibility of carrying out the invention

The method of preparation of the catalyst is that high-purity powdered aluminum oxide, in which the total content of impurities (sodium oxide (Na2O), ferric oxide (Fe2About3) and titanium oxide (TiO2)) preferably does not exceed 500 ppm, moisturize first and then heliroute 1.5 to 5%nitric acid solution, and then in a jelly-like mass is added 5-40% crystalline mesoporous aluminosilicate with a molar ratio Si/Al equal to 10-60, under continuous stirring at a temperature of 5-10°C. the resulting carrier formed into pellets, dried, calcined and impregnated carrier joint solution of hexachloroplatinic, acetic and hydrochloric acids.

The invention is illustrated by the following examples.

Example 1.

78.5 per g of wet alumina powder, the content of impurities which do not exceed 500 ppm, mixed with 51.7 g of wet powder crystalline mesoporous alumosilicates molar ratio Si/Al=10. The mixture is first moistened with distilled water, and then with vigorous stirring, a mixture heliroute 1.5% solution of nitric acid at a temperature of 5°C. the Obtained plastic mass media formed into cylindrical pellets by extrusion.

Granules of the carrier is dried at room temperature for 24 h, then dried in a stream of air for 2 h at 60°C, 2 h at 80°C, 2 h at 120°C. the Dried granules media then calcined in air flow at 550°C for 3 h with the rise of temperature of calcination 100°With in the hour.

of 99.85 g of calcined carrier vacuum for 30 min, and then placed in a 150 ml joint impregnating solution containing 315 mg of hexachloroplatinic acid, 3.0 g of 98.5% concentrated acetic acid and 2,78 g of 37% concentrated hydrochloric acid.

Impregnation of the carrier is carried out at room temperature for 1 h, and then at a temperature of 80°C for 3 h with constant stirring. The excess impregnating solution is separated by decantation.

The catalyst is dried in a stream of air for 2 h at 60°C, 2 h at 80°C, 2 h at 100°C, 2 h at 120°C and 2 h at 140°C.

The composition of the obtained catalyst, wt.%:

Platinum (Pt)0,15
Aluminum oxide (Al2About3) 59,85
Crystalline mesoporous aluminosilicate (AlxSiyOz,
where x=0,017-0,1, y=1, z=2,026-2,15)40,00
with a molar ratio Si/Al=10

Example 2.

of 104.5 g of wet alumina powder, the content of impurities which do not exceed 500 ppm, mix 25.2 g of wet powder crystalline mesoporous aluminosilicate with a molar ratio Si/Al=30. The mixture is first moistened with distilled water, and then with vigorous stirring, a mixture heliroute a 3.0% solution of nitric acid at a temperature of 7.5°C. the Obtained plastic mass media formed into cylindrical pellets by extrusion.

Granules media dried, dried and calcined as in example 1.

99,60 g of calcined carrier vacuum for 30 min, and then placed in a 150 ml joint impregnating solution containing 841 mg of hexachloroplatinic acid, 3.0 g of 98.5% concentrated acetic acid and 2.77 g of 37% concentrated hydrochloric acid.

The impregnation of the support and drying of the catalyst is carried out analogously to example 1.

The composition of the obtained catalyst, wt.%:

Platinum (Pt)0,40
The aluminum oxide is (Al 2About3)79,60
Crystalline mesoporous aluminosilicate (AlxSiyOz,
where x=0,017-0,1, y=1, z=2,026-2,15)20,00
with a molar ratio Si/Al=30

Example 3.

123,9 g wet powder of aluminum oxide, the content of impurities which do not exceed 500 ppm, mixed with 6.3 g of wet powder crystalline mesoporous aluminosilicate with a molar ratio Si/Al=60. The mixture is first moistened with distilled water, and then with vigorous stirring, a mixture heliroute 5,0% solution of nitric acid at a temperature of 10°C. the Obtained plastic mass media formed into cylindrical pellets by extrusion.

Granules media dried, dried and calcined as in example 1.

99,40 g of calcined carrier vacuum for 30 min, and then placed in a 150 ml joint impregnating solution containing 1261 mg platinochloride Noi acid, 2,99 g of 98.5% concentrated acetic acid and 2.76 g of 37% concentrated hydrochloric acid.

The impregnation of the support and drying of the catalyst is carried out analogously to example 1.

The composition of the obtained catalyst, wt.%:

Platinum(Pt)0,60
Aluminum oxide (Al2About3)94,40
Crystalline mesoporous aluminosilicate (AlxSiyOz,
where x=0,017-0,1, y=1, z=2,026-2,15)5,00
with a molar ratio Si/Al=60

Example 4.

of 104.5 g of wet alumina powder obtained by precipitation aluminate way, the impurity content of which is 2000 ppm (including Fe2About3200 ppm, Na2O 200 ppm), mixed 25.2 g of wet powder crystalline mesoporous aluminosilicate with a molar ratio Si/Al=30. The mixture with vigorous stirring heliroute a 3.0% solution of nitric acid at a temperature of 7.5°C. the Obtained plastic mass media formed into cylindrical pellets by extrusion.

Granules media dried, dried and calcined as in example 1.

99,60 g of calcined carrier vacuum for 30 min, and then placed in a 150 ml joint impregnating solution containing 841 mg of hexachloroplatinic acid, 3.0 g of 98.5% concentrated acetic acid and 2.77 g of 37% concentrated hydrochloric acid.

The impregnation of the support and drying of the catalyst is carried out analogously to example 1.

The composition of the obtained catalyst, wt.%:

Platinum (Pt)0,40
Aluminum oxide (Al2About3)79,60
Crystalline mesoporous aluminosilicate (AlxSiyOz,
where x=0,017-0,1, y=1, z=2,026-2,15)20,00
with a molar ratio Si/Al=30

The catalysts prepared according to examples 1, 2, 3, 4, was tested for activity in the hydrogenation reactions of arenes in the laboratory running the installation under hydrogen pressure at model raw. The composition model of the raw materials shown in table 1. Conditions and results of tests of the catalysts are presented in table 2. The activity of the catalysts was evaluated by the degree of hydrogenation of arenes, expressed in % relative. For comparison, table 2 shows the data obtained when testing the aluminium oxide-platinum catalysts: similar catalyst E-801 R (0.4 wt.% Pt on a γ-Al2About3), the prototype of 0.4 wt.% Pt on the mesoporous aluminosilicate brand SIRAL 30

Table 1
Component composition model materials
ComponentContent, wt.%
Toluene14,2
n-Octane26,9
ISO-Octane 0,04
n-Nonan26,1
out-Nonan0,03
n-Decane25,5
TRANS-Decalin0,02
CIS-Decalin0,02
Tetralin4,60
Naphthalene2,54
Other0,05
Total100

Industrial applicability

The proposed catalyst for the hydrogenation of arenes that are included with diesel and oil fractions, and the proposed method of its preparation can be used in the oil industry.

1. The catalyst for the hydrogenation of arenes containing platinum on a carrier comprising alumina containing not more than 500 million-1impurities in a mixture with crystalline mesoporous aluminum silicate with a molar ratio Si/Al equal to 10-60, with the following content, wt.%:

platinum (Pt)0,15-0,60
aluminum oxide (Al2About3)59,85-94,4
crystalline mesoporous
the aluminosilicate (AlxSiyOz),
DG is x=0,017-0,1, y=1, z=2,026-2,155-40

2. The preparation method of catalyst for the hydrogenation of arenes, including the production of media, drawing on media platinum by the method of competitive impregnation of the joint solution of hexachloroplatinic, acetic and hydrochloric acids, subsequent drying and calcination, wherein the carrier is produced by mixing a powder of aluminum oxide containing not more than 500 million-1impurities and crystalline mesoporous aluminosilicate AlxSiyOz(where x=0,017-0,1, y=1, z=2,026-2,15), with a molar ratio Si/Al equal to 10-60, moistening the mixture and gelation of 1.5-5%solution of nitric acid.

3. The method according to claim 2, characterized in that the gelation moistened mixture is carried out at a temperature of 5-10°and With stirring.



 

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21 cl, 3 tbl

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SUBSTANCE: proposed carrier has metal base made from chromium and aluminum alloy and/or metallic chromium and coat made from chromium of aluminum oxides or oxides of chromium, aluminum, rare-earth elements or mixture of them. Method of preparation of carrier includes forming of metal powder containing aluminum and other powder-like components and calcination of carrier at solid phase sintering point; used as additional component of metal powder is powder-like chromium; mixture thus obtained is subjected to mechanical activation and is placed in mold accessible for water vapor, after which it is subjected to hydro-thermal treatment and molded product is withdrawn from mold, dried and calcined at respective temperature; then additional layer of aluminum and rare-earth elements oxides or mixture of solutions and suspensions is applied on calcined product followed by drying and calcination.

EFFECT: increased specific surface; enhanced heat resistance of carrier.

8 cl, 1 tbl, 5 ex

FIELD: chemical industry; methods of production of zirconium oxides

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the methods of obtaining of zirconium oxide for production of the catalytic agents used, for example, in the reactions of the organic synthesis. The invention presents the method of obtaining of zirconium oxide for production of the catalytic agents, which includes the operations of dissolution of the zirconium salt in water, treatment of the solution with the alkaline reactant, settling of the metals hydroxides, filtration, separation of the mother-liquor from the settlings, the settlings water flushing, its drying, calcination and granulation and-or granulation by molding. At that dissolution of the source zirconium chloride and-or zirconium oxychloride is conducted in the sodium chloride solution with concentration of 200-250 g/dc3 till reaching of the concentration of zirconium of 20-120 g/dc3. Settling of zirconium oxyhydrate is conducted by the adding the initial chloride solution in the solution of the sodium hydroxide with concentration of 20-80 g/dm3 up to reaching the suspension pH equilibrium value - 5-8. Then the suspension is filtered up to the zirconium oxyhydrate pasta residual humidity of 40-80 %. The mother chloride solution is separated from the settlings of zirconium oxyhydrate and again use it for dissolution of the next batch of zirconium chloride and-or zirconium oxychloride. The settlings of zirconium oxyhydrate are subjected to drying at 80-100°C within 2-6 hours, then the dry settlings are suspended in the water at the ratio of liquid to solid L:S = (5-10 :1, the suspension is filtered, the sediment on the filter is flushed by water, the chlorides are wash off up to the residual concentration of ions of chlorine in the flush waters of 0.1-0.5 g/dm3, divided into 2 parts, one of which in amount of 60-80 % is subjected to drying and calcinations at the temperatures of 300-600°C, and other part in amount of 20-40 % is mixed with the calcined part of the settlings and subjected to granulation by extrusion at simultaneous heating and dehydration of the damp mixture of zirconium oxide and zirconium oxyhydrate with production of the target product. The technical result of the invention is improvement of quality of the produced zirconium oxide for production of the catalytic agents due to provision of the opportunity to use ZrO2 for the subsequent production of the various catalytic agents of the wide range of application and thereby improving the consumer properties of the produced production.

EFFECT: the invention ensures improvement of the quality of the produced zirconium oxide for production of the catalytic agents with improved consumer properties.

1 ex

FIELD: technology for silicium dioxide production useful as additive for polymer reinforcement.

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.

EFFECT: improved material for polymer reinforcement.

FIELD: petrochemical process catalysts.

SUBSTANCE: invention provides paraffin isomerization catalyst containing platinum or palladium and γ-alumina as binding material and zeolite selected from zeolite beta and/or ZSM-5, zeolite beta and/or mordenite, and mesoporous aluminosilicate of the type Al-MCM-41 at following proportions: platinum and/or palladium 0.2-0.3%, zeolite (beta and/or ZSM-5, beta and/or ZSM-12, beta and/or mordenite) 30-60%, mesoporous aluminosilicate 5-20%, and γ-alumina the rest. In another embodiment, catalyst contains composite material BEA/Al-MCM-41, which is mixture of zeolite beta and mesoporous aluminosilicate Al-MCM-41 at following proportions: platinum and/or palladium 0.2-0.3%, composite material BEA/Al-MCM-41 30-60%, zeolite (ZSM-5 or ZSM-12, or mordenite) 0-10%, and γ-alumina the rest.

EFFECT: increased catalyst stability and selectivity with regard to 2,2-dimethylbutane, and reduced catalyst preparation time.

2 cl, 1 tbl, 25 ex

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