C4-c16 isoalkane synthesis method

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing a mixture of C4-C16 isoalkanes by bringing aliphatic alcohol - ethanol, 2-methyl-1-propanol, 3-methyl-1-butanol in an inert gas medium at 300-420°C, pressure 30-80 atm, bulk speed 0.2-0.8 h-1, into contact with a catalyst composition, which contains a hydride phase of an iron-titanium intermetallic compound, modified with group IV-VII metals, aluminium-platinum catalyst and a transition metal oxide, characterised by that, the transition metal oxide used is magnesium oxide in mass ratio 10:1:(0.8-1.2).

EFFECT: catalyst used in the method is highly active for a long period of time and the given method also widens the raw material base of aliphatic alcohols used.

1 cl, 7 ex, 1 tbl

 

The invention relates to the field of heterogeneous-catalytic transformations of organic compounds and, more particularly, to catalytic conversion of aliphatic alcohols in the mixture of isoalkanes C4-C16.

Fraction of alkanes, isotrate, as you know, are the most valuable components of motor fuel, providing a high octane number, low pour point, and high calorific value along with high storage stability.

In addition to fuels isoalkanes demand as solvents and thinners many organic industrial materials.

Given that one of the main sources of environmental pollution is transportation, in recent times there are specific requirements for the composition of the fuel, resulting in increased demand for isoalkanes, the most acceptable from an environmental point of view.

Known single-stage method of producing hydrocarbons From5from methanol in the presence of zeolite properties molecular filter [CN 1923770, class SS 1/20, SS 1/00, date 07.03.2007]. The disadvantages of this method include low concentration of isoalkanes and narrow fractional composition of the light part of the gasoline fraction. Also used as a raw material is not alcohol biological origin is.

[EN 2220940, class SS 1/20, SS 9/16, date 10.01.2004] describes a method for isoalkanes by contacting an aliphatic alcohol is Isobutanol or isopentanol in an inert gas environment at 300-420°C, a pressure of 30-80 MPa, flow rate of 0.1-0.8 h-1with a catalytic composition comprising a hydride phase celestianpower intermetallic compounds (IMC), modified with metals of IV-VII groups, and aluminium oxide-platinum or ecumenically catalyst, taken in a mass ratio of 10:1.

The disadvantage of this method is that it can be used for a limited number of bioportal, while not one of the most common - ethanol.

Also known the method according to [EN 2220941, option 1, class SS 1/20, SS 9/16, date 10.01.2004], according to which 40-60% aqueous solution of ethanol exposed in the environment of carbon dioxide at 350-380°C, a pressure of 8-12 bar and a flow rate of 0.2-0.8 h-1, with a catalytic composition consisting of IC, modified with metals of IV-VII groups, and γ-alumina, taken in a mass ratio of 10:1.

The disadvantage of this solution is the high yield of oxygenates, as well as low content of isoalkanes in alanovoy fraction4-C16.

The closest solution to obtain a mixture of isoalkanes is the work of [RU 2220941, option 2, class SS 1/20, SS 9/16, date 10.01.2004]. Danna is the method involves contacting 40-60% aqueous solution of ethanol, Isobutanol and isopentanol, taken in a mass ratio of 6:1:2, with a catalytic composition consisting of IC, modified with metals of IV-VII groups, aluminium oxide-platinum catalyst and γ-alumina (oxide non-transition metal) in the mass ratio of the components in the composition of 10:1:1, in an inert gas environment at 300-420°C, a pressure of 30-80 bar and a flow rate of 0.2-0.8 h-1.

The disadvantage of this method is the small period of time (10-12 hours) maintain a high activity catalyst composition.

The technical result of the invention is to maintain high activity of the catalyst over an extended period of time.

This technical result is achieved by a method of obtaining isoalkanes C4-C16by contacting an aliphatic alcohol - ethanol, 2-methyl-1-propanol, 3-methyl-1-butanol in an inert gas (nitrogen, argon or carbon dioxide) at 300-420°C, a pressure of 30-80 MPa, flow rate 0,2-0,8 h-1with a catalytic composition comprising the IC, modified with metals of IV-VII groups, aluminium oxide-platinum catalyst and the oxide non-transition metal is used MgO, taken in the mass ratio 10:1:(0,8-1,2).

The conversion of ethanol, 2-methyl-1-propanol, 3-methyl-1-butanol in isoalkanes with a large number of carbon atoms than the original with IRTE, implemented at a relatively high pressure in the inclination of the reagents to the development of adverse reactions of condensation, which lead to the formation of oxygen-containing products.

The proposed method involves the use of the IC of the following composition [iFof 0.95Zr0,03Mo0,02]as aluminium oxide-platinum catalysts used stamps AP-56, AP-64 (Overruled. "Heterogeneous catalysis", ICC called "Akademkniga", M, 2004, S. 548-5 49], and MgO additive, which improves the structure of the catalytic system by optimizing its specific surface area and increases the mechanical strength of the granules of the catalyst.

The catalytic composition was prepared by mechanical mixing IC with Pt/γ-Al2O3and magnesium oxide in the ratio IC: Pt/γ-Al2O3:magnesium oxide= 10:1:(0,8-1,2).

The capillary stream Parametrii shown that the addition of magnesium oxide leads to an increase in specific surface area.

The introduction of additives of magnesium oxide in the ratio of 10:1:(0,8-1,2) increases the mechanical strength of the granules of the catalyst. Notable grinding in the absence of MgO occurs in 15-20 hours of continuous operation of the catalyst. This supplements the catalytic system does not detect noticeable changes after 350-400 hours of continuous operation.

The following examples illustrate the re is the implementation of the proposed method.

Example 1

50%aqueous solution of ethanol is passed through 66 cm3catalyst consisting of a mixture of 55 cm3hydride phase intermetallic compounds [TiFeof 0.95Zr0,03Mo0,02]H2, 5.5 cm3PT/γ-Al2About3and 5.5 cm3MgO (volume and mass mixing ratio 10:1:1) at a temperature of 350°C, with a bulk velocity of 0.5 h-1under the pressure of argon of 50 ATM. The resulting product is top of the paraffin layer is separated from water, dried over l2, liquid product is filtered and distilled to a temperature of 250°C. Distilled organic substrate analyzed by gas chromatography-mass spectrometry and GC in linear programming, using a glass column (50 m × 0.2 mm) caused by the phase SE-30 and PID.

The results of the analysis showed that the conversion of ethanol is 87.3 per cent, 18.6 per cent of which are in the gaseous and 81,4% for liquid products. In the composition of the organic reaction products contained 24.0% of oxygen-containing products and 60% paraffin fraction C4-C16containing up to 42.2% of isoalkanes, and 26.2 per cent of these are dimethylselenide and 16,0% monomethylamine ISO.

Data on the catalyst are summarized in table.

Example 2

The conversion of ethanol is carried out in the presence of a catalytic mixture of TiFe0.95Zr0.03Ni0.02 +PT/γ-Al2About3+MgO at a mass ratio of 10:1:0.8 in conditions similar to example 1.

The results of the analysis showed that the conversion of ethanol is 85,3%, 17.8 per cent of which are in the gaseous and 82.2% for liquid products. In the composition of the organic reaction products contained 23,0% of oxygen-containing products and 59% paraffin fraction C4-C16containing to 40.1% of isoalkanes, and 25,0% of them in dimethylselenide, and 15.1% on monomethylamine ISO.

Data on the catalyst are summarized in table.

Example 3

The conversion of ethanol is carried out in the presence of a catalytic mixture of TiFe0.93Mn0.05Cr0.02+PT/γ-Al2O3+MgO at a ratio of 10:1:1.2 in conditions analogous to example 1.

The results of the analysis showed that the conversion of ethanol is 86.5%and 18.3%, of which are in the gaseous and 80.7% for liquid products. In the composition of the organic reaction products contained 25.0% of oxygen-containing products and 60.7% paraffin fraction C4-C16containing up to 43.1% of isoalkanes, and 27.1 per cent of these are dimethylselenide and 16,0% monomethylamine ISO.

Data on the catalyst are summarized in table.

Example 4

The conversion of ethanol is carried out in the presence of a catalytic mixture of TiFe0.95Zr0.03Mo0.02+Pt/γ-Al2O3 +MgO at a mass ratio of 10:1:2 under conditions similar to example 1.

The results of the analysis showed that the conversion of ethanol is 84.7 per cent, 16.9 per cent, of which are in the gaseous and 83.1% of liquid products. In the composition of the organic reaction products contains 24% of oxygen-containing products and 60% paraffin fraction C4-C16containing up to 41.2% isoalkanes, and 23.2 per cent of these are dimethylsiloxane, and 14.7 per cent on monomethylamine ISO.

Data on the catalyst are summarized in table. In continuous operation of the catalyst over 400 hours of its catalytic activity is reduced by 20-25%. Example 5

The conversion of ethanol is carried out in the presence of a catalytic mixture of TiFe0.95Zr0.03Mo0.02+PT/γ-Al2About3+MgO at a mass ratio of 10:1:0.5 V conditions similar to example 1.

The results of the analysis showed that the conversion of ethanol is 76,3%, 21.6 per cent of which are in the gaseous and 78.4% of the liquid products. In the composition of the organic reaction products contained 28,0% of oxygen-containing products and 52.6% paraffin fraction C4-C16containing up to 43.6% of isoalkanes, and 24,2% of them in dimethylselenide, and 19.4 per cent on monomethylamine ISO.

Data on the catalyst are summarized in table. In continuous operation of the catalyst within 200 is aces of its catalytic activity is reduced by 20-25%, and after 400 hours - 40%. Example 6

Carry out the conversion of 50% aqueous mixture of alcohols consisting of 30% ethanol, 5% 2-methyl-1-propanol and 15% of 3-methyl-1-butanol (mass ratio of 6:1:2) by passing through 66 cm3catalyst consisting of a mixture of 55 cm3hydride phase intermetallic compounds [TiFeof 0.95Zr0,03Mo0,02]H2, 5.5 cm Pt/γ-Al2O3and 5.5 cm MgO under conditions analogous to example 1.

The reaction products had the following composition: gaseous compounds -15%liquid and 40%, of which 27% is albanova fraction With4-C16, 13% are oxygen-containing compounds, the rest is water. Albanova fraction contains 83% of isoalkanes.

Example 7 (prototype)

a 50%aqueous solution of ethanol is passed through 66 cm3catalyst consisting of a mixture of 60 cm3hydride phase intermetallic compounds [iFof 0.95Zr0,03Mo0,02]H2and 6 cm3γ-Al2O3under conditions analogous to example 1. The results of the analysis showed that the conversion of ethanol is 70%, 5% of which are in the gaseous and 95% for liquid products. In the composition of the organic reaction products contains 40% diethyl ether and 60% paraffin fraction C8-C15containing up to 45% of isoalkanes, and 30% of them in dimerization, and 15% on monomethylethanolamine. After 20 hours there is a significant dispersion of the catalyst and its destruction.

The table presents the results on the study of resource (time of the catalyst without loss of activity) of all examples.

Table of resource intermetallic catalytic system

The operating time of the catalyst hour.Catalytic activity (alkanal), g/lcat.h
Example 1Example 2Example 3Example 4Example 5Example 6The placeholder
1120120120120120120120
5123126124125122121108
10125 12312412512512490
1512112012112112112181
2011812212211811712070
30121120120115115118
50120118116112112116
100118118118108108119
15011811611610398120
20012311411510093118
2501251161139885116
3001211131119575119
3501171121119372117
400116112110 9068117

Thus, from the comparable analysis follows that in the proposed method (catalyst, containing as oxide non-transition metal MgO) catalytic system while maintaining high catalytic activity increases to 400 hours, which is higher than the prototype more than 20 times.

The method of obtaining a mixture of isoalkanes C4-C16by contacting an aliphatic alcohol - ethanol, 2-methyl-1-propanol, 3-methyl-1-butanol in an inert gas environment at 300-420°C, a pressure of 30-80 MPa, flow rate 0,2-0,8 h-1with a catalytic composition comprising a hydride phase celestianpower intermetallic compounds modified with metals of IV-VII groups, aluminium oxide-platinum oxide catalyst and non-transition metal, characterized in that as the oxide non-transition metal is magnesium oxide in a mass ratio of 10:1:(0,8-1,2).



 

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17 cl, 7 ex, 2 tbl

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FIELD: petroleum processing and petrochemistry.

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EFFECT: reduced tar and coke formation and prolonged lifetime of catalyst.

4 cl, 2 tbl, 12 ex

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