Method of hydrogenating olefins and oxygen-containing compounds in synthetic liquid hydrocarbons obtained via fischer-tropsch method and catalyst for realising said method

FIELD: chemistry.

SUBSTANCE: invention relates to a catalyst for realising a method of hydrogenating olefins and oxygen-containing compounds in synthetic liquid hydrocarbons obtained via a Fischer-Tropsch method, containing a porous support made from γ-aluminium oxide on which a catalytically active palladium component is deposited, characterised by that pores in the support have effective radius of 4.0-10.0 nm, wherein content of foreign-metal impurities in the support is not more than 1500 ppm, and content of palladium in the catalyst is equal to 0.2-2.5 wt %. The invention also relates to a hydrogenation method using said catalyst.

EFFECT: invention enables to obtain saturated hydrocarbons from liquid Fischer-Tropsch synthesis products, which are a complex mixture of paraffin hydrocarbons with 5-32 carbon atoms, with ratio of normal paraffin hydrocarbons to isoparaffin hydrocarbons ranging from 1:1 to 7:1, containing up to 50% olefins and up to 5% oxygen-containing compounds.

2 cl, 1 tbl, 7 ex

 

The invention relates to gas and gas processing, namely the technology of synthetic saturated hydrocarbons by hydrogenation of the fractions isolated from the products of the Fischer-Tropsch synthesis.

Light fractions isolated from synthetic liquid hydrocarbons (SIU)obtained by Fisher-Tropsch, along with saturated paraffin hydrocarbons normal, isotrate contain unsaturated hydrocarbons. In order to use fractions corresponding to gasoline, as a component or feedstock for motor fuels in processes of isomerization, aromatization, etc. need to tuck the hydrogenation of unsaturated and oxygenated compounds.

A method of obtaining liquid hydrocarbons in the process of converting synthesis gas according to the method of Fischer-Tropsch. The process of catalytic conversion of the synthesis gas is carried out at a temperature of 220-270°C., a pressure of 0.1 to 5.0 MPa, space velocity of 50-5000 h-1on a cobalt catalyst supported on a carrier containing alumina and zeolite (Patent GB 2 211 20,1988).

The disadvantage of this method is the low yield of the target product, and this method provides only an intermediate product, and not the end in the form of commercial fuel.

A method of obtaining hydrocarbon fuel from the of Reducto process for the synthesis of hydrocarbons from carbon monoxide and hydrogen by contacting the products with hydrogen in the presence of catalyst hydroconversion. Stage hydroconversion carried out in two stages: the first stage carry out the contacting of the hydrocarbon product with hydrogen in the presence of a catalyst under such conditions, under which hydrogenation occurs and, in fact, no isomerization or hydrocracking product, and the second stage carry out the contacting at least part of the hydrocarbon product of the first step with hydrogen in the presence of catalyst hydroconversion in such conditions, in which the hydrocracking and isomerization of the hydrocarbon product with obtaining a hydrocarbon fuel containing mainly paraffin hydrocarbons (Patent RU 2101324, 1998).

The shortcoming of the above method is the lack of pre-separation of the mixture of synthetic hydrocarbons into fractions, because the distribution of olefins in the products of the Fischer-Tropsch synthesis unevenly and decreases with increasing number of carbon atoms in hydrocarbons.

The closest to a method of hydrogenation of synthetic liquid olefin is a method for jet and diesel fuels products from the Fischer-Tropsch synthesis by pre-separation into fractions (wikipaedia to 260°C and wikipaedia above 260°C) and separate hydrogenation and isomerization of light fraction and isomerization heavy fraction. On the adiya's hydrogenation was used sulfatirovanne alumonickelsilicate catalysts and ecumenically catalysts (Patent US 5378348, 03.01.1995).

The disadvantages of the method is inefficient use of the pre-stage hydrogenation to obtain jet and diesel fuel by hydrogenation and isomerization faction, wikipeida below 260°C. Such catalytic systems are ineffective in the hydrogenation of a wide factions.

The closest technical solution catalyst for the hydrogenation products of the Fischer-Tropsch synthesis is a catalyst containing Nickel, platinum or palladium supported on diatomite, magicality or activated carbon (Patent EP 1927643, 2008).

The shortcoming of the above catalysts is their low efficiency at space velocities of more than 1 hour-1in the process of hydrogenation products of the Fischer-Tropsch synthesis.

The aim of the invention is to obtain saturated hydrocarbons from the liquid products of the Fischer-Tropsch synthesis, a complex mixture of paraffin hydrocarbons with the number of carbon atoms from 5 to 32 with a ratio of normal paraffin hydrocarbons to isoparaffin is from 1:1 to 7:1, containing up to 50% of olefins and up to 5% of oxygen-containing compounds.

The technical problem solved by the present invention is the use of fractions corresponding to gasoline, isolated from a mixture of synthetic liquid hydrocarbons obtained by Fisher-the Ropsha, previously subjected to hydrogenation, as a component or feedstock for motor fuels in the processes of isomerization, and aromatization.

This technical task and the specified objective is achieved by separation of the liquid products obtained during Fischer-Tropsch synthesis, catalytic hydrogenation of selected light fractions: Nicholas -85°C and 85-140°C or Nicholas -140°C (where NK is the beginning of the boil under normal conditions) on a stationary catalyst bed containing 0.2-2.5 wt.% palladium supported on a carrier, representing a γ-alumina, the content of impurities contaminating metals which does not exceed 1500 ppm, with a predominant effective radius of the pores is from 4.0 to 10.0 nm, at a temperature of 100-250°C., hydrogen pressure of 1.5 to 5.0 MPa, the space velocity of the raw material of 0.2-10.0 h-1and the ratio of hydrogen: feedstock 200-2000:1 nl/L.

These distinctive features significant.

In order to use fractions corresponding to gasoline, as a component or feedstock for motor fuels in processes of isomerization, aromatization, etc. need to tuck the hydrogenation of unsaturated and oxygenated compounds.

The highlight for the rectification of light fractions: Nicholas -85°C and 85-140°C or Nicholas -140°C containing unsaturated hydrocarbons, allows them separately the first hydrogenation on the specific catalyst, ensure the effectiveness of the process for these fractions. Increasing limits boiling fractions of olefins and oxygen-containing compounds decreases as their distribution in the products of the Fischer-Tropsch synthesis unevenly and decreases with increasing number of carbon atoms in hydrocarbons. The declared modes hydrogenation in the presence of the claimed catalyst provides the largest weight obtain saturated synthetic hydrocarbons containing olefins.

The method is implemented as follows.

Obtained by Fischer-Tropsch synthesis products, having a form of synthetic liquid hydrocarbons, a complex mixture of paraffin hydrocarbons with the number of carbon atoms from 5 to 32, with respect to the normal paraffin hydrocarbons to isoparaffin-1-7:1, containing up to 50% of olefins and up to 5% of oxygen-containing compounds into fractions: Nicholas -85°C and 85-140°C or Nicholas -140°C. the Selected fraction containing olefins and oxygenated compounds, is subjected to catalytic hydrogenation at a temperature of 100-250°C., hydrogen pressure of 1.5 to 5.0 MPa, the space velocity of the raw material 0,2-10,0 h-1and the ratio of hydrogen:feedstock 200-2000:1 nl/L. For hydrogenation using a catalyst containing 0.2-2.5 wt.% palladium supported on a carrier, with representing the ow of γ-alumina, the content of metal impurities which does not exceed 1500 ppm and with a predominant effective radius of the pores is from 4.0 to 10.0 nm.

Examples 1-4 illustrate a method of hydrogenation of olefins and oxygen-containing compounds, and examples 5-7 demonstrate the technology of preparation of the catalyst for implementing the method of hydrogenation of olefins and oxygen-containing compounds in the composition of synthetic liquid hydrocarbons obtained by Fisher-Tropsch process.

Table 1 shows the results of the hydrogenation according to the above mentioned examples 1-4 implement the method.

Example 1

A mixture of synthetic liquid hydrocarbons is subjected to rectification with the release fraction Nicholas -85°C containing 50% olefin, and 5% oxygenated compounds. The resulting fraction is subjected to hydrogenation in the presence of hydrogen at a temperature of 250°C and a pressure of 5.0 MPa, the space velocity of the raw material of 0.2 h-1. The ratio of hydrogen:raw support is 2000:1 nl/L. Hydrogenation is carried out in the presence of a catalyst containing as the catalytically active palladium component in an amount of 2.5 wt.%. As a catalyst carrier use of porous γ-alumina with an average pore size of 4.0 nm, the impurity content of extraneous metal which does not exceed 1500 ppm.

Example 2

The mixture of synthetic liquid coal is of hydrocarbons is subjected to rectification with the release fraction 85-140°C, containing 30% olefins and 3% of oxygen-containing compounds. The resulting fraction is subjected to hydrogenation in the presence of hydrogen at a temperature of 200°C and a pressure of 3.0 MPa, the space velocity of the raw material 5 h-1. The ratio of hydrogen:raw support equal to 500:1 nl/L. Hydrogenation is carried out in the presence of a catalyst containing as the catalytically active palladium component in an amount of 1 wt.%. As a catalyst carrier use of porous γ-alumina with an average pore size of 10.0 nm, the impurity content of extraneous metal which does not exceed 1500 ppm.

Example 3

A mixture of synthetic liquid hydrocarbons is subjected to rectification with the release fraction Nicholas -140°C, containing 40% olefins and 4% of oxygen-containing compounds. The resulting fraction is subjected to hydrogenation in the presence of hydrogen at a temperature of 220°C and a pressure of 4 MPa, the space velocity of the raw material of 7.5 h-1. The ratio of hydrogen: raw support 600:1 nl/L. Hydrogenation is carried out in the presence of a catalyst containing as the catalytically active palladium component in an amount of 1.1 wt.%. As a catalyst carrier use of porous γ-alumina with an average pore size of 6.0 nm, the impurity content of extraneous metal which does not exceed 1500 ppm.

Example 4

A mixture of various is their liquid hydrocarbons is subjected to rectification with the release fraction Nicholas -140°C., containing 15% olefins and 1.5% of oxygen-containing compounds. The resulting fraction is subjected to hydrogenation in the presence of hydrogen at a temperature of 100°C and a pressure of 1.5 MPa, the space velocity of the raw material 10 h-1. The ratio of hydrogen:raw support equal to 200:1 nl/L. Hydrogenation is carried out in the presence of a catalyst containing as the catalytically active palladium component in an amount of 0.2 wt.%. As a catalyst carrier use of porous γ-alumina with an average pore size of 6.0 nm, the impurity content of extraneous metal which does not exceed 1500 ppm.

Example 5

128,9 g of powder of aluminum hydroxide, the impurity content of extraneous metal which does not exceed 1500 ppm, first moistened with distilled water. Wet paste of aluminum hydroxide peptizer aqueous solution of nitric acid solution, taken in an amount such that the pH patinirovannoy mass corresponded to 4.5. The resulting mass is thoroughly mixed, evaporated to a moisture content of 70 wt.% and molded 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 about Alki 50°C per hour.

and 99.8 g of calcined carrier vacuum for 30 min, and then placed in a 150 ml joint impregnating solution containing 0.09 g of palladium chloride; 0,22 ml 98.5% of concentrated acetic acid and 0.23 ml 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, 2 h at 140°Poluchenii the catalyst has a pore of 6.0 nm. The impurity content of extraneous metal in the catalyst does not exceed 1500 ppm.

The composition of the obtained catalyst, wt.%:

Palladium(PD)0,2
Aluminum oxide (γ-Al2O3)99,8

Example 6

to 127.9 g of powder of aluminum hydroxide, the impurity content of extraneous metal which does not exceed 1500 ppm, first moistened with distilled water. Wet paste of aluminum hydroxide peptizer aqueous solution of nitric acid solution, taken in an amount such that the pH patinirovannoy mass corresponded to 5. The resulting mass is thoroughly mixed, upriv the Ute to a moisture content of 80 wt.% and molded into cylindrical pellets by extrusion.

Granules media dried, dried and calcined as in example 5.

a 99.0 g of calcined carrier vacuum for 30 min, and then placed in a 150 ml joint impregnating solution containing 1,679 g of palladium chloride; 1,15 ml 98.5% of concentrated acetic acid and 1.18 ml of 37% concentrated hydrochloric acid.

The impregnation of the support and drying of the catalyst is carried out analogously to example 5. The resulting catalyst has a pore of 10.0 nm. The impurity content of extraneous metal in the catalyst does not exceed 1500 ppm.

The composition of the obtained catalyst, wt.%:

Palladium(Pd)1,0;
Aluminum oxide (γ-Al2O3)99,0.

Example 7

125,9 g of powder of aluminum hydroxide, the impurity content of extraneous metal which does not exceed 1500 ppm, first moistened with distilled water. Wet paste of aluminum hydroxide peptizer aqueous solution of nitric acid solution, taken in an amount such that the pH patinirovannoy mass corresponded to 4. The resulting mass is thoroughly mixed, evaporated to a moisture content of 60 wt.% and molded into cylindrical pellets by extrusion.

Granules media dried, dried and calcined analogues is but example 5.

97.5 g of calcined carrier vacuum for 30 min, and then placed in a 150 ml joint impregnating solution containing 4,198 g of palladium chloride; 2,87 ml (98.5 per cent) of concentrated acetic acid and 2.95 ml (37%) of concentrated hydrochloric acid.

The impregnation of the support and drying of the catalyst is carried out analogously to example 5. The resulting catalyst has a pore 4.0 nm. The impurity content of extraneous metal in the catalyst does not exceed 1500 ppm.

The composition of the obtained catalyst, wt.%:

Palladium(PD)2,5
Aluminum oxide (γ-Al2O3)97,5

Physico-chemical properties of synthetic fractions subjected to hydrogenation according to examples 1-4 shown in the table.

no
Name examplesOlefins, wt.%The content of oxygen-containing compounds, wt.%Exit
gaseous products, wt.%
Example 1nono0,3
Example 2nono
Example 3nono0,2
Example 4no0,1no

The results in the table confirm the efficiency of the method and the proposed catalyst for production of synthetic liquid hydrocarbon products of the Fischer-Tropsch synthesis, not containing olefins and oxygen-containing compounds.

1. The method of hydrogenation of olefins and oxygen-containing compounds in the composition of synthetic liquid hydrocarbons obtained by Fisher-Tropsch process, including the selection of the synthesized liquid products of light fractions containing olefins and oxygen-containing compounds and their catalytic hydrogenation, wherein the light fraction NK - 85°C and 85-140°C or Nicholas -140°C separated from a mixture of synthetic liquid hydrocarbons by distillation and hydrogenation carried out at a stationary catalyst bed according to claim 2 at a temperature of 100-250°C., hydrogen pressure of 1.5 to 5.0 MPa, the space velocity of the raw material 0,2-10,0 h-1and the ratio of hydrogen: feedstock - 200-2000: 1 nl/L.

2. Catalysis is the PR for implementing the method of hydrogenation of olefins and oxygen-containing compounds in the composition of the synthetic liquid hydrocarbons, obtained by Fisher-Tropsch containing porous carrier of γ-alumina coated with a catalytically active component is palladium, characterized in that the pores of the media have an effective range from 4.0 to 10.0 nm, and the impurity content of extraneous metal in the media does not exceed 1500 million-1and the palladium content in the catalyst is 0.2 to 2.5 wt.%.



 

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