Catalyst, a method of its preparation and a method of isomerization of olefins with use of this catalyst

FIELD: chemical and petrochemical industries; isomerization of olefins.

SUBSTANCE: the invention is dealt with of the field of deposition on carbon materials of catalysts of the basic nature being of interest for processes of isomerization of olefins. There is a description of a catalyst of isomerization of olefins containing metal sodium deposited on a composite porous carbon material, which represents a three-dimensional porous carbon die with the following structural characteristics: d002 =0.343-0.350 nm, the average size of the crystallite in a direction of "a"-La=l-14 nm, the average size of the crystallite in a direction of "c"-Lc=2-12 nm, real density of 1.8-2.1 g/cm3, with distribution of pores by sizes having a maximum in the range of 20-200 nm and an additional maximum in the range of 1-20 nm. Also there is a description of a method of preparation of the catalyst providing for deposition of metal sodium on the composite porous carbon material and a method of isomerization of olefins with use of this catalyst. The technical result is a possibility to conduct the process of isomerization at low temperatures, increased catalytic activity and selectivity, decreased output of by-products.

EFFECT: the invention ensures a possibility to conduct the process of isomerization at low temperatures, increased catalytic activity and selectivity, decreased output of by-products.

6 cl, 10 ex, 2 tbl

 

The present invention relates to the field applied on carbon materials catalysts basic nature of interest processes for the isomerization of olefinic hydrocarbons.

Known heterogeneous catalysts for the isomerization of olefinic hydrocarbons and methods for their preparation are described in [Zhorov, Y.M., Panchenkov G.M., Volokhov G.S.// Isomerization of olefins. M., 1977]. These catalysts on their ability to accept a proton (or give away electrons) and to give a proton (or give away electrons) is usually divided, respectively, in acid and alkaline. To acid catalysts include “hard” acids (acid media), oxides and mixed metal oxides, transition metals deposited on various porous materials, as well as silicates and zeolites.

The main catalysts of nature are “solid” base (alkali and alkaline earth metals, their hydrides, amides, oxides and hydroxides deposited on various porous materials, oxides, salts and amides of metals, and alkaline forms of the zeolites. Alkaline heterogeneous catalysts allow for the isomerization of a double bond at low temperatures (24-175° (C) [Zhorov, Y.M., Panchenkov G.M., Volokhov G.S.// Isomerization of olefins. M., 1977]. The main catalysts of nature are used for the isomerization of butene-1 and other acyclic is such olefins [.Hattori// RDAs. Catal., vol. 222 (2001), R; Pat.GB 1355688, C 07 C 5/30, 23.12.75], and olefins, more complex structures, including for terpene olefins containing three - and four-membered cycles [G.Suzukamo, .Fukao, .Minobe// Chem. Lett., (1987), R; .Gorzawski, W.F.Hoeldrich// J. of Mol. Catal., Vol.144 (1999), p.181].

Known catalyst consisting of an alkali metal, pending in the amount of 2-20 wt.% aluminum oxide Al2About3promoted metal hydroxide in the amount of 5-15 wt.%. This catalyst is used in an industrial process for the isomerization of 5-vinylbital[2,2,1]Heptene-2 5-ethylidenebicyclo[2,2,1]heptan-2 (isomer on the position of the double bond), which allows the process at a temperature of 20°With conversion of the substrate 99.7%, and the selectivity of 99.9% [Pat.GB 1355688]. The same catalyst used in the isomerization β-pinene in α-pinene [.Gorzawski, W.F.Hoeldrich// J. of Mol. Catal., Vol.144 (1999), p.181]. The reaction is carried out in the liquid phase at a temperature of 25-150°With, in optimal conditions, the conversion of the substrate reaches 99% for 30 minutes the closest to the technical nature of the claimed is a catalyst containing metallic sodium in amounts of 5-30 wt.% coconut angle [Pat. GB 1008964, C 07 C 5/25, 03.11.65]. Used carrier has the following structural characteristics: specific surface 950-1200 m2/g, with a predominant pore size of 1-2 nm. X-ray characteristics meeples ostmoe distance in the direction 002 - d002=0,356 nm, the average size of crystallite in the direction of “and” - La<1 nm, the average size of crystallite in the direction “C” - Lc<1 nm, the true density of 1.7 g/cm3. The catalyst is prepared as follows: coconut activated carbon is dried in a stream of nitrogen at 250 to 300°add sodium metal and the mixture is heated at a temperature 125-190°to complete adsorption of sodium activated carbon. This catalyst is used for the isomerization of 2-methylpentan-1 at 2-methylpentene-2 (one of the stages of the synthesis of isoprene from propylene). The reaction is carried out in the gas or liquid phase in the presence of inert gas at a temperature of 140 to 175°S, 0.03-3.5 MPa and space velocity of the liquid raw material is 0.1-10 h-1. After the reaction, the catalyst is activated with hydrogen at 200°C for 6 hours maximum yield of 2-methylpentene-2 is observed in the gas phase at 175°and 0.035 MPa. The selectivity of 79%; the yield of by-products of isomerization (4 methylpentene-1 and 4-methylpentene-2) 19%.

The disadvantages of the known catalysts are low catalytic activity, a significant output of by-products and high temperature process of isomerization.

The invention solves the problem of increasing the activity and selectivity of the catalyst and optimization of the isomerization process of using it.

The problem is solved of train the catalyst for isomerization of olefins, containing sodium metal on a carbon carrier, as the carrier it contains composite porous carbon material constituting the three-dimensional porous carbon matrix with the following structural characteristics: interplanar distance in the direction 002 - d002=0,343-0,350 nm, the average size of crystallite in the direction of “and” - La=1-14 nm, the average size of crystallite in the direction “C” - Lc=2-12 nm, a true density of 1.8-2.1 g/cm3with a distribution of pore sizes , with a maximum in the area of 20-200 nm and an additional maximum in the region of 1-20 nm. The ratio of the volume of the applied metal Na to the pore volume of the composite porous carbon material is 0.01 to 0.5.

The task is also solved by a method of preparation of the catalyst for isomerization of olefins, comprising the application of metallic sodium on a carbon carrier, as carbon media use composite porous carbon material. Composite porous carbon material is a three-dimensional porous carbon matrix with the following structural characteristics: d002=0,343-0,350 nm, the average size of crystallite in the direction of “and” - La=1-14 nm, the average size of crystallite in the direction “C” - Lc=2-12 nm, a true density of 1.8-2.1 g/cm3with the distribution of the pore is the sizes, having a maximum in the area of 20-200 nm and an additional maximum in the region of 1-20 nm [U.S. Pat. USA 4978649, From 01 To 31/10, 18.12.1990].

Composite porous carbon material pre-calcined under vacuum at a temperature of 300-1000°C.

The ratio of the volume of the applied metal Na to the pore volume of the composite porous carbon carrier is 0.01 to 0.5.

The task is also solved by a method for the isomerization of olefins in which the catalyst using the catalyst described above.

The invention is illustrated by the following examples.

Example 1. In a vial made of quartz glass download granular carbon media, representing a three-dimensional porous matrix formed by bent layers of carbon of a thickness of 10-1000 nm, the radius of curvature of 10-1000 nm, with the following structural characteristics: d002=0,349 nm, the average size of crystallite in the direction of “and” - La=3,9 nm, the average size of crystallite in the direction “C” ” - Lc=3,0 nm, the true density of 2.05 g/cm3and distribution of pores having a maximum in the region of 30 nm and an additional maximum in the region of 2 nm. Carbon media, annealed in vacuum (10-2-10-3Torr) at a temperature of 900-1200°C for 5 o'clock To 8 g of the obtained carbon media add 2 g of metallic sodium and paramasivan is heated in vacuum for three hours at a temperature of 210-220° C. Obtain 10 g of a catalyst containing 20 wt.% metallic sodium in the carbon carrier with the ratio of the amount of metallic sodium”/“pore volume” media = 0,43.

The catalyst used in the reaction of isomerization of 1-hexene. In the glass cooled tubular reactor placed 2 g of catalyst. Establish operating temperature (25-150° (C) in the reactor, the gas flow 20 ml/min and dose of hexene-1 with a speed of 0.07 mmol/min At the outlet of the reactor products collected in a trap and analyzed by gas.

The composition of the reaction products:

To the reaction temperature of 25°S: 1.4% of the hexene-1, 82.1% of the hexene-2 (TRANS/CIS=3,2), 16.4% hexene-3 (TRANS/CIS=6,9).

To the reaction temperature of 70°S: 2% hexene-1, 79.6% of the hexene-2 (TRANS/CIS=2,7), and 18.3% hexene-3 (TRANS/CIS=7,7).

To the reaction temperature 100°S: 4.0% hexene-1, 77,1% hexene-2 (TRANS/CIS=2,6), 18,9% hexene-3 (TRANS/CIS=7,4).

To the reaction temperature of 150°W: 4.8% of hexene-1, 72,3% hexene-2 (TRANS/CIS=2.2), 22.9% of hexene-3 (TRANS/CIS=7.2).

Structural characteristics of the catalysts are summarized in table 1, the catalytic properties in table 2.

Example 2. Similar to example 1, except that 9 g of carbon media was added 1 g of metallic sodium. So, get 10 g of the catalyst containing 10 wt.% metallic sodium in the carbon carrier with the ratio of the volume of use is th sodium”/“pore volume” media = 0,21.

The composition of the products for the reaction temperature of 25°S: 1.2% of hexene-1, 82% hexene-2 (TRANS/CIS=2,9), 16.8% of hexene-3 (TRANS/CIS=7,0).

Example 3. Similar to example 1, with the difference that 9,8 g carbon media add 0.2 g of metallic sodium. So, get 10 g of the catalyst containing 2 wt.% metallic sodium in the carbon carrier with the ratio of the amount of metallic sodium”/“pore volume” media = 0,043.

The composition of the products for the reaction temperature of 25°W: 5.5% of hexene-1, 76,9% hexene-2 (TRANS/CIS=2,9), 18.1% of hexene-3 (TRANS/CIS=6,9).

Example 4. Similar to example 1, with the difference that 9,954 g carbon media type 0,046 g of metallic sodium. So, get 10 g of catalyst containing about 0.5 wt.% metallic sodium in the carbon carrier with the ratio of the amount of metallic sodium”/“pore volume” media = 0,01.

The composition of the products for the reaction temperature of 25°W: 7.6% of hexene-1, 76,3% hexene-2 (TRANS/CIS=2,8), 16,1% hexene-3 (TRANS/CIS=6,7).

Example 5. Similar to example 1, with the difference that use granular carbon media, representing a porous matrix formed by bent layers of carbon of a thickness of 10-1000 nm, the radius of curvature of 10-1000 nm, with the following structural characteristics: d002=0,343 nm, the average size of crystallite in the direction of “and” - La=14,0 nm, average the size of the crystallite in the direction “C” ” - Lc=12,0 nm, the true density of 2.10 g/cm3and distribution of pores having a maximum in the region of 200 nm and an additional maximum in the region of 20 nm. To 9 g of the obtained carbon media was added 1 g of metallic sodium and heated with stirring under vacuum for three hours at a temperature of 210-220°C. Obtain 10 g of a catalyst containing 10 wt.% metallic sodium in the carbon carrier with the ratio of the amount of metallic sodium”/“pore volume” media = 0,21.

The composition of the reaction products to a temperature of 25°S: 1.2% of hexene-1, 82.1% of the hexene-2 (TRANS/CIS=2,9), 16.7% of the hexene-3 (TRANS/CIS=6,3).

Example 6. Similar to example 1, with the difference that use granular carbon media, representing a porous matrix formed by bent layers of carbon of a thickness of 10-1000 nm, the radius of curvature of 10-1000 nm, with the following structural characteristics: d002=0,350 nm, the average size of crystallite in the direction of “and” - La=1.0 nm, the average size of crystallite in the direction “C” ” - Lc=2.0 nm, the true density of 1.80 g/cm3and distribution of pores having a maximum in the region of 20 nm and an additional maximum in the region of 1 nm. To to 7.67 g of the obtained carbon media type of 2.33 g of metallic sodium and heated with stirring under vacuum for three hours, during which the temperature of 210-220° C. Thus, obtain 10 g of a catalyst containing ~23 wt.% metallic sodium in the carbon carrier with the ratio of the amount of metallic sodium”/“pore volume” media = 0,5.

The composition of the reaction products to a temperature of 25°W: 3.8% hexene-1, 78,8% hexene-2 (TRANS/CIS=3,2), 19.1% of hexene-3 (TRANS/CIS=6,8).

Example 7. Similar to example 1, with the difference that use carbon media, representing a porous matrix formed by bent layers of carbon in the form of fibers having a thickness of 10-150 nm, the ratio of length to thickness 160-2500 and twisted randomly into granules, with the following characteristics: d002=0,345 nm, the average size of crystallite in the direction of “and” - La=4,5 nm, the average size of crystallite in the direction “C”” - Lc=6,8 nm, the true density of 1.9 g/cm3and distribution of pores with a maximum in the region of 200 nm and an additional maximum of 10 nm.

The composition of the reaction products to a temperature of 25°S: 1.3% hexene-1, 82.1% of the hexene-2 (TRANS/CIS=2,9), 16.6% of hexene-3 (TRANS/CIS=6,1).

Example 8. Similar to example 1, with the difference that use carbon media, representing a porous matrix formed by bent layers of carbon in the form of fibers having a thickness of 10-150 nm, the ratio of length to thickness 160-2500 and twisted randomly into granules, with the following ha what acteristically: d 002=0,343 nm, the average size of crystallite in the direction of “and” - La=5,5 nm, the average size of crystallite in the direction “C” - Lc=8,0 nm, the true density of 1.95 g/cm3and distribution of pores with a maximum in the region of 100 nm and an additional maximum of 4 nm.

The composition of the reaction products to a temperature of 25°C: 1.5% of hexene-1, 81,3% hexene-2 (TRANS/CIS=2,8), and 17.2% hexene-3 (TRANS/CIS=6,2).

Example 9. Similar to example 1, with the difference that instead of hexene-1 dose of butene-1 with a speed of 20 ml/min (0.8 mmol/min).

The composition of the reaction products:

To the reaction temperature of 25°W: 7.0% butene-1, 93% butene-2 (with a ratio of TRANS/CIS=2,3).

To the reaction temperature of 70°W: 7.2% of butene-1, 92,8% butene-2 (with a ratio of TRANS/CIS=2,1).

To the reaction temperature 100°W: 7.7% of butene-1, 92.3% of butene-2 (with a ratio of TRANS/CIS=2,1).

Example 10. Similar to example 1, with the difference that instead of 1-hexene metered 3-Karen, with a speed of 0.14 mmol/min, and the temperature of the reactor 130-200°C. At the outlet of the reactor products collected in a trap and analyzed by gas.

The composition of the reaction products:

For temperatures up to 130°S: 57,1% 3-Karen, 42,9% 2-Karen.

For temperature 150°S: 56,6% 3-Karen, 43,4% 2-Karen and 1% of the products of the disclosure a three-membered cycle Karen (parameterizedproperty, solimano).

For temperature 180°S: 33.6% of 3-Karen, 26.5 per cent Karen and 39.9% of the products of the disclosure a three-membered cycle Karen (parameterizedproperty, solimano).

For temperature 200°S: 1,2% 3-Karen, 0.9% of 2-Karen and 97.9% of the products of the disclosure a three-membered cycle Karen (parameterizedproperty, solimano).

As seen from the above examples and tables, the proposed catalyst has high catalytic activity and selectivity when used in isomerization processes decreases the yield of the by-products of the isomerization process may be carried out at low temperatures.

Table 1

Characterization of catalysts for the isomerization of olefins
Example

No.
The parameters of the carbon mediaThe maxima of the distribution of pore size, nmVNa/Vthen
d002nmLanmLcnmdEast, g/cm3
10,349a 3.93,02,0530 20,43
20,349a 3.93,02,0530 20,21
30,349a 3.93,02,0530 20,043
40,3493,9 3,02,0530 20,01
50,34314,0to 12.02,10200 and 200,21
60,3501,02,01,8020 and 10,50
70,3454,56,81,9200 and 100,12
80,3435,58,01,95100 40,1
The placeholder0,356<1<11,71-20,15

1. The catalyst for isomerization of olefins containing sodium metal on a carbon carrier, characterized in that as the carbon media it contains composite porous carbon material constituting the three-dimensional porous carbon matrix with the following structural characteristics: d002=0,343-0,350 nm, the average size of crystallite in the direction “a”-La=1-14 nm, the average size of crystallite in the direction “c”-Lc=2-12 nm, a true density of 1.8-2.1 g/cm3with a distribution of pore sizes , with a maximum in the area of 20-200 nm, and further the first maximum in the region of 1-20 nm.

2. The catalyst according to claim 1, characterized in that the ratio of the volume of the applied metallic sodium to the pore volume of the composite porous carbon material is 0.01÷0.5 in.

3. The method of preparation of the catalyst for isomerization of olefins, comprising the application of metallic sodium on a carbon carrier, characterized in that as the carbon media use composite porous carbon material constituting the three-dimensional porous carbon matrix with the following structural characteristics: d002=0,343-0,350 nm, the average size of crystallite in the direction “a”-La=1-14 nm, the average size of crystallite in the direction “c”-Lc=2-12 nm, a true density of 1.8-2.1 g/cm3with a distribution of pore sizes , with a maximum in the area of 20-200 nm and an additional maximum in the region of 1-20 nm.

4. The method according to claim 3, characterized in that the composite porous carbon material pre-calcined under vacuum at a temperature of 300÷1000°C.

5. The method according to claim 3, characterized in that the ratio of the volume of the applied metallic sodium to the pore volume of the composite porous carbon material is 0.01÷0.5 in.

6. The way isomerization of olefins, characterized in that the use of the catalyst according to any one of claims 1 to 5.



 

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FIELD: powder metallurgy; method of impregnation by a metal(of VIII group) of a molecular sieve extrudate with cementing material with the help of ion exchange with an aqueous solution of metal salt of VIII group.

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