Rhenium oxide catalyst for metathesis of olefinic hydrocarbons, method of preparation thereof, and a propylene synthesis process involving use thereof

FIELD: petrochemical processes and catalysts.

SUBSTANCE: invention provides rhenium oxide catalyst on anion-containing gamma-alumina-based support: 0.1-10.0% Re2O3 and 0.2-4.0% fluorine based on the weight of alumina. Catalyst is prepared by impregnating alumina, including 0.2-4.0 wt % fluorine, with rhenium compound solution, drying resulting mass, and subjecting it to heat treatment in oxidative and/or inert medium at 600-900°C. Propylene synthesis process including metathesis of C2-C4-olefinic hydrocarbon blend or ethylene alone is also described.

EFFECT: increased catalytic activity and simplified technology.

7 cl, 2 tbl, 8 ex

 

The technical field to which the invention relates.

The invention relates to catalysts for metathesis of olefinic hydrocarbons and relates to the rhenium oxide catalyst on bionaturae media on the basis of gamma-aluminium oxide, method of producing rhenium oxide catalyst and method for the synthesis of propylene by metathesis of olefinic hydrocarbons using a specified catalyst.

The level of technology

It is known that the rhenium oxide catalysts based on aluminum oxide have low activity in the reaction of metathesis of olefinic hydrocarbons, if the concentration of rhenium in them does not exceed 1 wt.% [.Amigues, Y.Chauvin and D.Commereuc, Stepd, ..Lai, Y.H.Liu; Metathesis of ethylene-butene mixtures to propylene with rhenium on alumina catalysts (Metathesis of ethylene-butenova mixtures to obtain propylene using rhenium catalysts on alumina). Journal of Molecular Catalysis, t (1991), cc.39-50]. Given the high cost of rhenium, the active catalyst with a low content of rhenium can significantly reduce the cost of preparation of the catalyst.

A method of obtaining a rhenium oxide catalyst for the metathesis of olefins, comprising impregnation with a solution of compounds of rhenium gamma-aluminum oxide, pretreated with an acid solution, inorganic (e.g., hydrochloric acid) or organic (e.g., acetic acid), sleduushuu drying the resulting paste, the calcination in an oxidizing atmosphere at 300-900°and a final treatment in an inert gas. The content of the oxide of rhenium in the catalyst is 0.1-40 wt.% (GB 1106015, 1968). The disadvantages of this method is the need for pre-treatment of the alumina with solutions of acids, which complicates the preparation method of the catalyst, as well as a high content of oxide of rhenium, which leads to high cost of the catalyst.

Closest to the proposed invention is the rhenium oxide catalyst for metathesis of olefinic hydrocarbons prepared by impregnation of alumina containing anionic additive, a solution of the compound of rhenium, drying the mass, and subsequent heat treatment in air and inert gas at 580°C. For the introduction of aluminum oxide anionic additives used mineral acids (e.g., H2SO4or their salts, such as phosphates (for example, (NH4)2HPO4), fluoride (NH4F), vanadates. When the content of aluminum oxide of more than 0.1 wt.% chemically related anions their excess is removed by washing with water or an alkaline solution (GB 1216587, 1970). The disadvantage of this catalyst is its low activity. The disadvantage of this method of preparation of the catalyst is the need for pre-treatment of the oxide is of luminia salt solutions and rinsing it with water or alkaline solution, what complicates the process.

The known method for the synthesis of propylene by metathesis reaction of ethylene and butenes-2 using rhenium oxide catalyst, in which the concentration of rhenium is 0.01-20 wt.% rhenium, and the carrier is γ-alumina or a mixture containing at least 20 wt.% aluminum oxide and other oxides (US 4795734, 1989). The disadvantage of this method of synthesis of propylene is that this way you cannot get only propylene from ethylene.

Disclosure of inventions

The task to be solved by the invention is the development of high activity rhenium oxide catalyst for metathesis of olefinic hydrocarbons with low cost. The result is achieved that for the preparation of the catalyst with a lower content of rhenium is used anion-containing medium on the basis of gamma-alumina, comprising 0.2 to 4.0 wt.% fluorine as an anion.

In accordance with this object of the proposed invention is the rhenium oxide catalyst for metathesis of olefinic hydrocarbon anion-containing media with a basis of gamma-alumina, which includes fluoride as an anion, with the following content of components in the calculation of the gamma-aluminum oxide, wt.%: Re2O7- 0,1-10,0; fluorine - 0,2-4,0. The preferred content of the oxide of rhenium in ka is alistare is 0.5 to 8.0 wt.% in the calculation of the gamma-alumina. The preferred fluorine content is 0.2-2.2 wt.% in the calculation of the gamma-alumina.

Another object of the invention is a method for production of rhenium oxide catalyst for metathesis of olefinic hydrocarbons, including impregnation bionaturae media with a basis of aluminium oxide with a solution of the compound of rhenium, drying the resulting mass and subsequent heat treatment in an oxidizing and/or inert medium, in which as bionaturae media use gamma-alumina, comprising 0.2 to 4.0 wt.% fluorine calculated on gamma-alumina, and heat treatment is carried out at a temperature of 600-900°C.

As starting compounds of rhenium may be used any compound which is in the process of heat treatment decomposes with the formation of oxide of rhenium Re207, for example a compound selected from the group comprising an oxide of rhenium (VII), ammonium perrhenate, rhenium acid.

In the particular case of the complete method corresponding to the invention, heat treatment is carried out at a temperature of 600-800°C.

Another object of the invention is a method for the synthesis of propylene, comprising the metathesis reaction mixture of olefinic hydrocarbons With2-C4or one only of ethylene in the presence of rhenium oxide catalyst, corresponding to the invention.

Domestic the inventions

For preparation of rhenium oxide catalyst for metathesis of olefinic hydrocarbons using gamma-alumina, comprising fluorine in amount of 0.2 to 4.0 wt.%, that allows you to increase the activity of the catalyst corresponding to the invention, while maintaining the high selectivity and significantly reduce the content of rhenium in the catalyst. Rhenium oxide catalyst for metathesis of olefinic hydrocarbon contains 0.1 to 10.0 wt.% oxide of rhenium in the calculation of the gamma-alumina (γ-Al2O3), the content of fluorine in γ-Al2About3is 0.2 to 4.0 wt.%.

Getting rhenium oxide catalyst for the metathesis of olefins carried out by impregnation bionaturae media with a basis of gamma-alumina, comprising 0.2 to 4.0 wt.% fluorine as an anion in an aqueous solution of compounds of rhenium at 20-70°With at least 5 hours, drying the mass to remove the main quantity of the solvent and heat treatment in an oxidizing and/or inert atmosphere at a temperature of 600-900°for the decomposition of compounds of rhenium. The preferred mode of heat treatment is annealing of the catalyst in novosstroitelnaya atmosphere in the temperature range 600-800°C. Storing the thus prepared rhenium oxide catalyst is carried out in an inert gas environment.

Implemented the e method of producing propylene by using a rhenium oxide catalyst, relevant to the proposed invention is illustrated by Examples 1-8. The results of testing the proposed rhenium oxide catalyst in the metathesis reaction of ethylene (GOST 25070-87) and butenes-2 (99,1%, of the company "Aldrich") at 25-30°and atmospheric pressure are given in Table 1.

Table 1

Obtaining propylene by metathesis reaction of ethylene and butenes-2
ExampleThe composition of the catalyst, % wt.Conditions on ignitionConversion of butenes-2, %The selectivity for C3H6, %
fluorideRe2O7T °Wednesday10 min70 min10 min70 min
The known method0,1712550the air62,2-99,9-
12,012550the air84,281,098,1of 99.1
22,02550the air40,1-95,5 -
32,02750the air82,379,7of 98.299,2
40,172750the air39,3-99,9-
52,01750the air73,5-98,3-
62,01750argon74,0-98,4-
72,06750the air80,5-of 99.1-
82,00,5750the air57,6-of 98.2-

The results of using the proposed rhenium oxide catalyst in the reaction of synthesis of only propylene from ethylene using stage metathesis are shown in Table 2.

Table 2

The conversion of ethylene
Catalysis torus in example No.T °CAbout the lending rate, h-1The conversion of ethylene, %The selectivity of the formation of products, mol.%
With3H6ISO-C4H10C4H8-1C4H8-2ISO-C4H8With5+
610614005,662,21,12,06,817,410,5
12570013,264,82,02,08,014,88,4

Example 1.

Rhenium oxide catalyst was prepared by impregnating 10 grams of gamma-alumina containing 2.0 wt.% fluoride, an aqueous solution of ammonium perrhenate NH4ReO4when 20-70°C for 6 hours, dried at 110°and conducting thermal treatment in air at 550°C for 2 hours, replace the air purge with argon and the catalyst for 1 hour at the same temperature. The catalyst contains 12 wt.% Re2O7in the calculation of the gamma-alumina.

A mixture of ethylene and butenes-2 in a molar ratio of 2.7:1 served in a flow reactor with a bulk velocity 645 h at room temperature and atmospheric pressure. A sample taken after 10 min and 7 min after establishing the desired mode (table 1).

For comparison, the prepared catalyst in a known manner (Patent GB 1216587) and tested in the reaction of metathesis of ethylene and butenes-2 (as in Example 1).

Example 2.

Getting rhenium oxide catalyst is carried out as in Example 1, but the amount of ammonium perrhenate in aqueous solution for impregnation of gamma-aluminum oxide is taken as a sample containing 2 wt.% Re2O7in the calculation of the gamma-alumina. The catalyst was tested in the reaction of metathesis of ethylene and butenes-2 (as in Example 1).

Example 3.

Getting rhenium oxide catalyst is conducted according to Example 2, but the temperature treatment is carried out at 750°in an atmosphere of air, and then cooling the sample to 500°replace the air with an inert gas (argon), aged in inert gas for 1 hour. The catalyst was tested in the reaction of metathesis of ethylene and butenes-2 (as in Example 1).

Example 4.

The catalyst was prepared for comparison. Obtaining catalyst is conducted according to Example 3, but using gamma-aluminum oxide with a fluorine content of 0.17 wt.%. The catalyst was tested in the reaction of metathesis of ethylene and butene-2 (as in Example 1).

Example 5.

Getting rhenium oxide catalyst is conducted according to Example 3, but the amount of ammonium perrhenate in aqueous solution for impregnation of gamma-aluminum oxide is taken as a sample of the composition of 1 mA is.% Re 2O7in the calculation of the gamma-alumina. The catalyst was tested in the reaction of metathesis of ethylene and butenes-2 (as in Example 1).

Example 6.

Getting rhenium oxide catalyst is conducted according to Example 5, but the temperature treatment is carried out at 750°With inert gas (argon). The catalyst was tested in the reaction of metathesis of ethylene and butenes-2 (as in Example 1) and in the conversion of only ethylene, the ethylene concentration in the initial mixture was 16-32%. (Table 2).

Example 7.

Obtaining catalyst is conducted according to Example 3, but as the parent compound of rhenium using the oxide of rhenium Re2O7that is, dissolving, gives rhenium acid. The number of Re2O7in aqueous solution for impregnation of gamma-alumina obtained for a sample of 6 wt.% Re2O7in the calculation of the gamma-alumina. A mixture of ethylene and butenes-2 in a molar ratio of 2.1:1 served in a flow reactor with a bulk velocity 645 h-1at 26°and atmospheric pressure.

Example 8.

Getting rhenium oxide catalyst is conducted according to Example 3, but the amount of ammonium perrhenate in aqueous solution for impregnation of gamma-aluminum oxide is taken as a sample composition of 0.5 wt.% Re2O7in the calculation of the gamma-alumina. The catalyst was tested in the reaction of metathesis of ethylene and butenes-2 (as, the example1).

Industrial applicability

Rhenium oxide catalyst corresponding to the proposed invention can be used in the processes of metathesis of olefinic hydrocarbons and allows high yield and selectivity to propylene get transformations as a mixture of olefins With2-C4and only one of ethylene. Rhenium oxide catalyst corresponding to the proposed invention, is characterized by thermal stability and low content of rhenium oxide, which reduces the cost of preparation of the rhenium oxide catalyst.

1. Rhenium oxide catalyst for metathesis of olefinic hydrocarbons to bionaturae form the basis of gamma-alumina, which includes fluoride as an anion at the following content of components in the calculation of the gamma-aluminum oxide, wt.%:

Re2O70,1-10,0
Fluoride0,2-4,0

2. Rhenium oxide catalyst according to claim 1, in which the content Re2O7in the calculation of the gamma-aluminum oxide is 0.5 to 8.0 wt.%.

3. Rhenium oxide catalyst according to claim 1, in which the content of fluorine in the calculation of the gamma-aluminum oxide is 0.2-2.2 wt.%.

4. The method of obtaining the rhenium oxide catalyst for metathesis of olefinic hydrocarbons, including the non-impregnated bionaturae media with a basis of aluminium oxide with a solution of the compound of rhenium, drying the resulting mass and subsequent heat treatment in an oxidizing and/or inert medium, characterized in that as bionaturae media use gamma-alumina, comprising 0.2 to 4.0 wt.% fluorine calculated on gamma-alumina, and heat treatment is carried out at 600-900°C.

5. The method according to claim 4, characterized in that compounds of rhenium is chosen from the group comprising an oxide of rhenium (VII), ammonium perrhenate, rhenium acid.

6. The method according to claim 4, characterized in that the heat treatment is carried out at 600-800°C.

7. The method of synthesis of propylene, comprising the reaction of metathesis of olefinic hydrocarbon, C2-C4, characterized in that the reaction is carried out in the presence of a catalyst according to claims 1 to 3, and is subjected to metathesis mixture of olefinic hydrocarbons With2-C4or only one ethylene.



 

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