Ethylene oxidation catalyst and a method for preparing the same

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention provides catalyst for oxidation of ethylene into ethylene oxide, which catalyst contains no rhenium and no transition metals and comprises up to 30% silver on solid support and promoter combination mainly consisted of (i) component containing alkali metal on amount from 700 to 3000 ppm of the mass of catalyst and (ii) component containing sulfur in amount from 40 to 100% by weight of amount required to form alkali metal sulfate and, optionally, a fluorine-containing component in amount from 10 to 300 ppm of the mass of catalyst. Ethylene oxide is produced via reaction of ethylene with molecular oxygen in presence of above-defined catalyst.

EFFECT: increased selectivity of catalyst.

9 cl, 3 tbl

 

Background of invention

The scope to which the invention relates.

The present invention relates to a catalyst for oxidation of ethylene to ethylene oxide, consisting of the mandatory combination of silver, alkali metal such as cesium, and sulfur deposited on a carrier such as alumina, and the acquisition of ethylene oxide with the use of such a catalyst; optional in the composition of the catalyst can be activated fluorine-containing or chlorine-containing component. The catalyst contains almost no components containing rhenium or transition metals.

The known technical solutions

Processes for the production of ethylene oxide include ethylene oxidation in the vapor phase with molecular oxygen using a solid catalyst containing silver on a medium, for example aluminum oxide. Many researchers have made significant efforts to improve the effectiveness and efficiency silver catalyst for production of ethylene oxide. Detailed analysis of these efforts, experts predecessors are presented in U.S. patent No. 5051395.

Among the many earlier publications on this area, mention should be made of U.S. patent No. 4007135 (see also UK patent No. 1491447), which describes various silver catalysts for the production of oxides ethyl is on and propylene, containing a promoting amount of copper, gold, magnesium, zinc, cadmium, mercury, strontium, calcium, niobium, tantalum, molybdenum, tungsten, chromium, vanadium and/or preferably barium, excess amounts of these elements present in immobilized form in the pre-molded carrier as impurities or binder (column 2, lines 1-15), silver catalysts for the production of propylene oxide containing a promoting amount of at least one promoter selected from the group comprising lithium, potassium, sodium, rubidium, cesium, copper, gold, magnesium, zinc, cadmium, strontium, calcium, niobium, tantalum, molybdenum, tungsten, chromium, vanadium and barium in excess of the amounts of these elements present in immobilized form in the pre-molded carrier as impurities or binder (column 2, lines 16-34), and silver catalysts for the production of ethylene oxide and propylene containing (a) a promoting amount of sodium, cesium, rubidium and/or potassium, and (b) magnesium, strontium, calcium and/or preferably barium in promoting amount (column 3, lines 5-8).

U.S. patent No. 5057481 and associated patent No. 4908343 touch the silver catalysts of the oxidation of ethylene containing cesium and oxyanion element belonging to groups 3b-7b of the periodic system.

In U.S. patent No. 888889 described catalysts, suitable for the oxidation of propylene to propylene oxide containing elemental silver and modified by the connection element group I and J. Although the patent mentions the media, their examples are not given. The use of cesium are not mentioned.

In the publication of European patent No. 0266015 described silver catalysts on carriers promoted with rhenium, and contains an extensive list of possible additional promoters.

In U.S. patent No. 5102848 described catalysts suitable for the production of ethylene oxide, containing a carrier, impregnated with silver, which caused at least one cationic promoter, such as cesium, and a promoter containing (i) a sulfate anion, (ii) fluoride anion, and (iii) oxyanion element belonging to groups 3b-6b, inclusive, of the periodic system. The patent describes (columns 21 and 22) catalyst 6, containing silver, cesium, sulfur and fluorine on a medium containing cesium 1096 million-1; perhaps this catalyst is mentioned for comparison purposes (because it is outside the essence of the claimed catalysts).

In U.S. patent 5486628 described silver catalyst promoted with alkali metal, rhenium and rare-earth or lantanoides component.

U.S. patent 5011807 relates to a catalyst for oxidation of ethylene, containing silver, alkali metal, transition metal and sulfur on alumina as the carrier. For comparison purposes described catalysts containing silver, alkali metal and sulfur aluminum oxide as a carrier, providing less effective results compared to catalysts containing a transition metal.

In this huge amount of data, obfuscating the subject matter and often contradictory, the applicant created a new improved catalyst for the production of ethylene oxide.

Brief description of the invention

The present invention relates to an improved catalyst for the oxidation of ethylene on the media containing promoter combination consisting of the required number of component-based alkali metal, preferably cesium, in combination with the sulfur-containing component, and to the preparation and application of the catalyst; the catalyst contains almost no components on the basis of rhenium and transition metal, and may optionally contain fluorine-containing or chlorine-containing component.

Detailed description

Preferred catalysts prepared in accordance with the present invention contain up to about 30% (wt.) silver (in terms of metal)deposited on the surface and in the pores of the porous heat-resistant carrier. Effective amount of silver in excess of 20% of the total mass produce the RA, but the resulting catalysts are too expensive. The preferred value of the silver content of approximately 5-20% (in terms of metal) of the total mass of the catalyst, and particularly preferred are catalysts with a silver content of from 8% to 15%.

In addition to the silver catalyst in accordance with the present invention contains a promoter combination consisting of the required quantities of the alkali metal and sulfur. Mandatory quantity of promoter based on the alkali metal is at least 500 million-1by weight of catalyst (in terms of alkali metal); the preferred content of the alkali metal ranges from 700 million-1up to 3000 million-1by weight of the catalyst. The preferred alkali metal is cesium, although you can also use lithium, sodium, potassium, rubidium and mixtures thereof. For the introduction of a cesium component in the catalyst is successfully used the methods of impregnation, as described, for example, in U.S. patent 3962136.

For the implementation of the invention requires the presence of sulfur in the catalyst as a promoter component in the required amount in relation to alkali metal. Sulfur-containing component can be introduced into the solution for impregnation in the form of sulfate, such as cesium sulfate, ammonium sulfate, para-toluensulfonyl is the notes etc. In U.S. patent 4766105 described the use of sulfur-containing promoter agents, for example in column 10, lines 53-60, and this information is here included in the present description. The amount of sulfur (in terms of elemental sulfur) in relation to the mass of catalyst in accordance with the present invention is critical and should be from 10% to 150% of the equivalent amount required for the formation of a sulfate of an alkali metal such as Cs2SO4preferably from 40% to 100% of this amount.

Found that the use of relatively large amounts of alkaline metal, above which, in the usual case would be formed inactive catalyst, when used in combination with the above amount of sulfur produces a catalyst having high characteristics of activity and selectivity.

The catalyst may also contain as an optional component of the fluorine-containing or chlorine-containing promoter in the amount of 10 million-1up to 300 million-1(in terms of elemental halogen), preferably from 30 million1up to 100 million-1by weight of the catalyst. For this purpose you can apply fluoride or ammonium chloride, fluoride or chloride of an alkali metal etc.

The catalysts manufactured using media, aderrasi aluminum oxide, silicon dioxide, aluminium silicates, or combinations thereof. Preferred are media containing mainly alpha-alumina, in particular the media containing 15% (wt.) silicon dioxide. The media, which is given special preference, have a porosity of approximately 0.1-1.0 cm3/vol, preferably about 0.2-0.7 cm3/, Preferred carriers have a relatively small specific surface area, i.e. about 0.2-2.0 m2/g, preferably 0.4 to 1.6 m2/g and most preferably 0.5 to 1.3 m2/g (when determining the BET method, see J. Am. Chem. Soc. 60, 3098-16 (1938)). The porosity is determined using mercury porosimetry; see Drake and Ritter (Drake and Ritter, Ind. Eng. Chem. Anal. Ed. 17, 787 (1945)). The distribution of pores and pore diameters determined from the values of specific surface and measurements of apparent porosity.

For application in the industrial production of ethylene oxide carriers, it is advisable to mould into granules correct forms, spheres, rings, etc. it is Desirable that the carrier particles had an equivalent diameter in the range from 3 mm to 10 mm, preferably from 4 mm to 8 mm, which are usually compatible with the internal diameter of the tube that holds the catalyst. "Equivalent diameter" is the diameter of sphere having the same value of the ratio of the external surface (i.e. excluding internally the surface of the pores of the particles) to the extent that used particles of the medium.

The silver is preferably added to the carrier by immersing the carrier in the solution for impregnation, containing a complex of silver with an amine, or a minimum of moisture. The liquid containing the silver penetrates into the pores of the carrier under the action of absorption, capillary forces and/or vacuum. You can use either a single impregnation, or the number of sequential impregnation with intermediate drying or without it; the choice of methods of impregnation depends in part on the concentration of silver salts in solution. To obtain a catalyst with silver content within the preferred range of solutions for impregnating must contain, as a rule, from 5% (wt.) up to 50% (wt.) silver (in terms of metal). Specific values of the applied concentrations, of course, is determined, among other factors, the desired silver content in the catalyst, the nature of the medium, the viscosity of the liquid and the solubility of silver compounds.

The solution for impregnation, as described above, is a solution of a complex of silver with the amine; the preferred solution is described in U.S. patent No. 3702259, information from which is incorporated into this description by this reference. For the introduction of a cesium component it is advisable to use methods of the impregnating, described in U.S. patent No. 3962136.

For the prior, simultaneous or subsequent deposition of various promoters can be used known methods.

After impregnating separate the excess impregnating solution and the carrier, impregnated with silver and the promoter or promoters, is subjected to calcination or activation. In the most preferred embodiment of the invention, the calcination is carried out according to the description presented in properly transferred to the U.S. patent No. 5504052, issued April 2, 1996, and in co-pending application No. 08/587281, filed January 16, 1996, the details of which are included in the present description data links. The annealing is accomplished by heating the impregnated carrier, preferably gradually, to a temperature in the range from 120°500°With in a period of time sufficient to turn supported on a carrier of silver to metallic silver and to decompose organic compounds and remove them in the form volatile products.

In the course of the entire procedure impregnated carrier is kept in an inert atmosphere until the temperature exceeds 300°C. regardless of theoretical studies it is believed that at temperatures between 300°and the higher is the absorption of significant quantities of oxygen in the volume of the E. silver, that has a negative effect on the characteristics of the catalyst. Inert atmospheres from the point of view of the present invention are atmosphere practically free from oxygen.

An alternative method of annealing is the heating of the catalyst in a stream of air at a temperature not exceeding 300°C, preferably not higher than 280°C.

The catalysts prepared in accordance with the present invention, exhibit improved performance characteristics, in particular stability in the production of ethylene oxide by oxidation of ethylene in the vapor phase with molecular oxygen. In such processes typically use a reaction temperature from about 150°With up to 400°typically from about 200°to 300°and the pressure in the reactor in the range from 0.3 bar to 35 bar. The initial mixture of the reagents contain from 0.5% to 30% of ethylene and from about 3 to 15% oxygen, the rest are relatively inert substances such as nitrogen, carbon dioxide, methane, ethane, argon, etc. As a rule, on each pass through the catalyst enters the reaction only a part of the ethylene and unreacted materials are returned to the oxidation reactor after separation of the target product of ethylene oxide and delete the appropriate purge flow and carbon dioxide in order to avoid uncontrolled accumulated what I inert substances and/or products.

A disadvantage of the known catalyst with rhenium promoter is the uncertainty associated with the use of such catalysts. The catalysts in accordance with the present invention, does not contain rhenium, have high selectivity and high stability.

The invention is illustrated by the following examples.

Example 1

Prepared solution of silver using the following components (amounts stated in mass parts):

The silver oxide - 834 parts

Oxalic acid - 442 parts

Deionized water - 2808 parts

The Ethylenediamine - 415 parts

The silver oxide was mixed with water at room temperature, and then was gradually added oxalic acid. Stirred the mixture for 15 min; after this time the black color of the suspension of silver oxide was passed in grayish-brown color of silver oxalate. The mixture was separated by filtration and washed solid residue 3 l of deionized water.

The vessel containing the washed solid product was placed in an ice bath and stirred, slowly adding Ethylenediamine and water (a mixture of 72%/28%) so that the temperature of the reaction mass does not exceed 33°C. After adding all of the mixture of ethylene diamine with water, the solution was filtered at room temperature. Clear filtrate was used as the initial solution of the complex is silver with the amine for the preparation of the catalyst.

The media used in the examples was obtained from the company "Norton" (Norton Co.) and was made mostly of alpha-alumina in the form of cylindrical granules with the size of 5/16 inch (7.9 mm). The carrier had a specific surface area of 0.95 m2/g, specific pore volume of 0.3 cm2/g and an average pore diameter of 1.5 μm.

For the preparation of catalysts according to the examples about 185 parts of a solution of silver was mixed with various quantities of the following materials:

1. The solution of cesium hydroxide (8% (wt.) Cs in water).

2. A solution of ammonium fluoride (3% (wt.) F in water).

3. A solution of ammonium bisulfate (1% (wt.) S in water).

The number of solutions of the promoters selected in such a way as to obtain the concentration of the promoters listed in tables.

The mixture of the source of the silver solution and the solutions of the promoters was stirred to ensure homogeneity, and then added to 400 parts of the media. Moist medium was stirred for 10 min, after which he progulivali.

During annealing the deposition of silver compounds caused by heating the catalyst to a temperature of decomposition of silver salts. This effect was achieved by heating in a furnace having multiple heating zones, in a controlled atmosphere. The catalyst was placed on a belt conveyor, which consisted in a furnace at ambient temperature. By passing the utilizator from one zone to the next, the temperature was gradually increased. After passing the catalyst through seven heating zones, it reached 400°C. After the heating zones of the conveyor belt passed through a cooling zone in which the catalyst is gradually cooled to a temperature below 100°C. the Total residence time of the catalyst in the furnace was 22 minutes the Atmosphere in the furnace was regulated by introducing a stream of nitrogen in the different heating zones. In some cases, specified in the following tables, the calcination was carried out in air.

The catalysts were tested in a tube heated by a salt bath. Through the layer of catalyst is passed under pressure of 300 pounds per 1 square inch (2,068 MPa) gas mixture containing 15% ethylene, 7% oxygen and 78% inert substances, mainly nitrogen and carbon dioxide. The reaction temperature was set with the expectation of performance for ethylene oxide 160 kg/h at 1 m3catalyst; this temperature is indicated in the table.

The results of the tests of the catalysts are presented in the following tables.

Table 1
ExampleThe content of Cs, mn-1The content of S, mn-1The ratio S/2CsTemperature,

°
Selectivity, %The ethylene oxide in o the bottom stream (% vol.) Notes
1 (Comparative)10500025877,31,5
21050850,67223584,51,56

Found that, when the sulfur concentration is from 20% to 150% of the equivalent concentration of cesium, the activity and selectivity of the catalyst is significantly increased. This advantage is particularly evident in cases where the sulfur concentration is from 50% to 100% of the equivalent concentration of cesium. The two above examples illustrate the impact of adding sulfur, in which the reaction temperature was lowered to 23°and the selectivity was increased by 7% in the case of the introduction of sulfur in a critical amount compared to a similar catalyst which does not contain sulfur.

Introduction to high concentrations of catalyst component containing alkali metal, results in almost complete loss of activity of the catalyst. Introduction sulfur, however, provides good performance, as illustrated by the examples presented in the table below.

Table 2
ExampleThe content of the W Cs, million-1The content of S, mn-1The ratio S/2CsTemperature, °Selectivity, %The ethylene oxide in the output stream (% vol.)Notes
3 (Comparative)2450About026030,00,03The catalyst is not active
42551307124385,01,5
511660026065,20,25The catalyst is not active
610923052,3225383,31,5
7 (Comparative)00260250,001The catalyst is not active
839534080,8625483,61,5
95418 precision mechanical5650,87243is 83.81,37

From this group of examples shows that the introduction is sulfur leads to a sharp increase in the selectivity and activity of the catalyst (compare examples 3 and 4, 5 and 6 and examples 7 and 8).

In the absence of sulfur and with the introduction of high concentrations of cesium (in excess of 1000 million-1) the catalyst is practically not active. However, the introduction of sulfur in the specified concentration range provides extremely high selectivity in excess of 84%, and moderate activity, which follows from the following tables.

Table 3
ExampleThe content of Cs, mn-1The content of S, mn-1The ratio S/2CsThe Ag content, %PromotersTemperature, °CSelectivity, %The ethylene oxide in the output on current (% vol.)
1014591801,012,27Cs2SO4/NH4Cl23485,91,5
1122822741,011,09Cs2SO424285,91,5
121566980,5211,96Cs2SO4/CsOH/NH4Cl23986,61,5
1214809811,98Cs2SO4/CsOH/NH4Cl24586,71,5
141460980,5611,93Cs2SO4/CsOH/NH4Cl24386,81,5
1515801150,611,68Cs2SO4/CsOH/NH4Cl243of 87.01,5

In the above tables, the ratio S/2Cs equal to 1 means 100% of sulfur, equivalent required for the formation of cesium sulfate. The value of the ratio S/2Cs equal to, for example, 0,86, means 86% of sulfur, equivalent required for the formation of cesium sulfate.

1. Catalyst for oxidation of ethylene to ethylene oxide not containing rhenium and transition metals with up to 30 wt.% silver on a solid medium and containing a promoter combination consisting mainly of (1) a component containing an alkali metal in an amount of from 700 to 3000 million-1from the mass of the catalyst; and (2) a component containing sulfur in an amount of from 40 to 100% by weight, equivalent to the amount required for the formation of a sulfate of an alkali metal and, optionally, fluorine-containing component number (10 -300)m the n -1from the mass of the catalyst.

2. The catalyst according to claim 1, where the alkali metal is cesium.

3. The catalyst according to claim 1, where the carrier is alpha-alumina.

4. The catalyst according to claim 1, comprising from 5 to 20 wt.% silver.

5. The catalyst according to claim 1, containing a fluorine-containing component in an amount of from 10 to 300 million-1from the mass of the catalyst.

6. The catalyst according to claim 1, characterized in that the said solid carrier contains alpha-alumina containing up to about 15 wt.% silicon dioxide.

7. The catalyst according to claim 6, characterized in that the said solid support has a porosity of approximately 0.1-1.0 cm3/g and a specific surface area of about 0.2-1.0 m2/year

8. The catalyst according to claim 6, characterized in that the said solid support has a specific surface of approximately 0.5-1.3 m2/year

9. The method of producing ethylene oxide, comprising the reaction of ethylene with molecular oxygen in the presence of a catalyst according to claim 1.



 

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