The way to obtain a catalyst for production of vinyl acetate

 

The invention relates to a method for producing a catalyst for production of vinyl acetate by reaction of ethylene, oxygen and acetic acid containing porous media, porous surfaces of which is coated with an effective amount of copper, palladium and gold. The catalyst was prepared in stages, including pre-coating said carrier water-insoluble form of copper on the carrier with a preliminary coating is not water-soluble palladium compounds, recovery of the palladium compounds and, if not restored to earlier, insoluble form of copper to the catalytically effective amount of free metal impregnation copper - and palladium carrier solution Aurat potassium and restore Aurat potassium to catalytically effective amount of metallic gold. The method of the invention results in a catalyst in which Pd, Cu and Au form a layer of metal distribution on the catalyst carrier. The technical result is lower selectivity for CO2while maintaining higher levels of retention of the gold catalyst. 7 C.p. f-crystals, 1 table.

This invention relates to new and improved catalysts for Tata reaction of ethylene, oxygen and acetic acid using a catalyst consisting of metallic palladium, gold and copper supported on a carrier (see, for example, U.S. patent 5347046 and U.S. patent 5731457). Despite the fact that the way in which the use of such a catalyst, it is possible to obtain vinyl acetate with sufficient levels of performance, it is obvious that the preferred any technique by which you can achieve even greater performance during the service life of the catalyst.

More specifically, the foregoing catalysts containing metallic palladium, gold and copper, can be obtained by a process comprising a stage of impregnation of porous media one aqueous solution or separate solutions of water-soluble salts of these metals, the interaction of the absorbed water-soluble salts with an appropriate alkaline compound, for example sodium hydroxide, to "lock" these metals in the form of water insoluble compounds, such as hydroxides, and recovery of water insoluble compounds, such as ethylene or hydrazine, to translate these metals in the free metal form. This type of process has the disadvantage of having several stages, sometimes SAIs to consider the following links. In U.S. patent 5332710, issued July 26, 1994, Nicolau et al. that opened the way to obtain a catalyst for production of vinyl acetate by reaction of ethylene, oxygen and acetic acid, comprising the impregnation of porous media, water-soluble salts of palladium and gold, hold on medium of palladium and gold in the form of insoluble compounds by dipping and rolling the impregnated carrier in the reaction solution for the deposition of these compounds, and subsequent recovery of these compounds in the free metal form.

In U.S. patent 5347046, issued September 13, 1994, White et al., disclosed catalysts for vinyl acetate by reaction of ethylene, oxygen and acetic acid containing a metal of the group of palladium and/or its connection, gold and/or its connection, and copper, Nickel, cobalt, iron, manganese, lead or silver, or their compounds, preferably deposited on a material carrier.

In the United Kingdom patent 1188777, published on April 22, 1970, disclosed a method of simultaneous receipt of ester of unsaturated carboxylic acids, for example vinyl acetate, olefin, carboxylic acid and oxygen, and the corresponding carboxylic acid, for example acetic acid, from its aldehyde ispolzovanie compounds of any of various metals, for example, metallic gold, or a combination of gold, for example, such as Aurat potassium.

In U.S. patent 5700753 disclosed a catalyst for vinyl acetate (VA), obtained by addition of ORGANOMETALLIC complexes of gold to the previously restored palladium catalyst, obtained from Na2PdCl4. For ORGANOMETALLIC compounds of gold does not require the process of fixing.

In U.S. patent 5731457 described VA catalyst based on copper compounds not containing halogen.

In accordance with the invention provided the catalyst to obtain a vinyl acetate by reaction of ethylene, oxygen and acetic acid with a low selectivity for carbon dioxide, and the said catalyst contains a catalytically effective amount of metallic copper, palladium and gold deposited on the carrier, and received in stages, including pre-coating porous media catalytically effective amount of the water-insoluble form of copper, education on the media with pre-coating is not water-soluble palladium compounds, recovery of the palladium compounds and, if not restored to earlier, the water-insoluble form of copper, free IU the rata potassium to catalytically effective amount of metallic gold. The use of such a catalyst often leads to lower selectivity for carbon dioxide, which is usually accompanied by a higher performance vinyl acetate than using various conventional catalysts containing metallic palladium and gold.

Alternatively, the first carrier, pre-coated si, you can strike gold with subsequent carrier impregnated with palladium. The following alternative embodiment involves the use of reagents that do not contain sodium, as described in U.S. patent 5693586.

Disclosed is a method of obtaining a catalyst for the production of VA. Previously restored Pd/Au catalyst obtained by impregnation of the carrier with an aqueous solution ul2with subsequent fixation of NaOH. After this pre-coated si catalyst was impregnated with a solution of Pd, then realized fixation NaOH and then restored. Got a thin layer of Pd / C catalyst, which is then brought into contact with a solution of water Kaio2for the formation of the second layer of AU on the media. Ultimately was the catalyst layers of Pd and AI, where the AI was not required stage fixation. Pd and AU were distributed in the form of a thin metal layer on the pore selectivity for CO2reduced.

Although the presence of copper on the substrate in the area is largely covered with metallic palladium and gold, contributing to the reduction of CO2the selectivity of the catalyst was also found that the deposition of gold on a carrier in the form of a solution of Aurat potassium (Caio2after separately suffered and recovered palladium, with subsequent recovery of Aurat potassium to metallic gold, may further contribute to such lowering of the selectivity for CO2and may also contribute to the increased activity. Each of these reductions in the selectivity of carbon dioxide and increase the activity of the catalyst can lead to improved performance of vinyl acetate.

The material of the catalyst carrier consists of particles having any right or wrong forms, such as spheres, tablets, cylinders, rings, stars or other shapes, and may have dimensions such as diameter, length or width, comprising from about 1 to about 10 mm, preferably from about 3 to about 9 mm. are Preferred sphere of diameter from about 4 to about 8 mm, the Material of the carrier may consist of any suitable porous material, for example silicon dioxide, oxide of al is natov, spinel, silicon carbide, carbon, etc.,

The material of the carrier may have a density in the range, for example, from about 0.3 to about 1.2 g/ml, the absorbent capacity in the range of from about 0.3 to 1.5 g2O/g carrier, the surface area in the range of, for example, from about 10 to about 350, preferably from about 100 to about 200 m2/g, the average pore size in the range of, for example, from about 50 to about 2000 angstroms, and a pore volume in the range of, for example, from about 0.1 to about 2, preferably from about 0.4 to about 1.2 ml/g

Upon receipt of the catalyst used in this invention, the material of the carrier is first impregnated with an aqueous solution of water-soluble copper salt such as copper chloride (II), anhydrous or dihydrate, trihydrate nitrate copper (II) acetate copper (II) sulfate copper (II) bromide copper (II), etc. For impregnation of copper salt can be used impregnation methods known in the art. Preferably the impregnation can be carried out by the method of the "initial wetting", in which the quantity of a solution of copper compounds used for impregnation is from about 95 to about 100 percent of the absorption capacity of a material medium. The concentration of this solution is that the number is in the interval, for example, from about 0.3 to about 5.0, preferably from about 0.5 to about 3.0 g/l of catalyst.

After impregnation of the carrier with an aqueous solution of copper compounds copper "fix" that is precipitated in the form of a water-soluble compound such as a hydroxide by reaction with an appropriate alkaline compound, for example an alkali metal hydroxide, silicate, borate, carbonate or bicarbonate, in aqueous solution. The hydroxides of sodium and potassium are the preferred alkali locking connections. Alkali metal must be contained in the alkaline compound in the amount of, for example, from about 1 to about 2, preferably from about 1.1 to about 1.6 moles per mole of the anion present in soluble salts of copper. The fixation of copper can be performed by methods known in this field. However, it is preferable to carry out the fixation of copper by the method of initial wetting, in which the impregnated carrier is dried, for example at a temperature of 150oC for one hour, put in contact with a solution of alkaline compounds, approximately 95-100% of the pore volume of the media, and allowed to stand for a period of time of about 1/2 hour to about 16 hours; or Roto-immersion space overturn during at least the initial period of deposition, so, on the surface of the particle carrier or near it, and a thin band of precipitated copper compounds. Rotate or flip can be performed, for example, in the range of from about 1 to about 10 rpm for from about 0.5 to about 4 hours Estimated Roto-immersion method described in U.S. patent 5332710, the full disclosure of which is incorporated by reference.

Optionally, the medium containing a fixed copper can be cleaned up until the catalyst is substantially no traces of anions, such as halides, dried, for example, in a drying plant with fluidized bed under 100oC for one hour, ignited, for example by heating in air at 200oC for 18 h, and to restore, for example, in the gas phase in contact copper-containing media with gaseous hydrocarbon, such as ethylene (5% in nitrogen), for example, if 150oC for 5 h, or in the liquid phase in the contact carrier before washing and drying with an aqueous solution of hydrazine hydrate containing a molar excess of hydrazine with respect to copper, constituting, for example, from about 8:1 to about 12: 1, at room temperature, for from about 0.5 to about 3 hours, after which the carrier is washed and Talinya stage can be performed separately or in combination, these stages may not be necessary, since the washing, drying and, in particular, the recovery of copper compounds often can be performed appropriately by similar stages performed on the compound of palladium, which subsequently impregnated with copper-bearing media, which ultimately will be described next.

After that, the material of the carrier, containing an area of fixed-insoluble copper compounds such as copper hydroxide (II), or free of metallic copper, perhaps with a certain amount of oxide, process for applying a catalytically effective amount of palladium on a porous surface of the particles of the medium by methods similar to the methods that were previously described for the deposition of copper. So, the media that is pre-plated with copper, as described, can be impregnated with an aqueous solution of water-soluble palladium compounds. Examples of suitable water-soluble palladium compounds are palladium (II) chloride, palladium(II) chloride sodium (i.e. palladium(II)tetrachloride sodium, Na2PdCl4), palladium(II)tetrachloride, potassium nitrate, palladium (II) or sulfate, palladium (II). The preferred salt for impregnation is palladium(II)tetrachloride sodium, SLE who eat initial wetting, as the concentration of the solution is such that the number of elemental palladium absorbed in the carrier solution was equal to the desired predetermined amount. Impregnation is to provide, for example, from about 1 to about 10 grams of elemental palladium per liter of the final catalyst.

After impregnation of the carrier with an aqueous solution of water-soluble salts of palladium palladium is fixed, that is precipitated in the form of a water-soluble compound such as a hydroxide by reaction with an appropriate alkaline compound, for example an alkali metal hydroxide, as described in the case of copper, preferably by the initial moisture or Roto-immersion method.

If a fixed connection of palladium and copper was not previously restored, restore them later, for example, in the gas phase ethylene, after the initial washing and drying the catalyst containing the fixed connection of palladium and copper, if they are not restored to earlier, or in the liquid phase at room temperature in an aqueous solution of hydrazine hydrate followed by washing and drying, both as previously described for copper. Recovery of fixed compounds of palladium and copper Pref is the amount of the metal oxides.

After receiving any of the methods previously described catalyst containing palladium in the free metal form applied on pre-coated with copper material of the carrier, it is impregnated with the aqueous solution of Aurat potassium, preferably by the initial wetting. Thereafter, the catalyst is dried, so that the catalyst contained Aurat potassium in a quantity sufficient to provide, for example, from about 0.5 to about 10 g of elemental gold per liter of the final catalyst, the amount of gold constituting from about 10 to about 125% based on the weight of palladium present. Then Aurat potassium reduced to metallic gold by using any of the techniques previously described for the recovery of palladium from a fixed, i.e. not water soluble compounds of palladium on the surface of the carrier. When carrying out such repair Aurat potassium there is no need for intermediate stages of fixation gold on the media in the form of a water-soluble compound and washing of such connection to its full exemption from chloride ions, as described above for the catalysts containing palladium and gold. An exception similar to the stages of fixation and washing in a tie is about, the catalysts of this invention have been described primarily in connection with the catalysts containing only palladium, gold and copper as catalytically active metal, the catalyst may also contain one or more catalytically active metal elements in the form of free metal, oxide or mixture of free metal and oxide. These metallic elements can represent, for example, magnesium, calcium, barium, zirconium and/or cerium. If the catalyst is desirable any metal in addition to palladium, gold and copper, the media usually can be impregnated with a water-soluble salt of the metal dissolved in the same solution used for impregnation, the solution containing a water-soluble salt of palladium. Thus, the carrier can be impregnated with a water-soluble salts of palladium and an additional metal, which are then simultaneously record and restore the same way as described previously for palladium and copper. After that, the catalyst containing copper and palladium in the form of free metals and additional metal oxide and/or free metal impregnated awrah of potassium, which is then reduced to gold in the form of free metal, without premiato addition to gold.

One of the problems in obtaining VA catalysts was low retention of noble metal on the catalyst carrier. Using Kaio2predecessors, offers a way to obtain fine metal particles that do not contain salts, without including phase commit for sets AI. The advantage of the absence of phase commit for complexes AI is to increase retention of gold, because according to the methods of the preceding region AI is partially washed out of the catalyst during the stage of fixing/washing. In this way there was obtained a catalyst with high holding gold. The catalyst also contains cu, Pd, AU, distributed in a thin layer on the surface of the catalyst carrier or near it.

Mainly a catalyst containing palladium and gold in the free metal form, supported on a carrier, pre-coated with copper, can optionally be impregnated with a solution of acetate of an alkali metal, preferably potassium acetate or sodium acetate, and most preferably potassium acetate. After drying the final catalyst may contain, for example, from about 10 to about 70, preferably from about 20 to about 60 g of the acetate of alkali m is the total invention on the catalyst flows through the gas flow containing ethylene, oxygen or air, acetic acid and, preferably, alkali metal acetate. The composition of the gas stream can be varied within wide limits, taking into account the explosive limits. For example, the molar ratio of ethylene and oxygen may range from about 80:20 to about 98:2, the molar ratio of acetic acid and ethylene may range from about 2:1 to about 1:10, preferably from 1:2 to 1:5, and the content of gaseous alkali metal acetate may be from about 1 to about 100 parts per million based on the used mass of acetic acid. In addition, the gas stream may contain other inert gases such as nitrogen, carbon dioxide and/or saturated hydrocarbons. The reaction temperature that can be applied, are elevated temperatures, preferably temperatures in the range of approximately 150-220oC. the Applied pressure can be up to certain limits reduced pressure, normal pressure or increased pressure, preferably a pressure of up to about 20 excess atmospheres.

As an alternative embodiment of the invention can be used reagents that do not contain sodium. For example, you and the Alt ERN variant embodiment includes simultaneous impregnation activating connection auratum complex. For example, Aurat potassium and potassium acetate can be placed on Pd/Cu catalyst with the carrier at one stage.

The following alternative embodiment includes the preparation of the catalyst, in which Aurat add-covered si media, followed by impregnation of the support connection Pd.

Examples 1 to 4.

These examples illustrate the obtaining of the catalysts according to this invention, containing variable amounts of palladium and gold in the form of free metals.

In example 1, the material of the carrier, pre-coated water-insoluble form of copper and containing pre-reduced metal palladium was prepared as follows.

Unmodified material of the carrier in an amount of 250 ml, consisting of spheres of silicon dioxide Sud Chemie KA-160, having a nominal diameter of 7 mm, a density of about 0,562 g/ml and an absorbent capacity of approximately 0,583 n n2O/g carrier, the surface area of from about 160 to about 1752/g and a pore volume of about 0.68 ml/g, was impregnated first with the initial wetting of 82.5 ml of an aqueous solution of copper chloride (II), enough to supply approximately 1.9 grams of elemental copper per liter of catalyst. The media was dissolved in the solution for 5 min for ha is the act of processed media by Roto-immersion for 2.5 h at approximately 5 rpm with 283 ml of an aqueous solution of sodium hydroxide, obtained from the 50% mass/mass of NaOH/H2O in the amount of 120% of the required transformation of copper in its hydroxide. The solution was decanted from the treated media, which is then washed with deionized water to remove chloride ions (about 5 h) and dried overnight at 150oWith constant purging with nitrogen.

After that, the media, pre-coated water-insoluble hydroxide copper (II) infused by the initial wetting of 82.5 ml of aqueous solution of palladium(II) tetrachloride sodium, Na2PdCl4that is sufficient to provide about 7 grams of elemental palladium per liter of catalyst, and the medium was shaken to ensure complete absorption of the solution, fixation of palladium in the form of its hydroxide by Roto-immersion in aqueous NaOH solution, draining NaOH solution and washing and drying the carrier using the same procedures that were described previously for coating media hydroxide copper (II). Then copper and palladium restored to the free metal by contact of the medium with ethylene (5% in nitrogen) in the gas phase at 150oC for 5 h to obtain the media containing the nominal amount of 1.9 g/l of copper and 7 g/l previously restored palladium.

A, AI(OH)3when mixing 300 g of gold(III)tetrachloride sodium, Na2AuCl4containing a solution of 0.20 g AI/g of solution, and 73,6 g of 50% mass/mass of NaOH/H2O dissolved in 200 ml deionized water. Added an excess of NaOH to bring the pH to approximately 8 and mixed, and the solution was heated to 60oC for 3 h before formation of an orange precipitate. Filtering allocated orange solid, which was washed with deionized water to remove chloride ions and dried in a vacuum oven at 50oWith the current N2to obtain a red-orange precipitate AI(OH)3.

The hydroxide of gold in the amount of 0.5 g was mixed with 0.12 g of KOH in 35 ml of water and heated received the orange suspension up to 82-85oC and stirred at this temperature until dissolution of all precipitation, having a transparent yellow solution of Aurat potassium, Caio2in number, containing about 0.4 g of elemental gold. This solution was added to 100 ml of media containing a nominal amount of 1.9 g/l pre-printed and pre-restored copper and 7 g/l previously restored palladium, prepared as described above, using ethylene as a reducing AgentLog nitrogen. After that, the gold in the treated catalyst was restored 5% ethylene in N2if 120oC for 5 hours to obtain a catalyst containing a nominal amount of 4 g/l of free metallic gold on the media.

Finally, the catalyst was impregnated by the initial wetting with an aqueous solution containing 4 g of potassium acetate in 33 ml of N2Oh, and dried in a drying plant with fluidized bed under 100oWith over 1,5 hours

In example 2 using the procedure of example 1 was prepared a double batch of catalyst.

In example 3, followed the procedures of example 1, except that the amount of materials and reagents proportionally increased so as to obtain a portion in 6 l of a catalyst containing the same nominal amount of copper, palladium and gold, as in example 1.

In example 4, followed the procedures of example 1, except that the amounts of reactants used to produce the solution Aurat potassium, changed so that this solution contained 0.5, and not 0.4 g of elemental gold, and the final catalyst, therefore, would contain a nominal amount of 5 instead of 4 g/l of free metallic gold.

Nominal amount of Pd, Au and is as Pd and Au on the catalysts of examples 1-4, defined as a result of the analysis, and retention of metals presented in the table.

The catalysts of these examples were investigated for their activity and selectivity for various byproducts in the production of vinyl acetate by reaction of ethylene, oxygen and acetic acid. To accomplish this, approximately 60 ml of the catalyst prepared in the manner described above, was placed in a stainless steel mesh with possibility of temperature measurement using thermocouples as above, so below this grid. The grid was placed in the reactor Bertie recirculation type with continuous stirring and kept at a temperature of providing about 45% conversion of oxygen by means of the electric heater casing. Through the mesh missed a gas mixture consisting of about 50 normal liters (measured at normal temperature and pressure (NTD)) of ethylene, about 10 normal liters of oxygen, about 49 normal liters of nitrogen, 50 g of acetic acid and about 4 mg of potassium acetate, under a pressure of about 12 atmospheres, and the catalyst was getting old in these reaction conditions at least 16 h, before the two-hour mode, after which the reaction was completed. Analysis of the products is outside of the flow or the flow of products at approximately 10oFor optimal analysis of the final products of carbon dioxide (CO2), heavy fractions (TF) and ethyl acetate (EtOAc), the results of which are used to calculate the percentage selectively (selectivity) of these substances for each example, as shown in the table. The relative activity of the reaction, expressed in the form factor activity (activity), also listed in the table and is designed on the computer in the following way: in the computer program used a series of equations that correlate the activity factor with the temperature of the catalyst during the reaction), the conversion of oxygen, and a number of kinetic parameters of reactions during the synthesis of the VA. In a more General sense, the activity factor is inversely proportional to the temperature necessary to achieve permanent conversion of oxygen.

The values given in the table show that the catalysts of the invention in many cases can be used for the synthesis of vinyl acetate by reaction of ethylene, oxygen and acetic acid with a lower selectively CO2than in the case of different conventional and/or industrial catalysts containing palladium and gold, while at the same time higher or equal levels keep the congestion provides a more reproducible and high levels of retention of gold in the catalyst.

Claims

1. The way to obtain a catalyst for production of vinyl acetate by reaction of ethylene, oxygen and acetic acid comprising pre-coating the porous media, water-insoluble form of copper, education on pre-coated carrier is not water-soluble palladium compounds, recovery of palladium compounds and, if not restored to earlier, the water-insoluble form of copper to the catalytically effective amount of free copper metal, impregnation mentioned copper - and palladium-containing carrier with a solution of Aurat potassium to catalytically effective amount of metallic gold.

2. The method according to p. 1, in which said media containing metallic copper and palladium, which is impregnated with the said Aurat potassium, gain stage, comprising impregnating said carrier with an aqueous solution of water-soluble salts of copper, tying mentioned copper in the form of water-insoluble compounds by reaction with an appropriate alkaline compound, impregnating said carrier, pre-coated with copper, an aqueous solution of water-soluble palladium salt, the binding mentioned palladium in the form of a water-soluble seedstore water insoluble compounds of copper and palladium, present on the media.

3. The method according to p. 2, in which the aforementioned water-soluble salt of copper is a copper chloride and water-soluble palladium salt is a palladium (II) tetrachloride sodium.

4. The method according to p. 1, in which the aforementioned porous carrier contains from about 0.3 to about 5.0 grams of elemental copper per liter of catalyst.

5. The method according to p. 1, in which the aforementioned porous carrier contains from about 1 to about 10 g of palladium, and about 0.5 to about 10 grams of gold per liter of catalyst, and the amount of gold is from about 10 to about 71% based on the weight of palladium.

6. The method according to p. 1, wherein said catalyst is impregnated with a solution of acetate of an alkali metal.

7. The method according to p. 6, wherein said alkali metal acetate is the acetate, potassium acetate, which is applied to the catalyst in an amount of from about 10 to about 70 g/l of catalyst.

8. The method according to p. 1, in which palladium, copper and gold form a metallic shell, distributed on the catalyst carrier.

 

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