Catalyst and process for the selective hydrogenation of acetylenic compounds

 

(57) Abstract:

The invention relates to catalysts and methods for selective hydrogenation of acetylene hydrocarbons, in particular ethylene by selective hydrogenation of acetylene in the gas phase, and may find application in processes for purifying gas mixtures from impurities acetylene. The problem solved by the present invention is to develop an efficient method of hydrogenation of acetylene hydrocarbons using catalysts containing precious metals. This task is solved by a method for selective hydrogenation of acetylene hydrocarbons at a temperature of 0-200oC and a pressure of 1-100 at on the catalyst comprising a product recovery in the atmosphere of hydrogen or nitric mixture at 250-800oFrom gidroksicarbonata cobalt and one or more metals 3 or 4 periods in the oxidation state 2+ or 3+ with structure type hydrotalcite, CoxMy(OH)2(x+y)CO3mo2About atomic ratio of x: y is from 0.1 to 10, where 0n<100, or product recovery in the atmosphere of hydrogen or nitric mixture at 250-800oWith product heat treatment at 300-900oFrom gidroksicarbonata cobalt and about>/BR>CoxMy(OH)2(x+y)CO3mo2About atomic ratio of x:y is from 0.1 to 10, where 0n<100. As acetylene hydrocarbons used acetylene, methylacetylene, vinylacetylene. The use of the claimed catalysts can significantly extend the temperature range of effective processes, selective hydrogenation of acetylene in the presence of significant quantities of CO and to avoid the use of expensive noble metals. 2 C. and 8 C.p. f-crystals, 3 tables.

The invention relates to catalysts and methods for selective hydrogenation of acetylene hydrocarbons, in particular ethylene by selective hydrogenation of acetylene in the gas phase and may find application in processes for purifying gas mixtures from impurities acetylene.

Selective hydrogenation of acetylene, present as impurities in the olefin (e.g. ethylene, obtained during thermal cracking of ethane), now usually made using a palladium-silver catalyst fixed on an aluminum oxide, mainly in accordance with the invention [US Pat. 4404124, 13.09.1983, C 07 C 5/08; US Pat. 4484015, 20.11.1984, C 07 C 5/08] and also [US Pat. 5488024, 30.01.1996, C 07 C 5/09, B 01 J 23/50; US Pat. is odya of the following two conditions: acetylene must be effectively removed from the mixture (up to a concentration of 10-20 ppm) and only a small amount of ethylene reacts with hydrogen, forming ethane. The first requirement determines the minimum temperature of the process Tminthe second requirement is that the maximum temperature of the process Tmaxabove which adverse reaction of hydrogenation of ethylene leads to a significant loss of ethylene. In General, the stability of the process of selective hydrogenation of acetylene is higher, the greater the difference between the two critical temperatures, i.e. wider temperature range effective process.

Patent US 5648576 says the process of selective hydrogenation of acetylene compounds in the gas phase using a catalyst containing alumina, palladium, metal band 1B, and possibly one of the alkali metals. With 80% of the active component (Pd and Ag) in the outer layer of the grain thickness of 0.2 radius of the grain. The authors of these inventions declare that this distribution of the active component along the radius of the grains of the catalyst significantly improves the properties of the catalyst, including reducing the rate of formation of ethane and products of oligomerization, i.e. providing better selectivity of the process. Characteristics of the described examples are shown in table 1 (similar to 1).

Patent US 5510550 WENRA and the inorganic carrier and the recovered liquid composition, containing the reducing agent. The authors discuss the invention of claim extended temperature range stable process (Tminand Tmax) in comparison with existing analogues - US Pat. 4404124 and US Pat. 4484015. Characteristics of the most successful examples in the invention US Pat. 5510550, are shown in table 2 (analogues 2 and 3). These catalysts allow stably and effectively carry out the process, but the width of the temperature range of the process of using them is not very large and does not exceed 70oC.

Due to the fact that the selective hydrogenation of acetylene is substantially exothermic reaction and the situation is complicated by the occurrence of more exothermic side reactions of hydrogenation of ethylene, limited temperature range effective process makes the process quite complicated. Usually use the schema from 2-5 consecutive adiabatic catalyst with intermediate cooling of the working mixture [US Pat. 6011188, 04.01.2000, C 07 C 5/08].

Another problem that occurs when using a Pd-containing catalysts is their sensitivity to the presence in the mixture monoxide diversified its use as catalyst for the selective hydrogenation of acetylene in the mixture containing significant concentrations (>1 vol.%). The need to create a catalyst that is resistant to the presence of high concentrations of CO, justified in detail in [US Pat. 4705906, 10.11.1987, C 07 C 5/05] and determined the existence of processes [EP 0163385 B 1, 12.10.1988, 01 3/44; EP 0178853 B 1, 25.04.1990, 01 3/02], producing a mixture of acetylene, ethylene, and hydrogen. For the removal of acetylene such mixtures in US Pat. 4705906 encouraged to use catalysts based on zinc oxide. However, these catalysts are much less selective in comparison with Pd-containing catalysts: selectivity to ethylene, according cited in the cited patent examples, does not exceed 80% (see table 3, similar to the 4). When this occurs the formation of ethane and higher hydrocarbons in large quantities. Lack of catalysts based on ZnO is a high temperature process for selective hydrogenation of using them - as a rule, it exceeds 250oC.

An additional circumstance, forced to continue the search for catalysts for selective hydrogenation of acetylene, is the high cost and limited stocks of palladium.

Known processes for the selective hydrogenation of talization significantly worse than for the known Pd-containing catalysts. Thus, in patent US Pat. 3691248, 12.09.1972, C 07 C 11/00, it is proposed to carry out selective acetylene hydrogenation catalyst containing Ni or Ni, and at least one of the metals of the VI or VIII group, with a ratio of Ni: Me from 0.5 to 500. Hydrogenation of the ethylene-ethane mixture containing about 85 ppm acetylene, 23% ethane and 77% of ethylene at 77oC, a pressure of 26 atmospheres and a contact time with the catalyst 0.7, led to the removal of acetylene to 1 ppm. However, the amount of ethylene in the mixture decreased, and ethane increased; the ratio of the ethylene-ethane was changed from 3.3 starting up 2.1 final, which indicates the low selectivity of the process.

As a prototype of the present invention features a process for the selective hydrogenation of acetylene using as catalyst hydride magnesium-cobalt intermetallic, as proposed in patent [RU Pat. 1638866, 08.04.1988, C 07 C 5/09, B 01 J 31/02]. In the cited patent States that the catalyst provides 100% selectivity. Performance characteristics of the catalyst of the prototype are shown in table 1. The disadvantage of the catalyst is a high temperature process for the selective hydrogenation is not below 200oC.

's hydrocarbons, using catalysts containing precious metals.

This task is solved by a catalyst for the selective hydrogenation of acetylenic compounds containing in their composition of cobalt and one or more metals 3 or 4 periods in the oxidation state 2+ or 3+, with respect to atomic fraction of cobalt to the total of the atomic fractions of other metals is from 0.1 to 10.

The catalyst is a product recovery in the atmosphere of hydrogen or nitric mixture at 250-800oFrom gidroksicarbonata cobalt and one or more metals 3 or 4 periods in the oxidation state 2+ or 3+ with structure type hydrotalcite, CoxMy(OH)2(x+y)CO3n H2O with an atomic ratio of x:y is from 0.1 to 10, where 0n<100 or product recovery in the atmosphere of hydrogen or nitric mixture at 250-800oWith product heat treatment at 300-900oFrom gidroksicarbonata cobalt and one or more metals 3 or 4 periods in the oxidation state 2+ or 3+ with structure type hydrotalcite,

CoxMy(OH)2(x+y)CO3n H2O with an atomic ratio of x:y is from 0.1 to 10, where 0n<100. As metals 3 or 4 periods use aluminium is and additionally may contain Nickel, while respecting the atomic relations of cobalt to Nickel is from 0.1 to 10 and relations atomic fraction of Nickel to the sum of the atomic fractions of other metals from 0.01 to 0,49. In the catalyst composition can optionally enter one or more base metals 5 and 6 periods, subject to the relations of the sum of the atomic fractions of metals 3 and 4 periods to the total atomic fraction of metals 5 and 6 periods of at least 2.

The task is also solved by a method for selective hydrogenation of acetylene hydrocarbons at a temperature of 0-200oC and a pressure of 1-100 antibodies in the presence of a cobalt containing catalyst of the above composition. As acetylene hydrocarbons used acetylene, methylacetylene, vinylacetylene. The initial mixture may contain carbon monoxide in an amount of from 0.1 to 40 vol.%.

The nature and effectiveness of the method is illustrated by examples.

Example 1. The process of selective hydrogenation of acetylene is carried out by passing a mixture of ethylene-acetylene containing 0.25% vol. acetylene and of 99.75 about. % ethylene with hydrogen in the ratio of 1:5 through the catalyst bed at temperatures up to 200oAnd atmospheric pressure. Using the catalyst obtained by reduction in a stream of hydrogen at 450oWith the product of the heat treatment in a stream of inert gas (argon) at a temperature of 500oFrom gidroksicarbonata cobalt-aluminum containing Co and Al in atomic with the>

Gidroksicarbonat cobalt-aluminium receive joint precipitation of metal ions from aqueous solutions of their nitrates aqueous solution of sodium carbonate at pH 7 and a temperature of 70oC. Identification of patterns obtained gidroksicarbonata cobalt-aluminum, carried out by the method of x-ray analysis and infrared spectroscopy showed that the structure of this compound is completely identical to the structure of hydrotalcite.

Performance characteristics of the catalyst are shown in table 1. Catalyst provides purification of the ethylene-acetylene mixture of acetylene to clean 10 ppm at temperatures significantly lower than in the known methods of selective hydrogenation (prototype). The catalyst provides a selectivity approaching 100%. The speed of the adverse reactions of hydrogenation of ethylene to ethane is significantly small even at temperatures above 130o(See table 1). In General, the temperature range of effective processes (the content of the acetylene less than 10 ppm, the content of ethane less than 20,000 ppm) is wider than in the known methods (see table 2).

Example 2. Analogously to example 1, but the process is carried out using a catalyst obtained by reduction in the current video structure type hydrotalcite, Co2Al2(OH)8CO3n H2O.

Gidroksicarbonat cobalt-aluminum get like gidroksicarbonata cobalt-aluminum in example 1.

Performance characteristics of the catalyst are shown in table 1. Catalyst provides purification of the ethylene-acetylene mixture of acetylene to clean 10 ppm at temperatures significantly lower than in the known methods of selective hydrogenation (prototype). The catalyst provides a selectivity approaching 100%. The speed of the adverse reactions of hydrogenation of ethylene to ethane is significantly small even at temperatures above 120o(See table 1). In General, the temperature range of effective processes (the content of the acetylene less than 10 ppm, the content of ethane less than 20,000 ppm) is wider than in the known methods (see table 2).

Example 3. Analogously to example 1, but the process is executed by passing through a layer of catalyst mixtures containing 0,055% vol. acetylene, 16.6% of ethylene, 46% vol. hydrogen, 30% vol. WITH and 7.3% vol. of nitrogen.

Performance characteristics of the catalyst are shown in table 3. The catalyst provides a cleaning gas mixture of acetylene to the purity of less than 5 ppm at 110oC and a contact time of 1.0 seconds, which is not the existence of hydrocarbons in3+significantly small in a wide temperature range (see table 3). The deterioration of the catalyst activity compared with example 1 appears to be insignificant. Deterioration of the selectivity of the catalyst in comparison with example 1 is not marked.

Example 4. Analogously to example 1, but the process is carried out using a catalyst obtained by reduction in a stream of hydrogen at 450oWith the product of the heat treatment in a stream of inert gas (argon) at a temperature of 500oFrom gidroksicarbonata cobalt-zinc-aluminium containing Co, Al and Zn at the atomic ratio of Co:Al:Zn=1:2:1, with structure type hydrotalcite, CoZnAl2(OH)8CO3n H2O.

Gidroksicarbonat cobalt-zinc-aluminium receive joint precipitation of metal ions from aqueous solutions of their nitrates aqueous solution of sodium carbonate at pH 7 and a temperature of 70oC. Identification of patterns obtained gidroksicarbonata cobalt-zinc-aluminium, carried out by the method of x-ray analysis and infrared spectroscopy showed that the structure of this compound is completely identical to the structure of hydrotalcite.

The characteristic operation of the catalyst are shown in table 1. The catalyst to ensure the rounds are significantly lower than in the known method of selective hydrogenation (prototype). The speed of the adverse reactions of hydrogenation of ethylene to ethane is significantly low at temperatures up to 180o(See table 1). In General, the temperature range of effective processes (the content of the acetylene less than 10 ppm, the content of ethane less than 20,000 ppm) is significantly wider than in the known methods (see table 2).

Example 5. Analogously to example 4, but the process is executed by passing through a layer of catalyst mixtures containing 0,055% vol. acetylene, 16.6% of ethylene, 46% vol. hydrogen, 30% vol. WITH and 7.3% vol. of nitrogen.

Performance characteristics of the catalyst are shown in table 3. The catalyst provides a cleaning gas mixture of acetylene to the purity of less than 5 ppm at 110oC and a contact time of 1.0 seconds, which is not worse than the activity of the known catalysts. The speed of unwanted side reactions of hydrogenation of ethylene to ethane and hydrocarbon formation Sz+ significantly small in a wide temperature range (see table 3). The deterioration of the catalyst activity compared with example 3 appears to be insignificant. Deterioration of the selectivity of the catalyst in comparison with example 3 is not marked.

Example 6. Analogously to example 1,oFrom the product of thermal decomposition in a stream of inert gas (argon) at a temperature of 500oFrom gidroksicarbonata cobalt-magnesium-aluminum-containing Co, Al and Mg atomic ratio of Co: Al: Mg=1:2:1, with structure type hydrotalcite, CoMgAl2(OH)8CO3n H2O.

Gidroksicarbonat cobalt-magnesium-aluminium receive joint precipitation of metal ions from aqueous solutions of their nitrates aqueous solution of sodium carbonate at pH 10, and a temperature of 70oC. Identification of patterns of gidroksicarbonata cobalt-magnesium-aluminum, carried out by the method of x-ray analysis and infrared spectroscopy showed that the structure of this compound is completely identical to the structure of hydrotalcite.

The characteristic operation of the catalyst are shown in table 1. Catalyst provides purification of the ethylene-acetylene mixture of acetylene to clean 10 ppm at temperatures significantly lower than in the known method of selective hydrogenation (prototype). The speed of the adverse reactions of hydrogenation of ethylene to ethane is significantly low at temperatures up to 140o(See table 1). In General, the temperature range of effective processes (the content of the acetylene less than 10 ppm ocess carried out using a catalyst, received and recovery in a stream of hydrogen at 450oFrom the product of thermal decomposition in a stream of inert gas (argon) at a temperature of 500oFrom gidroksicarbonata cobalt-calcium-scandium-chromium-aluminum containing Co, CA, Sc, Cr and Al atomic ratio of Co:Ca:Sc:Cr:Al=4:1:0.25:1:3.75, structure type hydrotalcite, Co1.6Ca0.4Sc0.1Cr0.4Al1.5(OH)8CO3n H2O.

Gidroksicarbonat cobalt-calcium-scandium-chromium-aluminium receive joint precipitation of metal ions from aqueous solutions of their nitrates aqueous solution of sodium carbonate at pH 7 and a temperature of 70oC. Identification of patterns of gidroksicarbonata cobalt-calcium-scandium-chromium-aluminum, carried out by the method of x-ray analysis and infrared spectroscopy showed that the structure of this compound is completely identical to the structure of hydrotalcite.

The characteristic operation of the catalyst are shown in table 1. Catalyst provides purification of the ethylene-acetylene mixture of acetylene to clean 10 ppm at temperatures significantly lower than in the known method of selective hydrogenation (prototype). The speed of the adverse reactions of hydrogenation of ethylene to ethane sudeste process (the content of the acetylene less than 10 ppm and the content of ethane less than 20,000 ppm) not worse than in the known methods.

Example 8. Analogously to example 1, but the process is carried out using a catalyst obtained and restoration in a stream of hydrogen at 450oFrom the product of thermal decomposition in a stream of inert gas (argon) at a temperature of 500oFrom gidroksicarbonata cobalt-copper-iron-gallium-aluminum containing Co, cu, Fe, Ga and Al atomic ratio of Co:Cu:Fe:Ga:Al=1:0.1:0.1:0.1:0.9, structure type hydrotalcite, Co2Cu0.2Fe0.2Ga0.2Al1.8(OH)8.8CO3nH2O.

Gidroksicarbonat cobalt-copper-iron-gallium-aluminium receive joint precipitation of metal ions from aqueous solutions of their nitrates aqueous solution of sodium carbonate at pH 7 and a temperature of 70oC. Identification of patterns of gidroksicarbonata cobalt-copper-iron-gallium-aluminum, carried out by the method of x-ray analysis and infrared spectroscopy showed that the structure of this compound is completely identical to the structure of hydrotalcite.

The characteristic operation of the catalyst are shown in table 1. Catalyst provides purification of the ethylene-acetylene mixture of acetylene to clean 10 ppm at temperatures significantly lower than in the known method Centeno small at temperatures up to 120o(See table 1). In General, the temperature range of effective processes (the content of the acetylene less than 10 ppm and the content of ethane less than 20,000 ppm) is not worse than in the known methods.

Example 9. Analogously to example 1, but the process is carried out using a catalyst obtained and restoration in a stream of hydrogen at 450oFrom the product of thermal decomposition in a stream of inert gas (argon) at a temperature of 500oFrom gidroksicarbonata cobalt-Nickel-magnesium-aluminum-containing Co, Ni, Mg and Al atomic ratio of Co:Ni:Mg:Al=1:0.1:1:2, with the structure type hydrotalcite, CoNi0.1MgAl2(OH)8.2CO3n H2O.

Gidroksicarbonat cobalt-Nickel-magnesium-aluminium receive joint precipitation of metal ions from aqueous solutions of their nitrates aqueous solution of sodium carbonate at pH 7 and a temperature of 70oC. Identification of patterns of gidroksicarbonata cobalt-Nickel-magnesium-aluminum, carried out by the method of x-ray analysis and infrared spectroscopy showed that the structure of this compound is completely identical to the structure of hydrotalcite.

The characteristic operation of the catalyst are shown in table 1. Catalyst provides purification of the ethylene-accting hydrogenation (prototype). The speed of the adverse reactions of hydrogenation of ethylene to ethane is significantly low at temperatures up to 120o(See table 1). In General, the temperature range of effective processes (the content of the acetylene less than 10 ppm and the content of ethane less than 20,000 ppm) is not worse than in the known methods.

Example 10. Analogously to example 1, but the process is carried out using a catalyst obtained and restoration in a stream of hydrogen at 450oFrom the product of thermal decomposition in a stream of inert gas (argon) at a temperature of 500oFrom gidroksicarbonata cobalt-strontium-barium-aluminum containing Co, Sr, BA and Al atomic ratio of Co:Sr:Ba:Al=1.6:0.3:0.2:2, with the structure type hydrotalcite, Co1.6Sr0.3VA0.2Al2(OH)8.2CO3n N2O.

Gidroksicarbonat cobalt-strontium-barium-aluminium receive joint precipitation of metal ions from aqueous solutions of their nitrates aqueous solution of sodium carbonate at pH 9, and a temperature of 70oC. Identification of patterns of gidroksicarbonata cobalt-strontium-barium-aluminum, carried out by the method of x-ray analysis and infrared spectroscopy showed that the structure of this compound completely identity is R provides purification of the ethylene-acetylene mixture of acetylene to clean 10 ppm at temperatures significantly lower than in the known method of selective hydrogenation (prototype). The speed of the adverse reactions of hydrogenation of ethylene to ethane is significantly low at temperatures up to 120o(See table 1). In General, the temperature range of effective processes (the content of the acetylene less than 10 ppm and the content of ethane less than 20,000 ppm) is not worse than in the known methods.

Example 11. Analogously to example 1, but the catalyst composition further added molybdenum compliance with the atomic ratio of Co:Mo=9.

Gidroksicarbonat cobalt-molybdenum-aluminium receive joint precipitation of metal ions from aqueous solutions of their nitrates aqueous solution of sodium carbonate at pH 7 and a temperature of 70oC. Identification of patterns of gidroksicarbonata cobalt-molybdenum-aluminum, carried out by the method of x-ray analysis and infrared spectroscopy showed that the structure of this compound is completely identical to the structure of hydrotalcite, l(OH)4(Mo2O7)0,055(CO3)0,445n N2O.

The characteristic operation of the catalyst are shown in table 1. Catalyst provides purification of the ethylene-acetylene mixture of acetylene to clean 10 ppm when temperatoron reaction of hydrogenation of ethylene to ethane is significantly low at temperatures up to 120o(See table 1). In General, the temperature range of effective processes (the content of the acetylene less than 10 ppm and the content of ethane less than 20,000 ppm) is not worse than in the known methods. The introduction of the molybdenum in the catalyst composition does not lead to a significant deterioration in its characteristics.

Example 12. Analogously to example 1, but the catalyst composition further added lanthanum compliance with the atomic ratio Co:La=9.

Gidroksicarbonat cobalt-lanthanum-aluminum get by joint precipitation of metal ions from aqueous solutions of their nitrates aqueous solution of sodium carbonate at pH 7 and a temperature of 70oC. Identification of patterns of gidroksicarbonata cobalt-lanthanum-aluminum, carried out by the method of x-ray analysis and infrared spectroscopy showed that the structure of this compound is completely identical to the structure of hydrotalcite, Coa 1.8Laof 0.2Ala 1.8(OH)7,6CO3n N2O.

The characteristic operation of the catalyst are shown in table 1. Catalyst provides purification of the ethylene-acetylene mixture of acetylene to clean 10 ppm at temperatures significantly lower than in the known method of selective hydrogenation (prototype). Rate tender the table 1). In General, the temperature range of effective processes (the content of the acetylene less than 10 ppm and the content of ethane less than 20,000 ppm) is not worse than in the known methods. The introduction of lanthanum in the composition of the catalyst does not affect its performance.

Thus, the use of the claimed catalysts can significantly extend the temperature range of effective processes, selective hydrogenation of acetylene in the presence of significant quantities of CO and to avoid the use of expensive noble metals.

1. Catalyst for selective hydrogenation of acetylene hydrocarbons containing in its composition cobalt, characterized in that it contains one or more metals 3 and 4 periods in oxidation state 2+ or 3+, with respect to atomic fraction of cobalt to the total of the atomic fractions of other metals is from 0.1 to 10.

2. The catalyst p. 1, characterized in that it is the product of the recovery in the atmosphere of hydrogen or nitric mixture at 250-800oFrom gidroksicarbonata cobalt and one or more metals 3 or 4 periods in the oxidation state 2+ or 3+ with structure type hydrotalcite, CoxMy(tives such as those he is a product of the recovery in the atmosphere of hydrogen or nitric mixture at 250-800oWith product heat treatment at 300-900oFrom gidroksicarbonata cobalt and one or more metals 3 or 4 periods in the oxidation state 2+ or 3+ with structure type hydrotalcite, CoxMy(OH)2(x+y)CO3n N2About atomic ratio of x: y is from 0.1 to 10, where 0 n <100.

5. The catalyst PP. 1-4, characterized in that gidroksicarbonat structure type hydrotalcite further comprises Nickel, while respecting the atomic relations of cobalt to Nickel is from 0.1 to 10 and relations atomic fraction of Nickel to the sum of the atomic fractions of other metals from 0.01 to 0,49.

6. The catalyst PP. 1-5, characterized in that it additionally contains one or more metals from the group comprising strontium, molybdenum, barium and lanthanide, subject to relations of the sum of the atomic fractions of metals 3 and 4 periods to the total atomic fraction of strontium, molybdenum, barium and lanthanide not less than 2.

7. How selective guide is causesa fact, as the catalyst used, the catalyst according to any one of paragraphs. 1-6.

8. The method according to p. 7, characterized in that as acetylene hydrocarbons used acetylene, methylacetylene, vinylacetylene.

9. The method according to PP. 7 and 8, characterized in that the starting mixture contains carbon monoxide in an amount of from 0.1% to about 40. %.

10. The method according to PP. 7-9, characterized in that the selective hydrogenation of acetylenic compounds is carried out at 0-200oC.

 

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