Method for selective receipt of acetic acid and the catalyst

 

(57) Abstract:

The invention relates to a new method for selective receipt of acetic acid and used in the catalyst. Method for selective receipt of acetic acid from a gaseous feedstock containing ethane, or a mixture of ethane and ethylene, and oxygen, at elevated temperatures is that the gaseous feedstock is brought into contact with a catalyst obtained by mixing solutions of all of the catalytic elements, followed by drying and, if necessary, calcification, containing the elements Mo, Pd, X and Y in the gram-atom ratios a:b:c:d in combination with oxygen

MoaPdbXcYd(I)

where X is one or more of the elements selected from the group of Nb, Ti, V, or W; Y is one or more of the elements selected from the group of Al, Bi, Cu, Ag, Au, K, Rb, Cs, Mg, Ca, Sr, Ba, Zr, Sb and Sn; the indices a, b, C and d denote the gram-atom ratios of the respective elements, where a=1; b>0; C>0 and d=0-2, provided that the catalyst as X contains at least the elements of V and Nb, and that the Ministry of Defense and the elements of X are not based on heteropolyacids, and that if one element Y Zr means, one element of X is W, and if one element Y oznachnoe acid allows for maximum mild conditions to oxidize ethane or a mixture of ethane and ethylene with high selectivity, up to 86% acetic acid. 2 C. and 8 C.p. f-crystals, 2 tab.

The invention relates to a method for selective receipt of acetic acid catalytic gas-phase oxidation of ethane and/or ethylene in the presence of palladium catalyst.

Oxidative dehydrogenation of ethane to ethylene in the gas phase at temperatures above 500oSince it is known, for example, from U.S. patent US-A-4250346, US-A-4524236 and US-A-4568790.

Thus, in U.S. patent US-A-4250346 describe the use of a catalytic composition containing the element molybdenum, X and Y in the ratio a:b:C, for the conversion of ethane to ethylene, while X denotes chromium (CR), manganese (MT), niobium (Nb), tantalum (TA), titanium (Ti), vanadium (V) and/or tungsten (W), and Y denotes the bismuth (Bi), selenium (Se), cobalt (Co), copper (cu), iron (Fe), potassium (K), magnesium (MD), Nickel (Ni), phosphorus (P), lead (Pb), antimony (Sb), silicon (Si), tin (Sn), thallium (Tl) uranium (U), a=1, b=0.05 to 1, and s=0-2. The sum of the values for Co, Ni and/or Fe must be less than 0.5. The reaction is preferably conducted in the presence of the applied water. The above catalysts can also be used for the oxidation of ethane to acetic acid, and the efficiency of conversion into acetic acid is about 18% conversion of ethane to 7.5%.

On the contrary, in European patent application EP-IN-0294845 describes how selective obtaining acetic acid from ethane, ethylene or mixtures thereof and oxygen in the presence of a mixture of catalysts containing at least (A) one consisting of calcined catalyst of the formula MoxVyor MoxVyZywhere Z can be one or more of the metals Li, Na, Be, SB, CA, Sr, BA, Zn, Cd, Nd, Sc, Y, La, CE, Al, Tl, Ti, Zr, Hf, Pb, Nb, TA, As, Sb, Bi, Cr, W, U, Te, Fe, Co and Ni, and x=0.5 and 0.9, y=0.1 to 0.4, and z=0.001 to 1, and B) the catalyst for the hydration of ethylene and/or a catalyst for the oxidation of ethylene. This second component B of the catalyst is, in particular, the catalyst on the basis of molecular sieves or an oxidation catalyst containing palladium. Using this mixture of catalysts and the transmission of the original gaseous mixture consisting of ethane, oxygen, nitrogen and water vapor, through the reactor containing the catalyst, the maximum selectivity is 27% with a 7% conversion of ethane. High degree of conversion of ethane are obtained according to EP 0294845 only when the use is described of a mixture of catalysts and are not achieved when using the same catalyst containing components a and B.

Another way of obtaining producto ethylene and containing molecular oxygen gas lead at elevated temperature in contact with a catalytic composition, containing the elements A, X and Y. At this And indicates ModReeWf, X is Cr, Mn, Nb, TA, Ti, V and/or W and Y denotes Bi, CE, Co, cu, Fe, K, SB, Ni, P, Pb, Sb, Si, Sn, Tl and/or U. the Maximum selectivity that can be achieved using the described catalyst in the oxidation of ethane to acetic acid, is 78%. As byproducts carbon dioxide, carbon monoxide and ethylene.

None of the above publications, however, does not describe the use of a catalyst containing the elements palladium and molybdenum, for the selective oxidation of ethane and/or ethylene to acetic acid. In addition, known from the prior art selective oxidation to acetic acid achieved to date, is still unsatisfactory.

Therefore, the objective of the invention is to create a method that would allow simple, purposefully and with high selectivity at maximum mild reaction conditions to oxidize ethane and/or ethylene to acetic acid.

The problem is solved by the method of selective obtaining acetic acid from a gaseous feedstock containing ethane, or a mixture of ethane and ethylene, and oxygen, at high volume, obtained by mixing solutions of all of the catalytic elements, followed by drying and, if necessary, calcification, containing the elements Mo, Pd, X and Y in the gram-atom ratios a:b:C:d in combination with oxygen, the formula I

MoaPdbXcYd(I)

and X is one or more elements selected from the group:

Nb, Ti, V, or W;

Y represents one or more elements selected from the group of: B, Al, Bi, si, Ad, AI, K, Rb, Cs, SB, CA, Sr, Ba, Zr, Sb, and Sn; the indices a, b, C and d denote the gram-atom ratios of the respective elements, with and equal to 1, b is greater than 0, greater than 0 and d is 0 to 2, provided that the catalyst as X contains at least the elements of V and Nb, and that Mo and the elements of X are not based on the researched and that if one element Y Zr means, one element of X is W, and if one element of Y means Al, another element of Y means Sb.

It is desirable that X and Y had several elements, and the indices C and d for different optional elements take on different values, the temperature was in the range of 200 - 500oWith pressure in the range from 1 to 50 bar, b = 0,0001 0.5 in.

Preferably, the ethane was injected into the reactor in a mixture with at least another one is the catalyst contained, at least one of the following compositions in combination with oxygen:

Mo1,00Vof 0.25Nb0,12Pd0,0005< / BR>
Mo1,00Vof 0.25Nb0,12Pd0,0004< / BR>
Mo1,00Vof 0.25Nb0,12Pd0,0003< / BR>
Mo1,00Vof 0.25Nb0,36Sb0,01Ca0,01Pd0,0005< / BR>
Mo1,00Vof 0.25Nbfor 0.3Wof 0.2Pd0,0003< / BR>
Mo1,00Vof 0.25Nbfor 0.3Sba 0.1Pd0,0004,

moreover, the selectivity of the oxidation reaction to acetic acid of at least 60% conversion of ethane at least 4.

It is desirable that the catalyst was mixed with the material of the carrier or fixed on a material carrier.

The present invention also relates to a catalyst for selective oxidation of gaseous raw material obtained by mixing solutions of all of the catalytic elements, followed by drying and, if necessary, calcification, containing ethane and/or a mixture of ethane and ethylene, and oxygen, containing the elements Mo, Pd, X and Y in the gram-atom ratios a: b:c:d in combination with oxygen, the formula I

MoaPdbXcYd(I)

and X is one or more of the elements selected from the group of Nb, Ti, V, and W;

Y is one or neskolkomi ratio of the respective elements, and a = 1; b > 0; C > 0 and d = 0-2, provided that the catalyst as X contains at least the elements of V and Nb, and that the Mod and the elements of X are not based on the researched and that, if one element Y Zr means, one element of X is W, and if one element of Y means Al, another element of Y means Sb.

Examples of such preferred catalytic compositions used in the method according to the invention, include

Mo1,00Vof 0.25Nb0,12Pd0,0005< / BR>
Mo1,00Vof 0.25Nb0,12Pd0,0004< / BR>
Mo1,00Vof 0.25Nb0,12Pd0,0003< / BR>
Mo1,00Vof 0.25Nb0,36Sb0,01Ca0,01Pd0,0005< / BR>
Mo1,00Vof 0.25Nbfor 0.3Wof 0.2Pd0,0003< / BR>
Mo1,00Vof 0.25Nbfor 0.3Sba 0.1Pd0,0004.

Used according to the invention, the catalysts can be obtained in the usual way. With this purpose, prepare the initial suspension, in particular, an aqueous solution containing a separate source components elements according to their shares.

The starting materials of the individual components to obtain a catalyst according to the invention, includes, in addition to oxides, preferably, water-soluble substances such as Sona by heating into the corresponding oxides. For mixing the components to prepare aqueous solutions or suspensions of metal salts and mix them.

As starting compounds for molybdenum is recommended, due to their commercial availability, the corresponding molybdates, such as, for example, ammonium molybdate.

As the palladium compounds can be considered, for example, palladium(II) chloride, sulfate, palladium(II), terminated palladium(II) nitrate, palladium(II) and palladium acetylacetonate(II).

The reaction mixture is then stirred for from 5 min to 5 h at 50 - 100oC. Then remove the water and the remaining catalyst is dried at 50 to 150oWith, in particular at 80 - 120oC.

In the event of a subsequent calcination of the obtained catalyst, the process of calcination of the dried and turned into powder catalyst is recommended at 100 - 800oWith, in particular 200 - 500oWith the presence of nitrogen, oxygen or oxygen-containing gas. The duration of the process of calcification is 2 - 24 h

The catalyst can be used without a corresponding media or in a mixture with a carrier or supported on a carrier. Suitable are common carriers, the non-porous alumina, titanium dioxide, zirconium dioxide, thorium dioxide, lanthanum oxide, magnesium oxide, calcium oxide, barium oxide, tin oxide, cerium oxide, zinc oxide, boron oxide, boron nitride, boron carbide, boron phosphate, zirconium phosphate, aluminum silicate, silicon nitride or silicon carbide, but also glass, operadevelopment, metal oxide or metal mesh or appropriate monoliths.

Preferred carriers have a specific surface area less than 100 m2/, Preferred carriers are silica and alumina with a small specific surface area. The catalyst may be used after forming regular or irregular molded body or in powder form as a heterogeneous catalyst for the oxidation.

The reaction can be carried out in a fluidized bed or in a reactor with a fixed catalyst bed. For use in a fluidized bed, the catalyst was ground to a grain size in the range of 10 to 200 μm.

Containing molecular oxygen gas may be air or a gas containing molecular oxygen is greater than or less than air, such as oxygen. The proportion of water vapor can be in the range from 0 to 50% (vol.). Higher concentration which would further processing of the resulting aqueous solution of acetic acid. It is advisable to choose the ratio of ethane/ethylene to oxygen in the range from 1:1 to 10:1, preferably from 2:1 to 8:1. Preferred is a higher oxygen content, because it increases the achievable degree of conversion of ethane and thereby the yield of acetic acid. It is preferable to add oxygen or gas containing molecular oxygen, in concentrations outside the limit under the reaction conditions, as this simplifies the implementation of the method. However, it is also possible to set the ratio of ethane/ethylene to oxygen and within the limit.

The reaction can be carried out in a reactor with a fixed or fluidized bed of catalyst. Before the supply of oxygen or gas containing molecular oxygen, it is advisable to first mix ethane with inert gases such as nitrogen or water vapor. Before bringing the gas mixture into contact with a catalyst gas mixture is preferably heated in the heating zone to the reaction temperature. Acetic acid is separated from the flue gas by condensation. The remaining gases are then returned to the inlet of the reactor, which produces oxygen or containing molecular oxygen gas, and ethane and/or ethylene.

When compared the catalysts, according to the invention, allow, under the same reaction conditions (gas inlet to the reactor, pressure, residence time in the reactor), but at significantly lower temperatures, to achieve even higher selectivity for acetic acid (table 1; example 3 (invention): selectivity for acetic acid 77%; example 13 (EP-0407091): selectivity for acetic acid 60%). In comparison with the composition of the catalyst described in US-A-4250346, the selectivity of the reaction in acetic acid using a catalyst according to the invention, even at lower pressures and temperatures of reaction, and the smaller the times of stay in the reactor increases very strongly (cf. example 1 (invention): T= 250oC, p= 7 bar, the stay 14, the selectivity for acetic acid 84%; example 12 (US-A-4250346) T=280oC, p=15 bar, giving a residence time of 30 s, the selectivity for acetic acid 32%).

Using the catalysts according to the invention can be greatly increased the yield of product per unit volume per unit time (table 1). The output of product per unit volume per unit time characterizes the number of produced acetic acid per unit time per unit volume of catalyst. Higher output of product per unit of time e is When using the catalyst according to the invention, the selectivity is in the oxidation of ethane and/or ethylene to acetic acid of at least 60% (mol.), preferably at least 75% (mol.), in particular, at least 80% (mol.), so that the method according to the invention in comparison with prior art allows very simple to achieve higher outputs of acetic acid while reducing the amount of undesirable by-products.

Examples (see tab.1).

Given in the examples, the catalyst composition is specified in relative atomic ratios.

The preparation of the catalyst:

The catalyst (I):

There was obtained a catalyst of the following composition Mo1,00Vof 0.25Nb0,12Pd0,0005.

Solution 1:

10,22 g metavanadate of ammonia in 250 ml of water.

Solution 2:

61,75 g of ammonium molybdate and 0,039 g of palladium acetate in 200 ml of water.

Solution 3:

allocates 27,51 g of niobium oxalate in 25 ml of water.

The solutions are mixed separately with the 90oC for 15 minutes Then the third solution is added to the first. The combined mixture was stirred at 90oC for 15 min before added to them the second solution. The resulting mixture was stirred at 90oC for 15 minutes Then remove the water on the hot plate until you have a thick paste. The latter is dried over night at 120oC. Solid ve is giving 4 hours Thereafter, the catalyst was sieved to obtain the sieved fractions ranging in size from 0.35 to 1 mm

The catalyst (II):

There was obtained a catalyst of the following composition: Mo1,00Vof 0.25Nb0,12Pd0,0004.

The catalyst (II) are obtained as described in example 1, a catalyst, except that instead 0,039 g of palladium acetate is used 0,031,

The catalyst (III):

There was obtained a catalyst of the following composition:

Mo1,00V0,36Nb0,03Sb0,01Ca0,01Pd0,0005.

Solution 1:

to 20.0 g of ammonium molybdate in 100 ml of water.

Solution 2:

4.8 g of metavanadate of ammonia in 100 ml of water.

Solution 3:

2.6 g of niobium oxalate, of 0.48 g of antimony oxalate, 0.34 g of calcium nitrate in 50 ml of water.

Solution 4:

0,013 g of palladium acetate in 50 ml of acetone.

Solutions 1-3 mix each separately at 70oC for 15 minutes Then the third solution is added to the second. The combined mixture was stirred at 70oC for 15 min before being added to the first solution. After this, added to them the fourth solution. The resulting mixture was stirred at 70oC for 15 minutes Then quickly evaporated water acetone CME is (sieved fraction: 0,35-2 mm) and then calicivirus in still air at 300oC for 5 hours then the catalyst was sieved to obtain the sieved fractions of size 0,35 - 0,7 mm

The catalyst IIIa (the catalyst on the carrier):

There was obtained a catalyst of the following composition:

Mo1,00V0,36Nb0,03Sb0,01CA0,01Pd0,0005/Al2O3< / BR>
Solution 1:

to 20.0 g of ammonium molybdate in 100 ml of water.

Solution 2:

4.8 g of metavanadate of ammonia in 100 ml of water.

Solution 3:

2.6 niobium oxalate, of 0.48 g of antimony oxalate, 0.34 g of calcium nitrate in 50 ml of water.

Solution 4:

0,013 g of palladium acetate in 50 ml of acetone.

Material media:

-Al2O3, SA 5205 (company Norton): specific surface area of 0.08 m2/g; average pore diameter of 130 μm, water absorption 25%; shape - balls.

Solutions 1 to 3 are mixed separately at 70oC for 15 minutes Then the third solution is added to the second. The combined mixture was stirred at 70oC for 15 min, then added to the first solution. Then add to them the fourth solution. The resulting mixture was stirred at 70oC for 15 min 475 g of material media crush (sieved fraction of 0.7-1.5 mm) and then adds the obtained granules. Then quickly evaporated water-acetone mixture until you have a thick paste. The latter is dried over night at 120oC. the Solid is crushed (sieved fraction: 0,35-2 mm) and then calicivirus in still air at 300oC for 5 hours then the catalyst was sieved to obtain the sieved fractions of size 0,35 - 0,7 mm

The catalyst IIIB (the catalyst on the carrier):

A catalyst having the composition of the catalyst IIIa, was obtained as follows.

Similarly, to obtain a catalyst IIIa receive a mixture of solutions of 1-4. The resulting mixture was stirred at 70oC for 15 minutes At 475 g of spherical media (-Al2ABOUT3, SA 5205, firm Norton) pour the heated mixture of solutions 1 to 4 and the resulting mixture was stirred at 70oC for 15 minutes Then evaporated water-acetone mixture. The thus obtained solid substance is dried and calicivirus similar to obtaining a catalyst IIIa.

The catalyst V (the catalyst on the carrier):

A catalyst having the composition of the catalyst IIIa, was obtained as follows.

Similarly, to obtain a catalyst IIIa receive a mixture of solutions of 1-4. Spherical media (-Al2ABOUT3ptx2">

Comparative examples

The catalyst (IV):

For comparison get a catalyst in accordance with US-A-4250346 of the following composition:

Mo1,00Vof 0.25Nb0,12.

The catalyst (IV) are obtained as described in example (1) on catalyst, except that no use of palladium acetate.

The catalyst (V):

For comparison, get the catalyst according to EP-0407091 of the following composition:

Mo0,370Re0,248V0,259Nb0,070Sb0,030Ca0,019.

Solution 1:

10.0 g of ammonium perrhenate and 9.7 g of ammonium molybdate in 50 ml of water.

Solution 2:

4.5 g of metavanadate of ammonia in 50 ml of water.

Solution 3:

6.5 g of niobium oxalate, of 1.34 g of antimony oxalate, of 0.58 g of calcium nitrate in 180 ml of water.

The solutions are mixed separately at 70oC for 15 minutes Then the third solution is added to the second. The combined mixture was stirred at 70oC for 15 min before being added to the first solution. The resulting mixture was stirred at 70oC for 15 minutes Then remove the water on the hot plate until you have a thick paste. The latter is dried over night at 120oC. the Solid is crushed (sifted PR sieved to obtain sieved fractions ranging in size from 0.35 to 1 mm

Test method for catalyst

10 ml of the catalyst was loaded into a steel reactor with an internal diameter of 10 mm, the Catalyst is heated under an air flow of up to 250oC. Then install the pressure control source pressure. A mixture of ethane: oxygen: nitrogen composition served with water in evaporative zone, where the evaporation of water and its mixing with gases. The reaction temperature is measured with a thermocouple in the loose mass of catalyst. The reaction gas is analyzed in gas chromatography on-line.

In the examples, the following terms are defined as:

The conversion of ethane (%)=100x([WITH]/2+[CO2]/2+[P2H4]+ [SN3COOH]/([CO] /2+[CO2]/2+[P2H4]+[C2H6]+[SN3COOH]).

The selectivity to ethylene (%)= 100x([C2H4] )/([WITH] /2+[CO2] /2+[P2H4]+ [SN3COOH]).

Selectivity for acetic acid (%)=100x([CH3COOH])/([WITH]/2+ [CO2] /2+[P2H4]+[SN3COOH])

where [] denotes concentration in % (mol.) and

[C2H6] denotes the concentration of unreacted ethane.

A stay is defined as:

(s)=bulk volume of the catalyst (m is BR> The gas inlet to the reactor consists of 40%(vol.) ethane, 8%(vol.) oxygen, 32%(about. ) nitrogen and 20%(about. ) water vapor. Reaction conditions and results are presented in table 1.

In comparison with the comparative catalysts (IV) and (V) catalysts (I), (II) and (III) allow to achieve at lower temperatures and pressures of the reaction, significantly higher values of selectivity for acetic acid. Catalysts I Mo1,00Vof 0.25Nb0,12Pd0,0005), II Mo1,00Vof 0.25Nb0,12Pd0,0004and Mo1,00V0,36Nb0,03Sb0,01Ca0,01Pd0,0005show in comparison with the catalysts IV Mo1,00Vof 0.25Nb0,12= US-A-4250346) and V Mo1,00Re0,67V0,70Nb0,19Sb0,08Ca0,05= EP-0407091) higher output per unit volume per unit time.

Comparative experiments on thermal stability of the catalyst

For radiation heat resistance of the catalyst charged to the reactor, the catalysts (I) and (V) and work with them for 100 h (reaction conditions: 280oC, 15 bar, giving a residence time of 30 s, the composition of the reaction gas: see above). By the end of the exhaust cycle of the selected sample with the input side of the filled catalyst layer and quantitatively analyze the composition of the catalyst. In the already over 100 hours of work will lose 44.4% of primary rhenium. On the contrary, the fresh and used catalyst (I) has the same composition.

1. Method for selective receipt of acetic acid from a gaseous feedstock containing ethane, or a mixture of ethane and ethylene, and oxygen, at elevated temperature, characterized in that the gaseous feedstock is brought into contact with a catalyst obtained by mixing solutions of all of the catalytic elements, followed by drying and, if necessary, calcification, containing the elements Mo, Pd, X and Y in the gram-atom ratios a:b:c:d in combination with oxygen

MoaPdbXcYd(I)

and X is one or more of the elements selected from the group of Nb, Ti, V, or W;

Y is one or more of the elements selected from the group of Al, Bi, cu, Ag, AI, K, Rb, Cs, Mg, Ca, Sr, Ba, Zr, Sb and Sn;

the indices a, b, C and d denote the gram-atom ratios of the respective elements, where a= 1; b>0; C>0 and d=0-2, provided that the catalyst as X contains at least the elements of V and Nb, and that the Mod and the elements of X are not based on heteropolyacids, and that if one element Y Zr means, one element of X is W, and if one element of Y means A1, another element of Y means Sb.

2. The method according to p. 1, featuring imaut different values.

3. The method according to p. 1 or 2, characterized in that the temperature is in the range 200 - 500oC.

4. The method according to one of paragraphs.1-3, characterized in that the pressure in the reactor is in the range from 1 to 50 bar.

5. The method according to one of paragraphs.1-4, characterized in that b = is 0.0001 to 0.5.

6. The method according to one of paragraphs.1-5, characterized in that the ethane is introduced into the reactor in a mixture with at least one gas.

7. The method according to p. 6, characterized in that as another gas is injected nitrogen, oxygen, methane, carbon monoxide, carbon dioxide, ethylene and/or water vapor.

8. The method according to one of paragraphs.1-7, characterized in that the catalyst contains at least one of the following compositions in combination with oxygen:

Mo1,00Vof 0.25Nb0,12Pd0,0005;

Mo1,00Vof 0.25Nb0,12Pd0,0004;

Mo1,00Vof 0.25Nb0,12Pd0,0003;

Mo1,00V0,36Nb0,03Sb0,01Ca0,01Pd0,0005;

Mo1,00Vof 0.25Nbfor 0.3Wof 0.2Pd0,0003;

Mo1,00Vof 0.25Nbfor 0.3Sba 0.1Pd0,0004,

moreover, the selectivity of the oxidation reaction to acetic acid is not less than 60% conversion of ethane at least 4%.

9. The method according to one La.

10. Catalyst for selective oxidation of gaseous raw material obtained by mixing solutions of all of the catalytic elements, followed by drying and, if necessary, calcification, containing ethane, or a mixture of ethane and ethylene, and oxygen, containing the elements Mo, Pd, X and Y in the gram-atom ratios a:b:c:d in combination with oxygen

MoaPdbXcYd(I)

and X is one or more of the elements selected from the group of Nb, Ti, V, or W;

Y is one or more of the elements selected from the group of Al, Bi, Cu, Ag, Au, K, Rb, Cs, Mg, Ca, Sr, Ba, Zr, Sb and Sn;

the indices a, b, c, d denote the gram-atom ratios of the respective elements, where a=1; b>0; C>0 and d=0-2, provided that the catalyst as X contains at least the elements of V and Nb, and that the Mod and the elements of X are not based on heteropolyacids, and that if one element Y Zr means, one element of X is W, and if one element of Y means Al, another element of Y means Sb.

 

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