Synthesis gas generation process via palladium-rhenium membrane-assisted steam reforming of dimethyl ether

FIELD: industrial organic synthesis.

SUBSTANCE: synthesis gas, which is various-destination product, is generated in reactor with palladium-rhenium membrane at dimethyl ether-to-water ratio 1:1, elevated temperature, atmospheric pressure, and reactants supply speed 60 to 1200 h-1. Process allows achieving essentially complete conversion of dimethyl ether without any increase in pressure and at lower temperature, whereas resulting gas mixture contains no unreacted water steam, nitrogen, and carbon dioxide.

EFFECT: enhanced process efficiency.

4 tbl, 4 ex

 

The invention relates to chemical industry and associated with obtaining synthesis gas in the process of steam reforming of dimethyl ether (DME), while using palladium-rhenium membrane to shift the equilibrium towards the formation of target products by removing one of the products (hydrogen) from the sphere of reaction.

Description of the invention

The invention relates to the chemical industry, for the generation of synthesis gas by steam reforming of dimethyl ether.

Synthesis gas is the most promising raw material source alternative to oil. An important advantage of the processes on the basis of the synthesis gas is that synthesis gas can be easily processed into methanol, which is a multi-purpose semi-product on the basis of which can be obtained valuable chemical products, such as acetic acid, ethylene glycol, high molecular weight hydrocarbons, alcohols or aldehydes. In addition, from synthesis gas using the traditional process of Fischer-Tropsch get lower olefins, alcohols and components of motor fuels. For production of methanol and Fischer-Tropsch synthesis the most favorable ratio in the synthesis gas WITH:N2=1:2.

The synthesis gas at the present time are mainly or gasification of solid fuels, or the conversion of natural gas. From the local methods of synthesis gas production from methane by means of water vapor (1300-1400° C η=90%) or by incomplete combustion of the Nickel catalyst (900-1000°). There are also a number of ways to produce synthesis gas from the DME [2].

Closest to the proposed method for production of synthesis gas is the way [3].

The disadvantages of this method are the need for high pressure, high temperature process, the need for air supply and a large ratio of water/DME, which leads to high concentrations in the target product, unreacted water vapor, nitrogen and carbon dioxide and requires further separation of the resulting mixture of products.

To address these shortcomings we propose a method of generating synthesis gas, characterized in that the steam reforming carried out on the catalysts in the presence of palladium-rhenium membrane at a temperature of 300 to 400°C, atmospheric pressure and feed rate of the reactants 60-1200 h-1.

Example 1.

The catalyst for steam reforming of dimethyl ether in the amount of 4.5 g containing 0.25% Pd, the rest of the media γ-Al2About3experience in a reactor equipped with a palladium membrane at temperatures 200-450°and atmospheric pressure with a flow of reactants into the reactor at a volumetric rate of 120 h-1in a molar ratio of dimethyl ether:N2O=1:1. Passed through the membrane, the hydrogen was evacuated by the vacuum. The results enumerated in m is l/1 mol supplied DME, shown in table 1.

Example 2.

The process was performed under conditions identical to example 1, but without a membrane reactor.

Table 1

The influence of palladium-rhenium membrane steam reforming of DME
ExampleTemperature, °C; pressure, ATMExit mol/1 mol of dimethyl etherConversion of DME, %
H2COCO2CH4
1300; 11,7441,2850,0290,02566,9
2300; 11,4270,8200,0150,110to 47.2

As can be seen from examples 1 and 2, the use of palladium membranes for removal of formed hydrogen from the scope of the reaction to shift the equilibrium reaction of steam reforming of dimethyl ether

CH3Och3+H2O↔2SD+4H2

towards the education of target products: their output increased 1.2-1.6 times, 42%, increases the degree of conversion of dimethyl ether, moreover, is greatly reduced content of by-product methane 77.3%.

Table 2

Usl is via conduction and composition of the products of the synthesis gas production prototype.
Pressure, ATMTemperature, °The composition of the gas mixture, %
H2H2AboutN2COCO2ArMeon
33350-45039,5831,3413,160,5215,210,160,03
39270-35032,7843,0510,970,4912,560,130,01

The comparison of the obtained results with the data of the prototype (table 2) shows that almost complete conversion of DME is achieved without increasing pressure and at a lower temperature using to shift the equilibrium towards the formation of target products palladium membrane and catalyst. In addition, the resulting gas mixture does not contain impurities that are made when using under the conditions of the prototype air as one of the reactants.

Example 3.

The process is conducted under conditions identical to example 1 in a reactor equipped with a palladium membrane. To select the optimal conditions of steam reforming of dimethyl ether using such a reactor is considered the influence of the molar relationship of H2A:the DOE catalyst composition of 0.25% Pd/γ -Al2About3. The composition of the products of steam reforming of DME are presented in table 3 mol/1 mol of dimethyl ether.

0,046
Table 3

The influence of the molar ratio of N2O:DME on the composition of the products of steam reforming of dimethyl ether
T °CO2H2COCH4DMEConversion of DME, %H2/CO
H2O/DME=1:1
2000,002to 0.0600,0340,0040,9802,01,8
2500,0050,1700,1690,0160,9059,51,0
3000,0151,4270,8200,1100,528to 47.21,7
3500,0632,3721,4140,2400,14285,81,7
4000,1802,1111,1820,4130,11388,71,8
4500,4402,0620,9720,4640,062 93,82,1
H2O/DME=2:1
2000,0010,0170,0000,0000,9990,1-
2500,011rate 0.1620,0230,0000,9831,77,1
3000,0191,0350,1210,0180,9217,98,5
3500,0181,0441,2530,1810,27472,60,8
4000,0341,2721,5250,2980,07192,90,8
4500,1501,1551,3230,406to 0.06094,00,9
H2O/DME=3:1
2000,0040,0220,0000,000is 0.9980,2-
2500,0060,0670,3280,0190,82417,60,2
3000,0120,8541,0550,44355,70,8
3500,0641,4881,6670,1230,073of 92.70,9
4000,1191,5101,5180,2890,03796,31,0
4500,3411,4161,2750,3560,01498,61,1

As can be seen from the table, when the molar ratio of N2O:DME=1:1 increase in process temperature from 300 to 400°With conversion of DME increases from 47.2 percent to 88.7 per cent, while the ratio of N2/CO in the produced synthesis gas is 1.7 to 1.8.

The increase in the supply stream molar relationship of H2O:DME to 2:1 leads to the fact that a significant conversion of DME is observed only at temperatures 350° (72.6%) and with increasing temperature up to 450°C, the conversion rate increases to 94%, but the ratio of N2:Becomes close to 1.

Further increase in the ratio of N2O:DME=3:1, leads to an increased CO2in the reaction products. According to equation three mole pair (H2On) required for the complete conversion of DME to carbon dioxide and hydrogen:

CH3Och3+3H2O=3H2+2SD2

Therefore, to increase the receiving water vapour in the reagents in the steam reforming of DME increases the tendency of formation of CO 2and H2in comparison with the formation of synthesis gas. Based on the data presented in table 3, the molar ratio of N2About:DME=1:1 is preferred for the formation of synthesis gas using a reactor with a palladium membrane.

Example 4.

The process is conducted under conditions identical to example 1 in a reactor equipped with a palladium membrane. To select the optimal conditions of steam reforming of dimethyl ether using such a reactor was studied the influence of the flow rate of the raw flow and molar ratio H2O:DME. The results are presented in table 4.

Table 4

The effect of the space velocity of the reactants on a steam reforming DME
Space velocity, h-1T °Exit mol/1 mol of dimethyl ether
CO2H2COCH4DMEConversion of DME, %H2/CO
60300being 0.0361,9431,1090,1930,33166,91,8
3500,1132,526at 1.5210,3180,0249,6 1,7
4000,3302,0911,1000,5010,03596,51,9
1203000,0151,4270,8200,1100,528to 47.21,7
3500,0632,3721,4140,2400,14285,81,7
4000,1802,1111,1820,1430,11388,71,8
3003000,0151,1050,6600,0490,63836,21,7
3500,0292,7461,5820,1420,12387,71,7
4000,1292,8141,5390,2140,05994,11,8
6003000,0030,5260,305being 0.0360,82817,21,7
3500,0131,7821,0320,1610,3971,7
4000,0332,4291,393rate 0.1620,20679,41,7
12003000,0020,2800,1540,0040,92081,8
3500,0080,9520,6100,0370,72281,6
4000,0262,2381,416of 0.1820,18881,21,6

From the data of example 4 shown in table 4, it is seen that the increase in the rate of flow of the reactants through the reactor shifts the maximum growth conversion of dimethyl ether in the high temperature region and affects the ratio of N2/WITH. At low feed rate of the reactants 60 h-1there is a high content of by-products: methane and CO2therefore , further reduction of the feed rate of the reactants is impractical. Increasing the feed rate of the reactants above 1200 h-1it is also impractical because of the shift of the maximum growth the conversion of DME in the area of higher temperatures and lower ratio of N2:WITH up to 1.6.

From the data presented in tables 3 and 4, it follows that the steam reforming of dimethyl ether to be used is of the palladium membrane for the selective synthesis gas production is preferably carried out at a molar ratio of the reactants in the feed stream N 2About:DME=1:1 and flow rate of feed Vo=120 h-1at a temperature of 300-350°C.

Sources of information

1. Shinada So, Ohno F., Ogawa b, It M, Mizuguchi M, Tomur K., Fujimoto K.//Kinetics and catalysis. - 1999, C. No. 3. - s-446.

2. U.S. Pat. No. 4356354. 1988.

3. EP 0931762 A1.

Method for production of synthesis gas steam reforming of dimethyl ether (DME) at elevated temperature and atmospheric pressure over the catalyst at a molar ratio of reagents DME:N2O=1:1, characterized in that the steam reforming is carried out in a reactor equipped with a palladium-rhenium membrane at a feed rate of the reactants 60-1200 h-1.



 

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21 cl, 2 dwg, 1 tbl, 9 ex

FIELD: chemical industry; methods of production of hydrogen.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to production of hydrogen. The method of start up of the evaporation installation for formation of the hydrocarbon-air mixture decomposed in the reformer for production of hydrogen contains the combustion/mixing chamber, in which through a device with inlet openings the air is fed; the porous evaporating medium and the first heating device added to it; the tool of a surface ignition for inflaming of hydrocarbon-air mixture present in the combustion/mixing chamber. The method includes the following stages: a) heating and evaporation of the liquid hydrocarbon or the hydrocarbon-containing liquids; b) mixing of the vapor produced at the b) stage with the air; c)inflaming of the mixture produced at the b)stage for starting up of a combustion procedure of the mixture; d)keeping up of the combustion procedure up to the end of the given duration of time and-or until the given temperature will be reached in one or several given zones of the installation; e) the termination of the combustion process after the given duration of time and-or after reaching the given temperature. The invention ensures an increase of efficiency of the process due to the temperature drop in the zone of the catalytic reaction.

EFFECT: the invention ensures an increase of efficiency of the process due to the temperature drop in the zone of the catalytic reaction.

7 cl, 2 dwg

FIELD: hydrocarbon conversion catalysts.

SUBSTANCE: catalyst for generation of synthesis gas via catalytic conversion of hydrocarbons is a complex composite composed of ceramic matrix and, dispersed throughout the matrix, coarse particles of a material and their aggregates in amounts from 0.5 to 70% by weight. Catalyst comprises system of parallel and/or crossing channels. Dispersed material is selected from rare-earth and transition metal oxides, and mixtures thereof, metals and alloys thereof, period 4 metal carbides, and mixtures thereof, which differ from the matrix in what concerns both composition and structure. Preparation procedure comprises providing homogenous mass containing caking-able ceramic matrix material and material to be dispersed, appropriately shaping the mass, and heat treatment. Material to be dispersed are powders containing metallic aluminum. Homogenous mass is used for impregnation of fibrous and/or woven materials forming on caking system of parallel and/or perpendicularly crossing channels. Before heat treatment, shaped mass is preliminarily treated under hydrothermal conditions.

EFFECT: increased resistance of catalyst to thermal impacts with sufficiently high specific surface and activity retained.

4 cl, 1 tbl, 8 ex

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