Zeolite catalyst, method of its production and method of methane nonoxidising conversion

FIELD: process engineering.

SUBSTANCE: invention relates to petrochemical and chemical industries, particularly, to production of methane conversion catalyst, method of its production and method of converting methane into aromatic hydrocarbons in nonoxidising conditions. Zeolite catalyst comprises molybdenum in amount of not over 4.0 % by wt as modifying element, carbamide as structure-forming additive, and nano-sized silver powder as second modifying element, said silver powder produced by conductor electrical blasting, at concentration varying from 0.1 to 2.0 wt %. Proposed method allows producing catalyst by dry mixing of zeolite modified by molybdenum with molybdenum content not exceeding 4.0 wt % with second promoting agent, i.e. nano-sized silver powder with its content in produced catalyst varying from 0.1 to 2.0 wt %. Method of methane nonoxidising conversion is performed in the presence of above described catalyst.

EFFECT: higher degree of methane conversion and yield of aromatic hydrocarbons along with catalyst longer life.

3 cl, 1 tbl, 8 ex

 

The invention relates to the petrochemical and chemical industries, in particular to the creation of a catalyst for conversion of methane, the method thereof and method for converting methane to aromatic hydrocarbons in a non-oxidizing conditions.

It is known that to improve time stable high action of zeolites of type ZSM-5 containing molybdenum, during non-oxidative methane conversion using additives such promoters as Fe, Cr, Ga [Dong Qun, Ichkawa M. Catalytic features of systems of Mo/HZSM-5 promoted additives of the second metal in the aromatization of methane // Fenzi cuihua = J.Mol.Catal. (China). - 2001. - Vol.15. No. 1. - 33-36] and [Tian Bing-Iun, Lui Hong-mei, Shu Yu-ying, Wang Lin-sheng, Xu Yi-de. Dehydroaromatization methane in the absence of oxygen in the presence of the modified cobalt catalysts of Mo/ZSM-5 // Fenzi cuihua = J.Mol.Catal.(China). 2000. - Vol.14. No. 3.-200-204].

Closest to the proposed catalyst for the way you cook and the way non-oxidative methane conversion is the technical solution according to the patent (Patent RF №2296009). The catalyst comprises molybdenum and the second modifying element is Nickel, the content of molybdenum in the catalyst is not more than 4.0 wt.% and Nickel from 0.1 to 0.5 wt.%. The method of producing the catalyst is in a dry mechanical mixture of zeolite ZSM-5 in the protonated form and nanosized powders (APCS) Mo and Ni obtained by electrical explosion of conductors metals in an argon atmosphere, followed by annealing the prepared mixture at a temperature of 500°C for 4 h The way non-oxidative methane conversion is carried out in the presence of the above catalyst.

The disadvantages of the known solutions are the low catalytic activity of the catalyst and the little time it stable steps.

Object of the present invention to provide a catalyst that increases the degree of conversion of methane and yield of aromatic hydrocarbons, as well as increasing the time a stable action of the catalyst.

The technical result is achieved in that the zeolite catalyst process for non-oxidative conversion of methane contains structure-forming additive is urea, includes as a modifying element molybdenum and the second modifying element nano-sized powder of silver, obtained by electrical explosion of wire, at a concentration of from 0.1 to 2.0 wt.%.

The method of preparation of the zeolite catalyst process for non-oxidative methane conversion includes the introduction of structuring additive is urea and the modification of the zeolite with molybdenum, followed by annealing and by adding a second promoting element is silver, which is administered in the form of nanosized powder dry mixing of reagents, and the silver content is from 0.1 to 2.0 wt.%.

The way non-oxidative methane conversion is carried out in the presence of razlagaemogo zeolite catalyst.

Zeolite ZSM-5 with a molar ratio of SiO2/Al2O3= 50, used to prepare the catalytic system Ag-Mo/ZSM-5, get with urea (urea) as a structure-forming additives. The catalyst Mo/ZSM-5 obtained by dry mechanical mixing of zeolite ZSM-5 in the protonated form and nanopowder Mo obtained by electrical explosion of wire metal in an argon atmosphere, followed by annealing the prepared mixture at 500°C for 4 h Catalysts Ag-Mo/ZSM-5 obtained by dry mechanical mixing of the prepared sample Mo/ZSM-5 and Ag nanopowder obtained by electrical explosion of wire metal in argon, without subsequent annealing of the catalytic system. The result catalysts Ag-Mo/ZSM-5, containing not more than 4.0 wt.% PPR Mo and not less than 0.1 wt.% APC Ag. Catalytic activity and stability of the prepared catalysts is higher than that of catalysts prepared by mechanical mixing of zeolite ZSM-5 with PPR Mo and modified with Ni nanopowder under the same process conditions.

Catalytic testing of the samples is carried out in a flow setting at a temperature of 700-750°C, space velocity of methane 800-1000 h-1and atmospheric pressure. The catalyst in the amount of 1 ml was placed in a quartz tubular reactor with a diameter of 12 mm Before the beginning of the process the catalyst naked is ewout in a stream of helium up to 700-750°C and maintained at the reaction temperature for 20 min, then, the reactor serves methane, the degree of purity is 99.9%. The reaction products and not converted methane come in castigados tap for sampling gas chromatography analysis. To prevent condensation or solid adsorption forming higher hydrocarbons tube at the exit of the reactor and castigados crane thermostatized at a temperature of 220°C. Analysis of the products of the methane conversion is carried out after 20 min of reaction, and then every 60 min of operation catalyst. The results are presented in the table.

Examples of specific performance.

Example 1. To 4.0 g decationizing zeolite ZSM-5 (molar ratio SiO2/Al2O3= 50), synthesized using urea, added 0.16 g PPR Mo (4.0 wt%), obtained by the method of electric explosion of molybdenum wire. The mixture is stirred in a vibratory mill for 0.5 h and calcined at 500°C for 4 h To the received sample Mo/ZSM-5 type of 0.004 g Ag APC (0.1 wt.%) and mixed in a vibratory mill for 0.5 h the mixture after the introduction of APCS Ag in the catalyst is not calcined. Then the prepared catalyst was pressed into tablets, cut up and taken away for research fraction of 0.5-1.0 mm

The conversion of methane at a temperature of 750°C and flow rate of feed 1000 h-1after 60 min of operation of the catalyst the leaves of 22.3%. Research of influence of duration of reaction on the catalyst activity show that the conversion of over 480 min of operation of the catalyst is reduced by 1.2%.

Example 2. In the same way as in example 1, but the content APC Ag is 0.5% by weight of the zeolite. Methane conversion at 750°C and 1000 h-118.8% after 60 min of operation of the catalyst and reduced to 10.0% for a reaction time of 480 minutes

Example 3. In the same way as in example 1, but the content APC Ag is 1.0% by weight of the zeolite. Methane conversion at 750°C and 1000 h-1contributes 17.4% after 60 min of operation of the catalyst and reduced to 8.0% for a reaction time of 480 minutes

Example 4. In the same way as in example 1, but the content APC Ag is 2.0% by weight of the zeolite. Methane conversion at 750°C and 1000 h-1is 16.5% after 60 min of operation of the catalyst and decreases to 6.5% for a reaction time of 480 minutes

Example 5. In the same way as in example 1, but the sample of Mo/ZSM-5 does not contain APCS Ag. Methane conversion at 750°C and 1000 h-1is 16,0% after 60 min of operation of the catalyst and decreases to 5.6% for a reaction time of 480 minutes

Example 6. In the same way as in example 1, but the temperature of the process of methane conversion is 700°C. the Conversion of methane at 1000 h-1is 15.1% after 60 min of operation of the catalyst and increases to 16.4% for a reaction time of 480 minutes

Example 7. In the same way as in example 6, but the volumetric flow rate of methane is 800 h-1. Env is rsia methane at 700°C is 14.4% after 60 min of operation of the catalyst and increases to 15.5% for a reaction time of 480 minutes

Example 8. In the same way as in example 1, but the volumetric flow rate of methane is 800 h-1. Methane conversion at 750°C amounted to 20.9% after 60 min of operation of the catalyst and reduced to 20.2% for a reaction time of 480 minutes

The table shows the comparative characteristics of catalytic activity and stability samples Ag-Mo/ZSM-5 obtained by modification of ZSM-5 nanopowders Mo and Ag and catalyst Ni-Mo/ZSM-5 obtained by modification of ZSM-5 nanopowders Mo and Ni (the prototype).

Thus, the proposed method allows to obtain a catalyst that is different from the prototype of the higher activity and stability in the process of conversion of methane into aromatic hydrocarbons.

Table
Comparative characteristic activity of modified zeolite catalysts
IndicatorsThe proposed methodPrototype
1234567 8
Temperature, °C750750750750750700700750750
Space velocity, h-11000100010001000100010008008001000
Conversion for a reaction time of 60 min, %22,318,817,416,516,015,114.4V20,913,6
Output arenes %17,815,013,913,112,812,111,416,810,7
Behold aktivnosti on arenas, %79,879,879,979,480,080,179,280,478,7
Conversion for reaction time 480 min, %21.110,08,06,55,616,415,520,28,4
The ratio of Ag(Ni)/Mo in the catalyst0,040,120,250,50-0,040,040,040,04

1. The zeolite catalyst process for non-oxidative methane conversion, including as a modifying element molybdenum in an amount of not more than 4.0 wt.% and second, the modifying element, characterized in that the catalyst contains structure-forming additive is urea, and the second modifying element contains nano-sized powder of silver, received the ing electric explosion of the conductor, at a concentration of from 0.1 to 2.0 wt.%.

2. The method of preparation of the zeolite catalyst process for non-oxidative methane conversion, including the modification of the zeolite with molybdenum in an amount of not more than 4.0 wt.% with subsequent annealing and adding a second promoting element, characterized in that the injected structuring additive is urea, and the second the promoting element - silver impose a nanoscale powder dry mixing of reagents, and the silver content is from 0.1 to 2.0 wt.%.

3. The way non-oxidative methane conversion in the presence of a zeolite catalyst, characterized in that the use of the catalyst according to claim 1.



 

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