Method of catalytic pyrolysis of methylene chloride

FIELD: chemistry.

SUBSTANCE: pyrolysis of methylene chloride is carried out on a catalyst with a carbonisation degree in the range of 2.6-5.2 wt %, which is obtained during 60-150 minutes of a reactor work, after which in order to support the obtained degree of carbonisation a catalyst is constantly discharged into a regenerator, excessive carbon is removed by burning with air at a temperature of 550°C. After that it is returned into the reactor, providing constant circulation of the carbonised catalyst from the reactor of pyrolysis into the regenerator and back.

EFFECT: application of the method makes it possible to increase selectivity of the process of obtaining lower olefins due to increase of the catalyst selectivity, applied in the process of methylene chloride pyrolysis.

2 ex, 2 tbl

 

The invention relates to a method of catalytic pyrolysis of methyl chloride, which is one of the main stages of obtaining lower olefins in the process of catalytic conversion of methane from natural gas through the intermediate synthesis of methyl chloride oxidative chlorination of methane.

Known way catalytic dehydrochlorination methyl chloride using silica fiberglass catalyst. The catalyst is characterized in the IR spectra of adsorbed ammonia in the presence of absorption bands with wave numbers in the range ν=1410-1440 cm-1contains the active ingredient and vysokoglinozemistyj media (EN 2333192, C07C 11/02, publ. 10.08.2009). With the addition of Cu, Zn, Ag catalyst provides high selectivity for ethylene, but has a very low conversion of methyl chloride 10-25%.

The pyrolysis of methyl chloride on silicoaluminate catalyst SAPO-34 at a temperature of 400-500°C is used as one of the stages of catalytic method for processing methane (EN 2394805, C07C 17/154, publ. 20.07.2010), in which the first stage receive methylene chloride oxychloination methane. In this process we get together with chloride stands methylene chloride and chloroform are not separated from the methyl chloride, and go into the pyrolysis reactor, which leads to a significant superusuario ka is alistor.

In the patent (RU 2451005, C07C 17/154, publ. 20.05.2012) proposed an improvement of the above process by separating from of methyl chloride methylene chloride and chloroform and hydrodechlorination to methyl chloride and methane, which are optional amount of ethylene and propylene. Due to the exclusion of the initial mixture of pyrolysis of methylene chloride and chloroform nauglerozhivaniya catalyst SAPO-34 is reduced to 18 times, however, the influence of supervivencia on the activity and selectivity of the catalyst is not considered.

There is a method of catalytic pyrolysis of methyl chloride using silicoaluminate catalyst (US 20080188701 A1) obtaining light olefins (ethylene and propylene), including the state of contact of the raw materials containing monohalogenated (all examples in methylene chloride), catalyst (various SAPO and metal substituted version of them) at temperatures from 350 to 600°C, a pressure of 0.05-1.1 MPa, the weight of the feed rate of the raw material is 0.1 to 100 h-1and the extraction of ethylene and propylene and galgenwaard (hydrogen chloride) from the reaction gas.

In the description of the examples, the highest total selectivity for ethylene and propylene 82,72% achieved in the process of pyrolysis of methyl chloride on the catalyst containing 50% SAPO-34 and 50% of alumina as a binder at a temperature of 450°C, the atmosphere is nom pressure, weight rate 1 h-1and the dilution of methyl chloride with water vapor in the ratio of 10:1.

The pressure increase, a decrease or increase in flow rate, and the use of other catalysts are not allowed to increase the yield of light olefins. A small increase in total selectivity to ethylene and propylene to 84,35 and 83,99% was achieved only when it is used as solvent of methanol and isopropanol. However, these substances are not just diluents, as they have in their pyrolysis to form light olefins, and the selectivity. The duration of the run was 1 hour, so how does the duration of operation of the catalyst on the performance of the process is unknown. It is also unknown what effect the regeneration of the catalyst in the subsequent pyrolysis of methyl chloride. Reported only that the regeneration was carried out oxygen-containing gas outside the reactor of pyrolysis.

It should be noted that the use of this method as a diluent is methyl chloride vapor is unacceptable for industrial environments because of severe corrosion of the equipment produced hydrochloric acid.

The disadvantage of this method is the low total selectivity to ethylene and propylene, despite the use of diluents. In addition, the use razbaby the oil reduces the performance of the equipment and worsens the conditions of selection of target products.

A method of obtaining lower olefins (mainly ethylene and propylene) catalytic pyrolysis of methanol on silicoaluminate catalyst (SAPO)in which to save the activity of the catalyst serves to mix the regenerated catalyst with a catalyst containing on their surface a coke. From literature it is known that the pyrolysis of methanol and methyl chloride is carried out on the same catalysts in the same conditions and with similar indicators of the processes that allows you to choose described in this patent a method of catalytic pyrolysis of methanol in the process of obtaining lower olefins for the prototype (US 7,033,971, CL C07C 1/00. publ. 25.04.2006).

According to the description to the specified patent coke content in the regenerated catalyst should be less than 1 wt.%, preferably less than 0.2 wt.% The content of the coke in splenorenal the catalyst is not less than 2 wt.%, in some embodiments, up to 7-8%. The number of regenerated catalyst in a mixture with neregenerativnymi at least 5%, preferably from 20 to 100%, i.e. superagency aregenerally the catalyst may be absent in a mixture of catalysts.

The catalyst in accordance with the invention recycles 10 g of methanol per 1 g of catalyst at 50% conversion of methanol, while the conventional catalyst recycles only is about 5 g of methanol per 1 g of catalyst. Thus, the catalyst in accordance with the invention retains a longer time their activity (~ 2 times). At the same time, the selectivity of the catalyst developed by major olefins (ethylene and propylene) - 73%, not much higher than the standard catalyst to 69.9%.

The main disadvantage of the above known method, chosen for the prototype is the use of a mixture of regenerated and pregenerating catalysts. When placing such a mixed catalyst in the reactor aregenerally catalyst will continue to superagents and thus lose their activity, and selectivity. The regenerated catalyst has some time to superagents in the pyrolysis process, until it reaches the level of superagonist in which its catalytic properties from the standpoint of activity and selectivity will be optimal.

The technical result of the present invention is to increase the selectivity of the process of obtaining lower olefins by increasing the selectivity of the catalyst used in the process of pyrolysis of methyl chloride.

To achieve a technical result of the proposed method for catalytic pyrolysis of methyl chloride in the process of obtaining lower olefins C2-C4mainly ethylene and PR is Elena, in the presence of silicoaluminate catalyst type SAPO, characterized in that the pyrolysis is performed on the catalyst type SAPO with a degree of supervivencia in the range of 2.6-5.2 wt.%, which is received within 60-150 minutes of operation of the reactor, after which for maintaining the obtained degree of supervivencia the catalyst is continuously directed to a regenerator, where remove excess carbon in the burning air at a temperature of 550°C, and then return to the reactor, while maintaining a constant circulation supereeego catalyst from the reactor of pyrolysis in the regenerator and back.

Unlike the prototype, the proposed method of catalytic pyrolysis of methyl chloride is used only superagency catalyst type SAPO with a degree of supervivencia in the range of 2.6-5.2 wt.%.

The invention is illustrated by examples of the process of pyrolysis of methyl chloride with determining the optimal degree of supervivencia catalyst and its use.

Example 1.

In a reactor with a diameter of 60 mm load 360 cm3catalyst SAPO-34 containing 40% alumina as a binder. Then the reactor is heated to 425°C with the loaded catalyst serves 0.2 nm3/h methyl chloride with volumetric feed rate of 550 h-1(weight of 2.1 h-1). The pyrolysis of methyl chloride was carried out in the course the e 30-210 minutes defining every 30 minutes the contents of ethylene and propylene derived hydrocarbons and the conversion of methyl chloride. The results, presented in table 1 show that the best selectivity for lower olefins (ethylene and propylene) obtained at 90-150 minutes of operation of the catalyst.

It was found experimentally that when carrying out the pyrolysis in these conditions, the degree of superagonist catalyst is 3-5 mass%. To maintain this degree of supervivencia catalyst him after 90-150 served with a speed of 6 cm/min from the reactor to the regenerator, placed next to the reactor and the same with him. The reactor is connected to a regenerator tube in which the catalyst is poured, picked up with air and fed into the regenerator. Regenerated to a desired degree of superagonist catalyst in the same amount according to the level of the regenerator return through the connecting tube into the reactor, providing a continuous circulation supereeego catalyst achieved a degree of superagonist.

The selectivity of the formation of ethylene on the catalyst with the degree of superagonist 3-5 wt.% 45.0-50,3%, and propylene 33,0 of 39.8%, the total selectivity to olefins C2-C383,3-87,2%. Conversion of methyl chloride 55,5 and 70.8% (table 1). The process proceeded in a stationary re who have stable performance.

Example 2.

In a reactor with a diameter of 60 mm load 360 cm3catalyst SAPO-61, containing 40% alumina as a binder. Then the reactor was heated to 450°C with the loaded catalyst is served at 0.42 nm3/h methyl chloride with volumetric feed rate of 1150 h-1, (weight 4,4 h-1). Carry out the pyrolysis of methyl chloride during 30-210 minutes, identifying every 30 minutes the contents of ethylene and propylene derived hydrocarbons and the conversion of methyl chloride. The results presented in table 2, show that the above conditions for the pyrolysis of methyl chloride the best results in terms of selectivity obtained in 60-120 minutes of operation catalyst. It was found experimentally that when carrying out the pyrolysis in these conditions, the degree of superagonist catalyst is 2.6-5.2 wt.%. After 120 minutes the regeneration of the catalyst and circulation supereeego to 2.6-5.2 wt.% the catalyst was carried out as described in Example 1, except that the flow of catalyst to the regeneration increased to 12 cm3/min. Carrying out the pyrolysis process in these conditions allowed slightly to increase the selectivity for ethylene to 43.9-51,3%, but due to the smaller content of total propylene selectivity for olefins 80,0 is 86.6% was lower than in Example 1. Conversion of the chloride mate is and 51,1-71.3 per cent. The process proceeded with stable performance.

See table 1 and 2 data, confirm the achievement of the claimed technical result is an increase in selectivity of the process of obtaining lower olefins by increasing the selectivity of the catalyst, depending on the degree of supervivencia.

As can be seen from the tables, as supervivencia catalyst activity (conversion of methyl chloride) monotonically decreases and the selectivity with respect to the sum of ethylene and propylene passes through a maximum. It's the most selective operation of the catalyst according to the amount of ethylene and propylene is higher than 80% when the carbon content on the catalyst surface in the range from 2.6 to 5.2 wt.%.

Table 1
The catalyst SAPO-34, the temperature of 425°C, supply CH3Cl - 550 h-1
Time, experience, minContent in the resulting hydrocarbon mol%.Conversion of CH3Cl %The total selectivity to ethylene and propylene, %The carbon content in the catalyst, wt.%
C2H4C H6
3024,125,580,4to 49.9
6035,6to 33.879,669,42,0
9045,039,870,884,83,0
12049,4of 37.863,787,24,0
15050,333,055,583,35,0
18050,029,841,479,86,0
21039,524,427,763,9

a 3.9
Table 2
The catalyst SAPO-61, the temperature of 450°C, supply CH3Cl - 1150 h-1
Time, experience, minContent in the resulting hydrocarbon mol%.Conversion of CH3Cl %The total selectivity to ethylene and propylene, %The carbon content in the catalyst, wt.%
C2H4C3H6
1523,124,179,0to 47.2
3027,228,878,156,01,3
6043,936,171,380,02,6
9050,336,365,586,6
12051,331,151,182,45,2
15050,925,235,076,16.5
18048,819,023,967,8

Method for catalytic pyrolysis of methyl chloride in the process of obtaining lower olefins C2-C4mainly ethylene and propylene, in the presence of silicoaluminate catalyst type SAPO, characterized in that the pyrolysis of methyl chloride is performed on the catalyst with a degree of supervivencia in the range of 2.6-5.2 wt.%, which is received within 60-150 minutes of operation of the reactor, after which to maintain received the degree of supervivencia the catalyst is continuously directed to a regenerator, remove excess carbon in the burning air at a temperature of 550°C, and then return to the reactor, while maintaining a constant circulation supereeego catalyst from the reactor of pyrolysis in the regenerator and back.



 

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EFFECT: conversion of hydrogen chloride remains stable when the claimed method is applied.

1 ex, 1 tbl

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