A method of producing benzene, toluene and xylenes

 

(57) Abstract:

A method of producing benzene, toluene and xylenes. Use: petrochemical synthesis. The inventive products: benzene, BF C6H6output 13,64 - 14,35%; toluene, BF C7H8output 22,32 - (LK 23: 43%; xylenes, BF C8H10the output of 14.5 - 14.8 per cent . Reagent: propane or butane, or a mixture. Catalyst: zeolite type JSM-5 containing 0.5 to 3.0% Ga. Conditions: 400 - 500°C, the reactor unit consisting of three reactors, recycling fraction C9+-aromatic hydrocarbons in the amount of 1 - 5% on raw materials in the third reactor unit; the contact time in the reactor of 0.5 - 1.5 C. 1 C.p. f-crystals, 2 ill., 10 table.

The invention relates to the field of petrochemical synthesis, namely the production of aromatic hydrocarbons from the lower paraffins WITH3-C4.

World production of propane and butane, belonging to the group of liquefied petroleum gases in the oil fields and refineries is about 200 million tons per year and is mainly used as energy sources. The reduction of oil reserves and the increasing demand for aromatic hydrocarbons has led to increased interest in propane and butane as petrochemical raw materials.

C, a pressure of 0.1-0.6 MPa on the high-silica zeolites of type ZSM-5 modified by various promoters, which are used zinc, gallium, platinum, chromium and other metals [1, 2, and 3].

Currently for obtaining aromatic hydrocarbons from a liquefied petroleum gases used process "Cyclar developed by firms "UOP" and "British Petroleum" [4]. The target products of the process are benzene, toluene and xylenes. The disadvantage of this method is the relatively low yield of the target products.

The closest in technical essence is an improved method of producing aromatics from hydrocarbons WITH3-C4recycle benzene or toluene in the reactor block [5]. The process is carried out as follows (see Fig.1). Propane (thread 1) together with the part highlighted in benzene or toluene to 8 mol.% (stream 2), and hydrogen (stream 4) are delivered to the reaction block 6 when 487-565aboutAnd pressure of 5-7 at. The total residence time of the raw material mixture in the reaction zone 6-7 C. as the catalyst is zeolite coated with gallium (0,1-10%). In the reaction of dehydrocyclization is obtained a mixture of products and unreacted propane (stream 7), which are sent to once the tick when recycling 6 mol.% benzene is 66%. Without recycle benzene conversion of propane to aromatics was 60%. Because ER N 0230655 not presents the material balance for products, we have reproduced this patent recycle 6 mol.% toluene and propane high purity catalyst ZSM-5 module 60 and applied Ga in the amount of 3% at 560aboutAnd the total residence time in the reaction zone 6-7 C. When the conversion of propane to aromatics amounted to 66 wt.%, content9+aromatics products 16,77%, and xylenes is 7.85% . The disadvantage of this method is the high content9+aromatics and low levels of xylenes.

The aim of the proposed method is to reduce the education side of heavy aromatic hydrocarbons and increase the yield of xylenes.

This goal is achieved by submission in the last reactor unit selected in the unit of division of fractions of aromatic hydrocarbons WITH9+in the amount of 1-5% by on fresh raw materials at the time of contact of the gas stream in the reactor with the catalyst is 0.5 to 1.5 sec.

The proposed process can be carried out in the reactor block with a fixed catalyst bed, or moving bed of catalyst and with continuous regeneration.

P. Fig.2). In the reactor unit consisting of three consecutive reactors, serves a mixture of hydrocarbons WITH3-C4(thread 1) in the first as the reactor 2. Hydrocarbons WITH3-C4with the reaction products consistently served in the second 3 and third 4 reactors. The process is carried out on silica zeolite ZSM-5 modified with gallium at 400-600aboutAnd the total time of contact 5-7.

The catalyst reactors distributed in such a way (with a fixed bed of catalyst), the time of contact in the third reactor was varied in the range of 0.5-1.5 C. In the reactor unit with a movable layer of the catalyst to the desired contact time in the last reactor with the catalyst is achieved by changing the location of the input fraction9+. The fraction of aromatics WITH9+after separating heated and served in the third reactor (stream 5). The reaction products from the third reactor (stream 6) through the cooler-condenser 7 are received in the separator 8, where the separation H2WITH1and C2. Then the reaction products and unreacted3-C4(stream 10) are separated in the stabilization column 11 of liquid products. Fraction WITH3-C4taken on the top of the column at 60aboutWith and davleniya (stream 13) is separated by rectification method in the system columns: in column 14 at 80-81aboutWith and reflux the number 10 at the top is selected benzene (stream 15), the bottom stream 16; column 17 on the top of the column is taken toluene at 110aboutWith and reflux 3 (stream 18), in column 20 of the cubic product of the column 17 at 138-142about(Stream 19), and reflux the number 5 are xylenes (stream 21), and from the cube column 20 is constantly displayed in fraction (stream 22) aromatic hydrocarbons9+, part of which is returned in recycling (stream 5).

The novelty of the invention is that at a certain contact time (0.5 to 1.5) of a gas stream, comprising fraction WITH9+with the catalyst in the last reactor intensive dealkylation, disproportionation, transalkylation9+aromatics without the formation of by-products - heavy aromatic hydrocarbons. As a result, in catalyzate combined process decreases the amount of heavy aromatic hydrocarbons in 2 and more times, and increases the content of xylenes from 7.0 to 14.6-14.8 per cent. In addition, catalyzate combined process increased the content of n-xylene, compared to the baseline (without recycling) catalyzate. All of this is a consequence of the fact that found in the conditions of processing of fractions WITH9+comes with high Celerity purpose of the invention - reducing the formation of heavy aromatic hydrocarbons, the authors give the example of the prototype recycle of toluene in the proposed conditions.

For convenience compared the performance of the process is at 100% conversion of propane.

P R I m e R 1. In the reaction block 6 (see Fig.1) at 560aboutC and a pressure of 5 at serves 100 kg/h of propane high frequency (stream 1), this comes from the column 21 stream 2, representing the toluene in the amount of 12,55 kg/h, which corresponds to 6 mol.% of toluene. The total residence time of the raw material mixture in the reaction zone 6-7 C. as the catalyst is zeolite ZSM-5 with a module 60 and deposited gallium in the amount of 3%. In the reaction of dehydrocyclization receive the mixture of reaction products (stream 7), which are sent to the separation (see Fig.1). The portion allocated toluene and re-circulated into recycling. Table 1 presents the material balance flow. The conversion of propane to aromatics is 66%. The yield of aromatics excluding recirculating flow - 66 kg/h Content9+aromatics products amounted 16,77%, and xylene - 7,0%.

P R I m m e R 2. In the reactor unit consisting of three consecutive reactors (see Fig.2), serves 100 kg/h of propane. P 500aboutC and flow rate 2 h-1the contact time of the gas stream with a catalyst in the last reactor is 1.5 S. posledni the reactor through the heater shall also be faction WITH9+in an amount of 5 kg/h (flow 5). Leaving the last reactor, the reaction products are cooled in the refrigerator 7 and fed to the separator 8, where the separated hydrogen and hydrocarbons1-C2. Liquid products are sent to a stabilization column 11 of liquid products, where on top of selected hydrocarbons WITH2-C4that is returned in the process. VAT product is sent to the column 14 allocation of benzene. CBM product columns 14 serves on the separation column 17, where the top emit toluene, and CBM product is fed to the column 20. In column 20 on top of the produce xylenes (stream 21), and Cuba - FROM9+the aromatics, some of which (stream 5) return in the process.

The material balance is presented in table.2. Content9+the aromatics in the reaction products was 6,02% against 16,77% in the prototype, and the content of xylenes increased to 14.6% (7.0% in the prototype).

P R I m e R 3. The process is conducted as described in example 2, but the aromatization3-C4performed at 600aboutWith e"ptx2">

The material balance is presented in table.3. Content9+the aromatics in the reaction products was 5,58% against 16,77% in the prototype, and the content of xylenes increased to 14.8% (7.0% in the prototype).

P R I m e R 4. The process is conducted as described in example 3, but the zeolite ZSM-5 contains 0.5% Ga. In the last reactor serves part of the fraction9+the aromatics in the amount of 1.0 kg/h and the time of contact of the thread in the last reactor of 0.5 sec.

The results are presented in table.4. Content9+the aromatics in the reaction products was 5,64% against 16,77% in the prototype, and the content of xylenes increased to 14.5%.

P R I m e R 5. The process is conducted as described in example 2, but the aromatization fraction3-C4goes on zeolite ZSM-5 containing 0.5% gallium, the process is carried out at 400aboutC. In the last reactor unit serves part of the fraction9+the aromatics in the amount of 3.2 kg/h

The material balance is presented in table.5. Content9+the aromatics in the reaction products amounted to 5.57% , and the content of xylenes increased to 14.8%.

P R I m e R 6. The process is conducted as in example 2, but at a temperature of 600aboutAnd in the last reactor unit serves aromatics increased in comparison with examples 2 and 3 to 6.9% (an increase of 14-24 Rel.%), and the content of the xylenes, compared with the prototype, increased to 13.6%. Thus, the degree of transformation recirculated9+fraction in the target products (benzene, toluene and xylenes) decreased.

P R I m e R 7. The process is conducted as in example 2, but the time of contact of the stream containing the recirculated portion of the fraction9+the aromatics in the last reactor unit with a catalyst 1,6 with.

The material balance is presented in table.7. Content9+aromatics products, compared with the results of example 2 increased from 6,02% to 7.1% (i.e. 18 Rel.%), although lower than in the prototype (16,77%). The content of the xylenes also decreased: 12,6% against 14.6% in example 2. When comparing these data with the data of example 9 (without recycling WITH9+fraction) shows that in the conditions of example 7 there is no advantage in increasing the yield of xylenes and, on the contrary, the content of C9+aromatics increased. Thus, when the contact time of 1.6 with increase in comparison with the sample without recycling, energy consumption per unit produced target products.

P R I m e R 8. The process is carried out as in example 3, but the time of contact of the stream containing the recirculated portion of the fraction9+aromatics, with catalg, compared with the results of example 3, much more: 7,3% compared to 5.58% . In addition, the content of the xylenes is also reduced to 13.7% (14.8% in example 3), which is higher than in the prototype, but is at the level of the content of the xylenes in example 9. Thus, when the decrease in contact time up to 0.4 with a fraction WITH the9+not have time to fully subjected to dealkylation reaction, and a positive effect is minimal.

P R I m e R 9. The process is conducted as in example 2, but without recycle fraction9+the aromatics in the last reactor of the reactor block.

The results are presented in table.9. Content9+the aromatics in the reaction products 5,59%, and xylene - 14,1%.

In table.10 presents comparative data the results given in examples 1-9.

1. A METHOD of producing BENZENE, TOLUENE AND XYLENES by contacting alkanes C3- C4with kalisoderjasimi vysokoglinozemistym zeolite catalyst ZSM-5 at an elevated temperature in the reactor unit, consisting of three series-connected reactors, with subsequent separation of the reaction products to recycle a fraction of the original alkanes, benzene, toluene, xylene and the fraction of C9+-aromatice the different topics that, to reduce the formation of C9+-aromatic hydrocarbons and enhance the yield of xylenes, as the fraction of aromatic hydrocarbon recycle fraction C9+-aromatic hydrocarbons in the amount of 1-5 wt.% the raw material in the third reactor of the reactor block and the process in the reactor is carried out at contact times of 0.5-1.5 C.

2. The method according to p. 1, characterized in that the process of contacting is conducted at a temperature of 400-600oC.

 

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1 cl, 5 ex, 5 tbl

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3 cl, 3 tbl

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2 cl, 1 tbl, 7 ex

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16 cl, 2 dwg, 2 tbl

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3 cl, 1 tbl, 7 ex

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5 cl, 5 tbl, 14 ex

FIELD: chemistry.

SUBSTANCE: method involves hydrocarbon transformation in a reactor in the presence of modified catalyst containing, mass %: 53.0-60.0 of ZSM-5 high-silica zeolite with the ratio of SiO2/Al2O3=39, 34.0-38.0 of Al2O3, 2.0-5.0 of B2O3, 1.0-5.0 of Zn, 0.0-5.0 of W, 0.0-3.0 of La, 0.0-3.0 of Ti at 300÷700°C, including separation of liquid and solid transformation products, followed by burning oxidation of gaseous products and addition of the obtained mix of carbon dioxide and water vapour to the source hydrocarbons at the rate of 2.0÷20.0 mass %. Before the raw material intake the reaction system is flushed by an inert gas (nitrogen), starting from 300°C and to the transformation temperature. Hydrocarbons used are alkanes, olefins or alkane olefin mixes C2-C15 without preliminary separation into fractions. Gaseous transformation products undergo burning and complete oxidation in the presence of an oxidation catalyst of vanadium/molybdenum contact piece, V2O5/MoO3. To sustain continuous process two identical reactors are used, where the catalyst is transformed and recovered in turns.

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2 ex

FIELD: chemistry.

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EFFECT: obtaining of a catalyst with higher activity during conversion of methane in aromatic hydrocarbons.

3 cl, 1 tbl, 7 ex

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