The method of separation of aromatic hydrocarbons from mixtures thereof with non-aromatic

 

(57) Abstract:

Usage: in the petrochemical technologies. The essence of the invention: separation of aromatic hydrocarbons from mixtures thereof with non-aromatic extraction with an aqueous solution of polyglycol in the presence of monoethanolamine with getting the raffinate and extract phase by distillation extract phase with water to obtain an extract of risaykl, water polyglycol, Department of risaykl and extract the aqueous layer, the return of risaykl on the extraction, separation of the aqueous polyglycol, water washing rafinate phase and the extract by distillation washed extract individual aromatic hydrocarbons, a feed water layer on the rectification of the extract phase, the use of the water layer separated from the risaykl, for washing of hydrocarbons, submission of monoethanolamine in water layer and/or the washing water, the direction of wash water to extraction. For washing rafinate phase using the aqueous layer was separated from the risaykl received the wash water is directed to the extraction of raw materials and/or risaykl, and for washing the extract phase using the aqueous layer was separated from the extract obtained the wash water is fed to the rectification of excobar selection of aromatic hydrocarbons from mixtures thereof with non-aromatic liquid extraction, and can be used in oil - and chemical-recovery industry.

A known method for separating aromatic hydrocarbons from mixtures thereof with non-aromatic, according to which the extraction is carried out by circulating an aqueous solution of diethylene glycol (deg), containing 7 wt. water, obtaining the raffinate and extract phases. This extract phase are sent to distillation with water to obtain risaykl, extract and water deg. From risaykl and the extract is separated by water layers, gather them in the tank, where through the heat exchanger is fed to the rectification in the form of steam.

The selected extract and rafinate phase is washed with water until the residual content of the solvent is not more than 0.005 wt. Extract serves to further processing to highlight the rectification of individual aromatic hydrocarbons.

Received the washing water directed to the regeneration of the extractant by distillation, most of the water from the last reset to the sewage system. Distilled and then under vacuum, the aqueous concentrate deg return in circulating deg.

To maintain the pH of aqueous deg in the system is not below 8.5 in regenerated deg and the aqueous layer serves monoethanol is correlated with a large circulation of risaykl (70-130 about. raw materials extraction) and water (7-13,5 t/hour) required for the distillation of hydrocarbons, as well as with the presence of a significant stage of distillation of water (3.2 t/h with regard to irrigation) during distillation the separation of wash water, a significant amount of wastewater (1.6 tons/hour) with a relatively high concentration of extractant (up to 0.2 wt.), several times the maximum permissible concentration for discharge to biological treatment, which is not only difficult, but also increases the cost of disposal of these waters. The latter contributes to increased losses of extractant from the raffinate and extract up to very high values (40 tons/year).

In the operation of industrial plants sometimes occurs periodic foaming products in various devices of the system, resulting in partial violation of the technological regime, which also leads to increased consumption of the extractant, the deterioration in the quality of the extract and secreted from an aromatic hydrocarbon.

In General, some of these reasons lead to a relatively low extraction of aromatic hydrocarbons under extraction (benzene 98, toluene 95 wt.).

Closest to the invention to the technical essence and the achieved result is mu liquid extraction is carried out with an aqueous solution of polyglycol in the presence of monoethanolamine with getting the raffinate and extract phases, the rectification extract phase with water to obtain risaykl, extract, water polyglycol, Department of risaykl and extract the aqueous layer, the return of risaykl on the extraction, separation of the aqueous polyglycol into two parts with the direction of one of them on the extraction, and the other

the regeneration polyglycol, water washing rafinate phase and extract with getting washed out of the raffinate and extract and wash water, by distillation washed extract individual aromatic hydrocarbons, a feed water layers of rectification extract phase with simultaneous use of 40-100 wt. the water layer separated from the risaykl, for washing of hydrocarbons rafinate phase and extract the filing of monoethanolamine in water layer and/or the washing water, the direction of wash water on the extraction of the two flows of raw materials and risaykl at mass ratio of 1:1 3:1 (prototype) [2]

However, this method is not high enough extraction in the extraction step such aromatic hydrocarbons, such as toluene or xylenes (when making their mark "with the quality mark" for example, catalyzate reforming faction 62-105oC removing the toluene is 97-98% and xylenes 73% ), as well as quality] - 0,18%). In addition, high energy consumption process that is associated with the still relatively high circulation of risaykl about 70-83. for raw water (for example, in examples 4 and 5 total distillate water in the extractive distillation column is 8.3 and 10.0 t/h, including filing a sharp pair of 7.0 and 5.0 t/h).

The aim of the invention is to increase the yield of aromatic hydrocarbons from raw material extraction, to improve their quality, reduce energy costs of the process.

This goal is achieved by the described method of separation of aromatic hydrocarbons from mixtures thereof with non-aromatic by solvent extraction with an aqueous solution of polyglycol in the presence of monoethanolamine with getting the raffinate and extract phases, distillation of the extract phase with water to obtain an extract of risaykl, water polyglycol, Department of risaykl and extract the aqueous layer, the return of risaykl on the extraction, separation of the aqueous polyglycol into two parts with the direction of one of them on the extraction, and the other

the regeneration polyglycol, water washing rafinate phase and extract with getting washed out of the raffinate and extract and appropriate wash water, by distillation washed extract from gaining what ispolzovaniem 40-100 wt. the water layer separated from the risaykl for washing rafinate phase, the direction of the wash water obtained in the extraction of raw materials and/or risaykl, the use of the water layer separated from the extract, for washing of the extract, the direction of the wash water obtained together with part of the water layer (0-60%), separated from the risaykl, rectification extract phase.

The difference of the proposed method from the prototype is that 40-100 wt. the water layer separated from the risaykl, used only for washing rafinate phase and the resulting wash water is sent to the extractor one or two streams: raw materials and/or risaykl. Washing of the extract hold water layer separated from the extract, and the resulting wash water together with part of the remaining water layer (0-60%), separated from the risaykl, sent for rectification extract phase (in the form of so-called sharp pair).

In particular, the proposed method allows you to abandon the regulation of the correlation of supply of wash water in raw materials and/or risaykl. Water may come from both streams (from raw material extraction and risaykl), or one of these threads.

Offer is uliuli water polyglycol line 2, containing 5-12 wt. water, in the middle part along the line 3 serves partial hydrocarbons together with part of the wash water flowing along the line 4 from the tank 22, and the lower part risaykl in the mix with the rest of the wash water supplied through the line 6 of the same capacity. If necessary, this wash water may be supplied and with only one hydrocarbon stream (raw or risaykl).

Rafinate phase on line 7 away from the top of the extractor 1, is fed into the lower section of the wash column 20 and then remove from the installation.

The extract phase is output from the bottom of the extractor 1 through line 8, somewhat cooled in the heat exchanger extract-water 9, into the chamber of a single evaporation (KOI) 10, and then the upper tray of the extractive distillation column 11. Steam flows 12 from the top KOI 10 and 13 from the top of column 11 are combined into a single stream 14, which is first condensed and cooled, and then the liquid is directed into the separation tank 15, where the demixing into two phases. The upper hydrocarbon phase (risaykl) served in the lower part of the extractor 1 through line 5. The aqueous phase is removed from the vessel 15 through line 16, and then 40-100% of its on line 17 is directed into the tank 18, where if necessary add Neut on line 19 in the upper part of the lower (raffinates) section of the wash column 20. Wash water is removed from the bottom of the specified section on the line 21 and enters the tank 22, which if necessary can also add a small amount of the IEA. From the tank 22 wash water in the lines 4 and 6 send one or two streams with flows of raw materials and/or risaykl in extractor 1.

If washing the raffinate not take the entire aqueous phase is separated from the risaykl in the vessel 15, the remainder is directed through line 23 to the collector 24 of the circulating water.

Steam stream 25 from the middle part of the column 11 condensed and cooled, and then the liquid is directed into the separation tank 26, where delamination occurs in two phases. The upper hydrocarbon phase (aromatic extract) on line 27 serves in the upper section of the wash column 20. The extract, after washing with water until the content of the extractant is not more than 0,001-0,005% (as in washed raffinate) is fed to the distillation for separation from it of individual aromatic hydrocarbons (not shown). The aqueous phase from the tank 26 through line 28 into the upper part of the upper (extract) section of the wash column 20. Wash water is removed from the bottom of that section, on the line 29 is supplied to the collection circulating water 24, which also receives (attachment 30 is fed into the heat exchanger 9, where this stream is heated further in the form of so-called direct steam is supplied via line 31 down the column 11 for Stripping from the extractant all hydrocarbons.

A small part of the circulating between columns 1 and 11 of the water extractant direct line 32 in the vacuum cube 33. Distilled at a residual pressure of 20 mm RT. senior water extractant is removed from the cube 33, line 34 serves in the collector 35, and return line 36 to the circulating flow of the extractant 2.

From the bottom of the vacuum cube 35 through line 37 to periodically merge the high-boiling residue.

P R I m e R 1 (comparative, a well-known example 4 in [2]). 36,12 t/h (49,4 m3/hour) catalyzate reforming faction 62-105oC containing t/h (wt. ): benzene 4,53 (12,54), toluene 7,10 (19,66), xylenes 0,58 (1,60) and 23,01 (66,20) nah, served at a temperature of 100oC 18-th plate extractor, 33,62 t/h or 41.0 m3/hours of risaykl (25,62 t/h aromatic and 8.00 t/h nah; respectively and 76,2 23,8 wt.) served under the 1st bottom plate of the extractor at a temperature of 60oC and on the upper plate 355 t/h (355 m3/hour) water deg at a temperature of 150oC, consisting of 328,0 t/h deg and 27,0 t/h of water.

what utilizaton and risaykl in the extractor serves another, respectively, 1.0 and 0.3 m3/h of wash water from the collector 22. The ratio between the amounts of these waters is 3.3:1.

The output from the top of the extractor raffinate 24,25 t/h (100 wt.) containing, t/h (dry wt.): benzene 0,01 (0,04), toluene 0,21 (0,86), xylenes 0,14 (0,58), nonaromatic hydrocarbons 23,80 (98,52), sent for water washing in the bottom section of the column 20 and the top of the column output with the installation.

The extract phase (401,78 t/h), containing t/h: aromatic hydrocarbons 37,47, nonaromatic hydrocarbons 8,01, deg 328,02, water 28,28, is sent to the heat exchanger 9, and then once in a blue moon 10 and up extractive distillation column 11, where this phase is divided into three parts in the presence of water supplied down the column 11 in the form of steam in the amount of 7.0 t/h of the collector 24.

Products from the top KOI 10 and the top of the column 11 unite (the total number 36,82 t/h), then share in the sump 15 to the hydrocarbon and water phases. The hydrocarbon phase (risaykl above composition) is sent to the extractor in the number 33,62 t/h. The aqueous phase is 3.2 t/h (100 wt.) divided into two parts: 1.9 t/h (60) it is sent to the collector 24 of the circulating water, and 1.3 tons/hour (40) in the collector 18, which also add to 1.35 l/day technical IEA. The water is then (1.3 tons/hour) of the collector 18 is directed to Ave the same type of 1.35 l/day technical IEA. From the collector 22 of the wash water in the amount of 1.3 t/h enters the above image extractor 1.

The product of the average of column 11 (16,97 t/h) are separated in the sedimentation tank 26 into two phases. The aqueous phase (5,1 t/h) is sent to the collector 24 where it is mixed with part of the water from the risaykl (1.9 t/h). Then the aqueous phase of the collector 24 in the amount of 7.0 t/h is fed through the heat exchanger 9 down the column 11 in the form of steam.

The hydrocarbon phase from the collection 26 (aromatic extract) 11.87 per t/h (100 wt. containing, t/h (dry wt.): benzene to 4.52 (38,07), toluene 6,886 (58,01), xylenes 0,44 (3,71), nonaromatic hydrocarbons 0,025 (0,21), sent for water washing in the upper section of the column 20, and then to the division with the aim of obtaining individual aromatic hydrocarbons.

From the extract by distillation get to 4.52 t/h of benzene brand "for the synthesis of higher grade (temperature of crystallization are 5.36oC, the content of impurities nah 0.23 wt. ), 6,89 t/h of toluene grade "a" (the content of non-aromatic impurities of 0.18 wt.), and of 0.44 t/h xylene fraction.

The degree of extraction of benzene from the potential content in raw materials extraction is 99.9 wt. toluene 97,0 wt. and xylene 75,9 wt.

From the bottom of the vacuum cube once in two months is drained of accumulated heavy black residue that is sent for incineration.

P R I m m e R 2. 36,12 t/h (49,4 m3/hour) catalyzate reforming faction 62-105oC containing t/h (wt. ): benzene 4,53 (12,54), toluene 7,10 (19,66), xylenes 0,58 (1,60) and 23,91 (66,20) nah, served at a temperature of 100oC 18-th plate extractor. 23,71 t/h or 29,64 m3/hours of risaykl (15,60 t/h and aromatic 8,11 t/h nah, respectively 65,8 and 34.2 wt.) served on the 1st plate of the extractor at a temperature of 60oC and on the upper plate 355 t/h (355 m3/hour) water deg at a temperature of 150oconsisting of 328 t/h deg and 27,0 t/h of water.

The mass ratio of water deg: the raw material was 9.8:1, and the ratio risaykl: the raw material is about 60.

Together with catalyzate in the extractor serves 0,84 t/h, and with risaykl 0,26 t/h of wash water from the collector 22. The ratio of these is ash, toluene 0,10 (0,42), xylenes 0,057 (0,24), nonaromatic hydrocarbons 23,885 (99,34), sent for water washing in the bottom section of the column 20 and the top of this section derive from the installation.

The extract phase (391,89 t/h), containing, t/h: aromatic hydrocarbons 27,65, nonaromatic hydrocarbons 8,14, deg 328,02, water 28,08, is sent to the heat exchanger 9, and then once in a blue moon 10 and up extractive distillation column 11, where this phase is divided into three parts in the presence of water supplied down the column 11 in the form of steam in the amount of 5.7 t/h of the collector 24.

Products from the top KOI 10 and the top of the column 11 unite (the total number 26,41 t/h), then share in the sump 15 to the hydrocarbon and water phases. The hydrocarbon phase (risaykl above composition) is sent to the extractor in the number 23,71 t/h. The aqueous phase (2,7 t/h) is divided into two parts: 1.6 tons/hour (60 wt.) she served in the collector 24, and 1.1 t/h (40 wt.) send in the tank 18 and then in the bottom section of the column 20 for washing the raffinate. From the bottom of this section to divert wash water (1.1 t/h) in the collector 22, whence it is directed above image extractor 1. Previously in the tank 18 and 22 add to 1.3 l/day IEA.

The product of the average of column 11 (16, is mevki extract. Wash water deduce from the bottom of this section in a collection of 24 where it is mixed with part of the water from the risaykl (1.6 tons/hour). Then the aqueous phase of the collector 24 in the amount of 5.7 t/h is fed through the heat exchanger 9 down the column 11 in the form of steam.

The hydrocarbon phase from the collection 26 (aromatic extract) 12,08 t/h (100 wt. containing, t/h (dry wt.): benzene 4,53 (37,51), toluene 7,00 (57,95), xylenes 0,523 (4,33), nonaromatic hydrocarbons 0,025 (0,21), sent for water washing in the upper section of the column 20, and then split it into individual aromatic hydrocarbons.

From the extract by distillation get a 4.53 t/h of benzene brand "for the synthesis of higher grade (temperature of crystallization are 5.36oWith the content of impurities nah 0.23 wt. ), 7,00 t/h of toluene grade "a" (the content of non-aromatic impurities of 0.18 wt.), and 0,523 t/h xylene fraction.

The degree of extraction from the potential content in raw materials extraction is: for benzene and about 100.0% toluene to 98.6 wt. xylene is 90.2 wt.

From the bottom of column 11 assign 355 t/h of water deg provided at the beginning of the sample composition and is directed to the top of the extractor. A small amount of water deg (0.5 to 2 wt. from his boot in the DAG is directed to a collection of 35, and then return to the circulating flow of the extractant 2.

From the bottom of the vacuum cube once in two months is drained of accumulated heavy black residue that is sent for incineration.

P R I m e R 3. Extraction in column 1 is carried out similarly using the same raw material and the extractant and in the same amounts as in example 2. However, the number of risaykl is 24,65 t/h or 30.63 per m3/h (16,46 t/h and aromatic 8,14 t/h nah, respectively 66,9 and 33.1 wt.).

The mass ratio of water deg: the raw material is 9.8:1, and the ratio risaykl: raw materials 62 about.

The output from the top of the extractor raffinate 24,063 t/h (100 wt.), containing, t/h (dry wt.): traces of benzene, toluene 0,11 (0,46), xylenes 0,068 (0,28), nonaromatic hydrocarbons 23,885 (99,26), sent for water washing in the bottom section of the column 20 and the top of this section derive from the installation.

The extract phase (392,76 t/h), containing, t/h: aromatic hydrocarbons 28,49, nonaromatic hydrocarbons 8,17, deg 328,02, water 28,08, is sent to the heat exchanger 9, and then once in a blue moon 10 and up extractive distillation column 11, where this phase is divided into three parts in the presence of 5.9 t/h steam supplied isradelic in the sump 15 to the hydrocarbon and water phases. The hydrocarbon phase (risaykl 24,65 t/h above composition) is sent to the extractor. The aqueous phase (2,7 t/h) is divided into two parts, 60% (1.6 t/h) is sent to the collector 24, and the remaining amount (1.1 t/h, 40%) is directed into the tank 18 and then in the lower section of the column 20 for washing the raffinate. From the bottom of this section of the wash water is directed to a collection of 22, where it is sent to the extractor 1 in the amount of 1.1 t/h together with the raw material. Previously in the tank 18 and 22 add 1.3 l/day IEA.

The product of the average of column 11 (16,36 t/h) are separated in the sedimentation tank 26 into two phases. The aqueous phase (4.3 tons/hour) is directed into the upper section of the column 20 for washing the extract. Wash water deduce from the bottom of this section in a collection of 24 where it is mixed with part of the water from the risaykl (1.6 tons/hour), and then in the form of steam is fed down the column 11 in the amount of 5.9 t/h.

The hydrocarbon phase from the collection 26 (aromatic extract) 12,06 t/h (100 wt. containing, t/h (dry wt.): benzene 4,53 (37,57), toluene 6,99 (57,97), xylenes 0,512 (4,25), nonaromatic hydrocarbons 0,025 (0,21), is directed into the upper section of the column 20, and then split it into individual aromatic hydrocarbons.

From the extract by distillation get a 4.53 t/h of benzene, oderjanie in raw materials amounted to, respectively: about 100.0; 98,4 and 88.3 wt.

Similarly performed, and vacuum distillation of part of the water DAN withdrawn from the bottom of column 11.

P R I m e R 4. The extraction of aromatic hydrocarbons and other process stages carried out in the same conditions as in example 3. The difference is only that the wash water generated during the cleaning of the raffinate in the same number of (1.1 t/h) is fed to the extractor 1, but not with raw materials and with risaykl.

When this is obtained the same results as in example 3, except for very small differences in the content of the xylenes in the raffinate and extract what little impact on the degree of extraction (88,7 wt.).

The composition of the raffinate: 24,061 t/h (100 wt.), including: benzene traces, toluene 0,11 (0,46), xylenes of 0.066 (0,27), nonaromatic hydrocarbons 23,885 (99,27).

The composition of the extract: 12,06 t/h (100 wt.), including: benzene 4,53 (37,57), toluene 6,99 (57,96), xylenes 0,514 (4.26 deaths), nonaromatic hydrocarbons 0,025 (0,21).

P R I m e R 5 (comparative known example 5 in [2]). 36,12 t/h (49,4 m3/hour) of the reforming catalyst fraction 62-105oC containing t/h (dry wt.): benzene 4,53 (12,54), toluene 7,10 (19,66), xylenes 0,58 (1,60), nonaromatic hydrocarbons 23,91 (66,20), served at a temperature of 100oC on the 18th of tandardov, accordingly 74,0 and to 26.0 wt. ) served under the 1st plate of the extractor at a temperature of 60oC and on the upper plate at a temperature of 150oC 260 t/h of aqueous triethylene glycol (TEG), consisting of 241,80 t/h and 18,20 t/h of water.

The mass ratio of water TAG: raw materials amounted to 7.2:1, and the ratio risaykl:the raw material is about 70.

Together with catalyzate in extractor 1 from the tank 22 serves to 2.5 t/h of wash water and together with risaykl 2.5 t/hour (a total of 5.0 t/h). The ratio of these water 1:1.

The output from the top of the extractor raffinate 24,13 t/h (100 wt.) containing, t/h (dry wt.): toluene 0,14 (0,58), xylenes 0,10 (0,41), nonaromatic hydrocarbons 23,89 (99,01), sent for water washing in the lower section of the column 20 and the top of this section derive from the installation.

The extract phase (305,02 t/h), contains (t/h) aromatic hydrocarbons 32,71, nonaromatic hydrocarbons 7,31 TAG 241,80, code, 23,20, is sent to the heat exchanger 9, and then once in a blue moon 10 and up extractive distillation column 11, where this phase is divided into three parts in the presence of steam supplied down the column 11 in the amount of 5.0 t/h.

Products from the top KOI 10 and the top of the column 11 unite (the total number 33,03 t/h), then share in the sump 15 is ctor 1 in the amount of 28,03 t/h. All of the aqueous phase (5.0 t/h) serves in the capacity of 18, and later in the wash column 20 for washing the extract and the raffinate. From this column, the washing water is directed to a collection of 22, where they are sent the above image extractor 1. Previously in the capacity of 22 add to 2.1 l/day IEA.

The product of the average of column 11 (16,99 t/h) are separated in the sedimentation tank 26 into two phases. The aqueous phase (5.0 t/h) is sent to the collector 24 from whence it is fed through the heat exchanger 9 down the column 11 in the form of steam.

The hydrocarbon phase from the collection 26 (aromatic extract) 11,995 t/h (100 wt. containing, t/h (dry wt.): benzene 4,53 (37,77), toluene of 6.96 (58,02), xylenes 0,48 (4,00), nonaromatic hydrocarbons 0,025 (0,21), sent for water washing in the upper section of the column 20, and then split it into individual aromatic hydrocarbons.

From the extract by distillation get a 4.53 t/h of benzene and of 6.96 t/h of toluene are given in examples 1-4 quality, as well as to 0.48 t/h xylene fraction.

The degree of extraction of aromatic hydrocarbons from the potential of their content in raw materials extraction amounted to benzene 100,0; toluene 98,0; xylene 82,7 wt.

Vacuum distillation of part of the water deg, exhaust from the bottom to the/SUP>/hour) catalyzate reforming faction 62-105oC containing t/h (wt. ): benzene 4,53 (12,54), toluene 7,10 (19,66), xylenes 0,58 (1,60), nonaromatic hydrocarbons 23,91 (66,20), served at a temperature of 100oC 18-th plate extractor 1. 23,71 t/h or 29,64 m3/hours of risaykl (15,60 t/h and aromatic 8,11 t/h nah, respectively 65,8 and 34.2 wt.) served under the 1st plate of the extractor at a temperature of 60oC and on the upper plate 260 t/h (260 m3/hour) water TAG at a temperature of 150oC, consisting of 241,80 t/h TAG and 18,20 t/h of water.

The mass ratio of water-TAG: the raw material was 7.2:1 and the ratio risaykl: the raw material is about 60.

Together with risaykl in the extractor serves 2.3 t/h of wash water from the collector 22.

The output from the top of the extractor raffinate 24,049 t/h containing t/h (dry wt.): toluene 0,10 (0,41), xylenes 0,064 (0,27), nonaromatic hydrocarbons 23,885 (99,32), sent for water washing in the bottom section of the column 20 and then from the top of this section derive from the installation.

The extract phase (298,38 t/h), containing, t/h: aromatic hydrocarbons 27,65, nonaromatic hydrocarbons 8,13, TAG 241,80, water 20,80, is sent to the heat exchanger 9, and then once in a blue moon 10 and the top of the column 11, where etot/hour.

Products from the top KOI 10 and the top of the column 11 unite (the total number 26,31 t/h), then share in the sump 15 to the hydrocarbon and water phases. The hydrocarbon phase (risaykl above composition) is sent to the extractor in the number 23,71 t/h.

All of the aqueous phase (2.6 t/h) is directed into the tank 18 and then in the bottom section of the column 20 for washing the raffinate. From the bottom of this section to divert wash water in the collector 22, whence it is sent to the extractor together with risaykl. Previously in the capacity of 22 add 32,1 l/d IEA.

The product of the average of column 11 ($15.87 with t/h) are separated in the sedimentation tank 26 into two phases. The aqueous phase (3.8 t/h) is directed into the upper section of the column 20 for washing the extract. Wash water is distilled off from the bottom of this section in a collection of 24 where it is in the amount of 3.8 t/h serves first in the heat exchanger 9, and then down the column 11 in the form of steam.

Aromatic extract 12,07 t/h (100 wt.), containing, t/h (dry wt.): benzene 4,53 (37,53), toluene 7,00 (57,99), xylenes 0,516 (4,27), nonaromatic hydrocarbons 0,025 (0,21), is directed into the upper section of the column 20, and then split it into individual aromatic hydrocarbons.

From the extract by distillation get a 4.53 t/h of benzalazine aromatic hydrocarbons from the potential of their content in raw materials extraction amounted to benzene 100,0, toluene 98,6, xylenes to 89.9 wt.

From the bottom of column 11 assign 260,0 t/h of water TAG above composition and then served in the upper part of the extractor. A small amount of water TAG (0.5 to 2 wt. from its load in the system) served in the cube 33, where it is distilled under a residual pressure of 20 mm RT.article Distilled under vacuum, water TAG, assign to the collector 35, and then return to the stream of circulating extract 2.

From the bottom of the vacuum cube 33 once in two months is drained of accumulated heavy black residue that is sent for incineration.

P R I m e R 7. 36,12 t/h (49,4 m3/hour) catalyzate reforming faction 62-105oC containing t/h (wt. ): benzene 4,53 (12,54), toluene 7,10 (19,66), xylenes 0,58 (1,60), nonaromatic hydrocarbons 23,91 (66,20), served at a temperature of 100oC 18-th plate extractor 1. 25,11 t/h or 31,12 m3/hours of risaykl (17,02 t/h aromatic and 8,09 t/h nah, respectively 67,8 and to 32.2 wt.) served under the 1st plate of the extractor at a temperature of 60oC and on the upper plate 260 t/h (260 m3/hour) water TAG, consisting of 241,80 t/h TAG and 18,20 t/h of water.

The mass ratio of water TAG: raw materials amounted to 7.2, and the ratio risaykl: the raw material is about 63.

The extract phase (300,14 t/h), containing, t/h: aromatic hydrocarbons 29,04, nonaromatic hydrocarbons 8,10, TAG 241,80, water 21,20, is sent to the heat exchanger 9, and then once in a blue moon 10 and the top of the column 11, where this phase is divided into three parts in the presence of water supplied down the column 11 in the form of steam in the amount of 4.4 t/h.

Products from the top KOI 10 and the top of the column 11 unite (the total number 28,11 t/h), then share in the sump 15 to the hydrocarbon and water phases. The hydrocarbon phase (risaykl above composition) is sent to the extractor in the number 25,11 t/h. All of the aqueous phase (3,0 t/h) is directed into the tank 18 and then in the bottom section of the column 20 for washing the raffinate. From the bottom of this section to divert wash water in the collector 22, whence it is sent to the extractor together with the raw material. Previously in the capacity of 22 add to 2.1 l/day IEA.

The product of the average of column 11 (16,433 t/h) are separated in the sedimentation tank 26 into two phases. The aqueous phase (to 4.4 t/h) is directed into the upper section of the column 20 for Fri first heat exchanger 9, and then down the column 11 in the form of steam.

Aromatic extract 12,033 t/h (100 wt.), containing, t/h (wt. ): benzene 4,53 (37,65), toluene 6,98 (58,01), xylenes 0,512 (4,25), nonaromatic hydrocarbons 0,11 (0,09), is directed into the upper section of the column 20, and then split it into individual aromatic hydrocarbons.

From the extract by distillation get a 4.53 t/h of benzene, 6,98 t/h of toluene and 0,516 t/h xylene fraction. In commodity products benzene and toluene have much higher quality. The crystallization temperature of the benzene 5,41oC. the Content of non-aromatic hydrocarbons to 0.12 wt. and in toluene 0,11% wt

The degree of extraction of aromatic hydrocarbons from the potential of their content in raw materials extraction amounted to benzene 100,0, toluene 98,3, xylenes 88,3 wt.

From the bottom of column 11 assign 260,0 t/h of water TAG above composition and then served in the upper part of the extractor. A small amount of water TAG (0.5 to 2 wt. from its load in the system) served in the cube 33, where it is distilled under a residual pressure of 20 mm RT.article Distilled under vacuum, water TAG, assign to the collector 35, and then return to the stream of circulating extract 2.

With a bottom in which Genie.

Main indicators of the proposed allocation of aromatic hydrocarbons according to examples 1-7 are presented in the table.

The proposed method can significantly reduce the energy consumption: the total distillate water column separation of the extract phase 11 is reduced by 16 to 36% and including a sharp pair for 12-24% in Addition, reduced by the circulation of risaykl on 10-28% Increases the extraction of aromatic hydrocarbons in the extraction step, thereby reducing their losses with flue raffinate at 15-53% (i.e., 1.3-2 times). Simultaneously can be improved and their quality. Thus, in example 7, along with the savings in energy costs of the process, the content of non-aromatic impurities in benzene and toluene decreased 1.6-2 times. If not ask to save energy when you use this method, you can achieve an even higher quality aromatic hydrocarbons (compared to that shown in example 7).

This method can be applied to the extraction facilities petroleum refining and coking industry.

The method of separation of aromatic hydrocarbons from mixtures thereof with non-aromatic by solvent extraction with an aqueous solution of polyglycol in prisutstvie is an extract, the risaykl, water polyglycol with subsequent separation from the risaykl and extract the aqueous layer, the return of risaykl on the extraction, separation of the aqueous polyglycol into two parts with the direction of one of them on the extraction and the other for regeneration polyglycol, water washing rafinate phase and extract with getting washed out of the raffinate and extract and wash water, distillation of the washed extract individual aromatic hydrocarbons, a feed water layer on the rectification extract phase comprising 40 to 100 wt. the water layer separated from the risaykl, water washing, the direction of wash water in liquid extraction, the flow of monoethanolamine in water layer separated from the risaykl and/or the washing water directed to liquid extraction, characterized in that the water layer is separated from the risaykl, use only for water washing rafinate phase and the resulting wash water is directed to a liquid extraction of raw materials and/or risaykl, and washing of the extract are water layer separated from the extract, and the resulting wash water is fed to the rectification of the extract phase.

 

Same patents:

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The invention relates to the production of aromatic hydrocarbons

FIELD: petrochemical processes.

SUBSTANCE: simultaneous dehydrogenation of mixture containing alkyl and alkylaromatic hydrocarbons is followed by separating thus obtained dehydrogenated alkyl hydrocarbon and recycling it to alkylation unit. Dehydrogenation reactor-regenerator employs C2-C5-alkyl hydrocarbon as catalyst-transportation carrying medium.

EFFECT: increased process flexibility and extended choice of catalysts.

36 cl

FIELD: organic synthesis catalysts.

SUBSTANCE: invention relates to catalyst for aromatization of alkanes, to a method of preparation thereof, and to aromatization of alkanes having from two to six carbon atoms in the molecule. Hydrocarbon aromatization method consists in that (a) C2-C6-alkane is brought into contact with at least one catalyst containing platinum supported by aluminum/silicon/germanium zeolite; and (b) aromatization product is isolated. Synthesis of above catalyst comprises following steps: (a) providing aluminum/silicon/germanium zeolite; (b) depositing platinum onto zeolite; (c) calcining zeolite. Hydrocarbon aromatization catalyst contains microporous aluminum/silicon/germanium zeolite and platinum deposited thereon. Invention further describes a method for preliminary treatment of hydrocarbon aromatization catalyst comprising following steps: (a) providing aluminum/silicon/germanium zeolite whereon platinum is deposited; (b) treating zeolite with hydrogen; (c) treating zeolite with sulfur compound; and (d) retreating zeolite with hydrogen.

EFFECT: increased and stabilized catalyst activity.

26 cl, 1 dwg, 5 tbl, 4 cl

FIELD: CHEMISTRY.

SUBSTANCE: zeolite catalyst for process of conversion of straight-run gasoline to high-octane number component is described. The said catalyst contains high-silica zeolite with SiO2/Al2O3=60 and residual content of Na2О of 0.02 wt.% maximum, metal-modified, Pt, Ni, Zn or Fe metals being in nanopowder form. Content of the said metals in the catalyst is 1.5 wt.% maximum. Method to manufacture zeolite catalyst for conversion of straight-run gasoline to high-octane number component is described. The said method implies metal modification of zeolite, Pt, Ni, Zn or Fe metals being added to zeolite as nanopowders, produced by electric explosion of metal wire in argon, by dry pebble mixing in air at room temperature. Method to convert straight-run gasoline using the said catalyst is also described.

EFFECT: increase in catalyst activity and gasoline octane number, accompanied by increase in yield.

4 cl, 3 tbl, 4 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.

EFFECT: longer working transformation cycle due to the continuous process scheme; higher yearly output of aromatic hydrocarbons; reduced energy capacity and improved ecology of the process.

2 ex

FIELD: chemistry.

SUBSTANCE: invention describes zeolite-containing catalyst for transformation of aliphatic hydrocarbons C2-C12 to a mix of aromatic hydrocarbons or high-octane gasoline component containing zeolite ZSM-5 with silicate module SiO2/Al2O3=60-80 mol/mol and 0.02-0.05 wt % of residual sodium oxide content, zeolite structural element, promoter and binding component, with zirconium or zirconium and nickel oxides as zeolite structural component, and zinc oxide as promoter, at the following component ratio (wt %): zeolite 65.00-80.00; ZrO2 1.59-4.00; NiO 0-1.00; ZnO 0-5.00; Na2O 0.02-0.05, the rest being binding component. Also, a method for obtaining zeolite-containing catalyst is described, which involves mixing reagents, hydrothermal synthesis, flushing, drying and calcinations of sediment. The reaction mix of water solutions of aluminum, zirconium and nickel salts, sodium hydroxide, silicagel and/or aqueous silicate acid, inoculating zeolite crystals with ZSM-5 structure in Na or H-form, and structure-former, such as n-butanol, is placed in an autoclave, where hydrothermal synthesis is performed at 160-190°C for 10-20 hours with continuous stirring; the hydrothermal synthesis over, Na-form pulp of the zeolite is filtered; the obtained sediment is flushed with domestic water and transferred to salt ion exchange by processing by water ammonium chloride solution with heating and stirring of the pulp; the pulp obtained from salt ion exchange is filtered and flushed with demineralised water with residual sodium oxide content of 0.02-0.05 wt % on the basis of dried and calcinated product; flushed sediment of ammonium zeolite form proceeds to zinc promoter introduction and preparation of catalyst mass by mixing of ammonium zeolite form modified by zinc and active aluminum hydroxide; obtained catalyst mass is extruded and granulated; the granules are dried at 100-110°C and calcinated at 550-650°C; calcinated granules of zeolite-containing catalyst are sorted, ready fraction of zeolite-containing catalyst is separated, while the granule fraction under 2.5 mm is milled into homogenous powder and returned to the stage of catalyst mass preparation. The invention also describes method of transformation of aliphatic hydrocarbons to high-octane gasoline component or a mix of aromatic hydrocarbons (variants), involving heating and passing raw material (gasoline oil fraction direct sublimation vapours or gas mix of saturated C2-C4 hydrocarbons) through stationary layer of the aforesaid catalyst.

EFFECT: reduced number of components and synthesis stages of zeolite-containing catalyst; increased transformation degree of raw material; improved quality and yield of target products with the said catalyst.

4 cl, 8 tbl, 12 ex

FIELD: chemistry.

SUBSTANCE: alkylbenzol with structure R1R2CH(Ph) is obtained from alkylphenyl alcohol with structure R1R2C(Ph)OH. Method includes following stages: (a) supply of initial flow, containing alkylphenyl alcohol with structure R1R2C(Ph)OH, into reactor with catalytic distillation zone; (b) simultaneously in reactor: (i) contacting of initial flow, containing R1R2C(Ph)OH, with hydrogen in catalytic distillation zone in order to convert R1R2C(Ph)OH into R1R2CH(Ph) and to form reaction mixture and (ii) separation of R1R2CH(Ph) from reaction mixture by fraction distillation in order to obtain higher than catalytic distillation zone, flow, which contains R1R2CH(Ph) with lower concentration of R1R2C(Ph)OH in comparison to initial reactor flow in position higher than catalytic reaction zone; R1 and R2 each represent hydrogen or hydrocarbon group with 1-10 carbon atoms and one of R1 and R2 is not hydrogen.

EFFECT: more pure alkylbenzol with smaller amount of undesirable by-products and using smaller number of stages.

6 cl, 5 tbl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention refers to the method for preparation of aromatic hydrocarbons accompanied with simultaneous obtaining of hydrogen, methanol, motor oils and fresh water from the unstable hydrocarbon gas condensate obtained from gas condensate and oil fields including if necessary its desulphurisation, following obtaining of synthesis gas by one-stage oxidising with air oxygen, its conversion to methanol, following catalytic conversion of methanol to motor oils, separation of the water formed on all process stages, evaporation of the hydrocarbons residues including methanol and fatty hydrocarbons from the water (united and formed on all process stages), water bioremediation and mineralisation. The initial hydrocarbon gas is unstable hydrocarbon gas condensate without preliminary separation of methane and ethane from propane and butane, the said initial gas before its conversion to synthesis gas undergoes the catalytic aromatisation during heating. Then the obtained aromatic hydrocarbon and hydrogen are separated, hydrogen is at least partially used for synthesis gas obtaining in order to change the ratio H2:CO 1.8-2.3:1), and if necessary it is partially used on the stage of desulphurisation with synthesis gas obtaining from hydrocarbon gases (unreacted and formed on the aromatisation stage). The invention refers also to the device for implementation of the method described above.

EFFECT: increasing of the processing of the efficiency of unstable hydrocarbon gas condensate with enhanced obtaining of target products, to make the process more environmentally safe, to increase the quantity and quality of the obtained fresh water.

2 cl, 5 ex, 1 dwg

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