Method of preparing benzene and debenzenized high-octane blend

FIELD: petroleum processing and petrochemistry.

SUBSTANCE: catalysate of reforming of long gasoline fractions containing more than 2% benzene is separated by rectification into three fractions: light-boiling fraction containing mainly nonaromatic C4-C6-hydrocarbons and no more than 1%, preferably no more than 0.5%, benzene; high-boiling fraction containing mainly aromatic and nonaromatic hydrocarbons C7 or higher and no more than 1%, preferably no more than 0.5%, benzene; and benzene fraction boiling within a range of 70-95°C and containing no more than 0.1%, preferably no more than 0.02%, toluene and no more than 0.02% nonaromatic hydrocarbons with boiling temperature above 110°C. Benzene fraction is routed into benzene isolation process involving extractive rectification with polar aprotic solvent having ratio of dipole moment to square root of molar volume above 0.3 db/(cm3/g-mole)1/2, preferably above 0.4 db/(cm3/g-mole)1/2, and boiling temperature 150 to 250°C.

EFFECT: improved quality of benzene.

4 dwg, 2 tbl, 5 ex

 

The invention relates to the field of production of benzene and high-octane mixtures.

More specifically the invention relates to the field of production of benzene and dibenzocrown high-octane hydrocarbon mixture from catalyzate reforming wide gasoline fractions.

One of the areas for improvement of the ecological state of the environment worldwide is the translation of the car Park on gasoline with improved characteristics, which sets forth limits on the content of individual components when compounding. In particular, the European community has established maximum limits for the content of carcinogenic benzene in gasoline Euro-3, Euro-4 and Euro-5 not more than 1% of the mass.

In Russia prospective requirements for gasoline evolve in a similar direction. The production of gasoline with a high, in particular, the content of benzene and now lowers their demand and cost when selling abroad.

The research work of a number of domestic catalytic reforming units wide gasoline fractions, wikipaedia within 62-180°, 70-180°and 85-180° (Listokin GA and other "lessons learned from the design and development of catalytic reforming units". Browse M., Tsniiteneftehim, 1979, 28 C.), showed that the content of carcinogenic gasoline katalysator reformin is and ranges from 2 to 10 wt% depending on the applied pressure, the temperature of the reforming catalyst. Raising the boiling point of the feedstock for catalytic reforming to reduce the formation of benzene leads to a narrowing of the raw material base for the production of gasoline, as well as to receive catalization, have often overestimated in comparison with the requirements of GOST temperature that meets the 10 and 50%to the remote sites, so that for the preparation of commercial gasoline have to add a significant amount of expensive low-boiling high octane components. Regulation mode reforming (lower temperature, higher pressure) usually results not only in decreased concentrations of benzene, but also to reduce the octane number catalyzate.

Modern world science and practice suggests several ways to reduce the benzene content in catalyzate reforming, most of which involves preliminary fractionation catalyzate emitting light reformate with a high content of benzene. The benzene contained in the reformate can be providerone (RF patent 2228948, class C 10 G 59/02, op. 20.05.2004,), or proaccelerin light olefins (RF Patent 2186829, class C 10 G 50/00, op. 10.08.2002, or provided as a commercial product by combining methods of rectification with extraction (Patent RF 2194740, class C 10 G 35/085, op. 20.12.2002, or extractive distillation (Patent RF 2153485, CL 07 C7/08, op. 27.07.2000 year). Methods based on the selection, allow, along with the reduction of benzene content in the gasoline fraction, in addition to obtain valuable target product is benzene having a high cost of production volumes which do not satisfy the growing needs of the market.

The closest to the technical nature of the claimed method is a method (Patent RF 2153485, CL 7/08 C 07 C, op. 27.07.2000 g) the production of benzene and dibenzocrown high-octane mixture of hydrocarbon mixtures containing at least an aromatic and nonaromatic hydrocarbons having six or more carbon atoms, according to which the initial mixture is separated by distillation at CBM product containing not more than 3 wt%, preferably not more than 1% of the mass of benzene, and the distillate containing mainly hydrocarbons With6in which not more than 5 wt%, preferably not more than 0.5 wt%, toluene and no more than 36,6% of the mass, preferably not more than 10 wt%, hydrocarbon, C7which is subjected to extractive distillation in the presence of a polar, organic, aprotic solvent having a ratio of the dipole moment to the square root of the molar volume of more than 0.3 dB/(cm3/g·mol1/2preferably more than 0.4 dB/(cm3/g·mol1/2and the boiling temperature of 150-250°s as SW is late output stream, mainly containing non-aromatic hydrocarbons With6-C8that may unite with kubovy product of rectification, as well as the cubic product is a mixture of the indicated solvent with the hydrocarbon from which further distilled stream containing mainly benzene, which can be further subjected to further distillation of hydrocarbons with higher boiling points.

The known method has significant disadvantages when used for the production of benzene and dibenzocrown high-octane mixture of catalyzate reforming wide gasoline fractions, the main ones are:

- low degree of extraction of benzene from catalyzate reforming wide gasoline fractions, because when the content of benzene in catalyzate reforming wide gasoline fractions from 2 to 10% of the mass residual content in the bottom product of the rectification column is allowed up to 3% of the mass;

a significant number of permissible content of toluene in the distillate the rectification column (from 0.5 to 5% of the mass). The boiling point of toluene 110°and when it is extracted in significant quantities in the composition of the distillate with him to retrieve the non-aromatic hydrocarbons With7with close to toluene boiling point. The presence of such non-aromatic hydrocarbons is W in the power of the column extractive distillation significantly complicates the problem of allocation of benzene of high purity (>99.5% of the mass), leading to the need to increase the efficiency of the extractive distillation column, reflux ratio and circulation of the extractant and, ultimately, to increase the capital cost and power consumption. In addition, if permissible in the known method the content of toluene in the distillate mandatory condition for obtaining benzene of high purity is rectification of desorbed benzene extracted with him toluene, the presence of which also complicates the conditions of desorption of hydrocarbons from saturated solvent;

- separation of catalyzate reforming wide gasoline fractions containing from 2 to 10% of the mass of benzene and having a source of octane number on the research method 92-94, two factions allows you to get as dibenzopyrans high-octane mixture only CBM product of rectification. Adding the entire amount of the distillate of the column extractive distillation reduces the octane number as compared with the initial octane number catalyzate reforming wide gasoline fractions by 1-2 points. The use of distillate column extractive distillation as feedstock for catalytic reforming units without additional rectification is impossible due to the low temperature of the beginning of the boil.

The present invention is the reduction of the of atrat of power when receiving dibenzopyrans high-octane mixture, meet the future requirements on the content of benzene while enhancing the quality of benzene emitted as a commercial product.

This result is achieved by a method of producing benzene and dibenzocrown high-octane mixture of catalyzate reforming wide gasoline fractions containing more than 2% of the mass of benzene, by separation by distillation and extractive distillation with a polar, aprotic solvent having a ratio of the dipole moment to the square root of the molar volume of more than 0.3 dB/(cm3/g·mol1/2preferably more than 0.4 dB/(cm3/g·mol1/2and a boiling point of from 150 to 250°in which the reforming catalysate separated by distillation into three fractions: boiling fraction containing mainly non-aromatic hydrocarbons With4-C6and not more than 1%, preferably not more than 0.5% of the mass of benzene, tagalakis fraction containing mainly aromatic and nonaromatic hydrocarbons With7and above and less than 1%, preferably not more than 0.5% of the mass of benzene, and the benzene fraction, wikipaedia within 70-95°and containing toluene - not more than 0.1 wt%, preferably not more than 0.02 wt%, of non-aromatic hydrocarbons with a boiling point of more than 110° - not more than 0.02 wt%, which is sent on vudelayaetsya extractive rectification.

There is a separation of catalyzate reformer to carry out rectification in the same column with the selection boiling fraction as a distillate, taglocity faction as the cubic product and benzene fraction as a side selection from a point above the point of supply.

The effectiveness of the zone located between the input power supply in a rectification column and a side selection of benzene fraction, can be from 5 to 20 (preferably from 10 to 15 theoretical plates.

It is also possible boiling fraction to combine with taglocity faction with getting dibenzopyrans high-octane mixture. The distillate of the column extractive distillation has the lowest octane number of the selected fractions and it is better to use as feedstock in catalytic reforming units, that does not preclude its use in the compounding of gasoline with the additional use of high-octane components.

The process of the production of benzene and dibenzocrown high-octane mixture of catalyzate reforming wide gasoline fractions containing more than 2% of the mass of benzene, according to the proposed method allows to achieve a significant reduction in cost of power expense:

- separation from benzene fraction boiling fraction, which contains Asa mainly nonaromatic hydrocarbons With 4-C6before sending benzene fraction to extractive distillation;

- determine the optimal limits of the content of benzene fraction of toluene and non-aromatic hydrocarbons with a boiling point of more than 110°With, in the most affecting terms of extractive distillation, which allows to obtain a benzene of high purity;

- preferred separation catalyzate reforming wide gasoline fractions containing more than 2% of the mass of benzene, into three fractions in a single column. In this case, the simplified process scheme for up to three columns and possibly optimal use of the power spent in the first column in the selection side product and directing it into the extractive distillation column in the vapor phase.

The use of the method is illustrated by the following drawings and examples. See the drawings and the examples do not exhaust all of the options for implementing the method, and any other technological solutions, while respecting the essence of the invention set forth in the claims.

According to figure 1 of the original hydrocarbon mixture F served in the distillation column 1. On top of the column 1 deduce boiling fraction D1containing mainly non-aromatic hydrocarbons With4-C6. CBM product W1column 1 serves in rivers is ification column 2. From the cube column 2 select tagalakis fraction of W2containing mainly aromatic and nonaromatic hydrocarbons With7and above. On top of the column 2 remove the benzene fraction of D2that is directed to the separation in the extractive distillation column 3. In the upper part of the column 3 serves desorbed extractant W4. From the top of column 3 are selected fraction of D3containing mainly non-aromatic hydrocarbon With6-C7. From the cube column 3 rich extractant W3sent to the desorption column 4. From the top of column 4 are selected commodity benzene D4. From the cube column 4 desorbed extractant W4return to the extractive distillation column 3.

According to figure 2 of the original hydrocarbon mixture F served in the distillation column 1. On top of the column 1 display the fraction of D1containing mainly non-aromatic hydrocarbons With4-C7and benzene. From the cube columns 1 select tagalakis fraction of W1containing mainly aromatic and nonaromatic hydrocarbons With7and above. On top of the column 2 deduce boiling fraction D2containing mainly non-aromatic hydrocarbons With4-C6. From the cube column 2 select the benzene fraction of W2that is directed to the separation in the extractive distillation column 3. In the top part of the column 3 serves desorbed extractant W 4. From the top of column 3 are selected fraction of D3containing mainly non-aromatic hydrocarbons With6-C7. From the cube column 3 rich extractant W3sent to the desorption column 4. From the top of column 4 are selected commodity benzene D4. From the cube column 4 desorbed extractant W4return to the extractive distillation column 3.

According to figure 3 of the original hydrocarbon mixture F served in the distillation column 1. On top of the column 1 deduce boiling fraction D1containing mainly non-aromatic hydrocarbons With4-C6. From the cube columns 1 select tagalakis fraction of W1containing mainly aromatic and nonaromatic hydrocarbons, C7and above. Side selection from a point lying above the point of supply to the column 1, remove the benzene fraction BO, which is directed to the separation in the extractive distillation column 3. In the upper part of the column 3 serves desorbed extractant W4. From the top of column 3 are selected fraction of D3containing mainly non-aromatic hydrocarbons With6-C7. From the cube column 3 rich extractant W3sent to the desorption column 4. From the top of column 4 are selected commodity benzene D4. From the cube column 4 desorbed extractant W4return to the extractive column the rectification 3.

In order to save heat required for the separation, and/or enable optimal heat recovery column can operate at different pressure side selection can be selected in the vapor or in the liquid phase. To reduce the boiling point of the extracting agent can be used mixed extractants, including extractants containing water. To reduce entrainment of extractants from hydrocarbon streams may be used any known methods.

Figure 4 shows a diagram of the process in accordance with the prototype. According to figure 4 of the original hydrocarbon mixture F served in the distillation column 1. On top of the column 1 display the fraction of D1containing mainly non-aromatic hydrocarbons With4-C7and benzene, which is directed to the separation in the extractive distillation column 3. From the cube columns 1 select tagalakis fraction of W1containing mainly aromatic and nonaromatic hydrocarbons, C7and above. In the upper part of the column 3 serves desorbed extractant W4. From the top of column 3 are selected fraction of D3containing mainly non-aromatic hydrocarbons With4-C7. From the cube column 3 rich extractant W3sent to the desorption column 4. From the top of column 4 select the benzene D4that addi is entrusted cleaned toluene and taglocity hydrocarbons in column 5. From the cube column 4 desorbed extractant W4return to the extractive distillation column 3. Commodity benzene D5taken from the top of the column 5. From the cube column 5 select a mixture of benzene with toluene and magelonidae hydrocarbons W5.

Examples illustrating the use of the invention, are given in table 1 and table 2. The source of the reforming catalysate had an octane number according to research method 94.

In example 1 as the polar solvent used is N,N-dimethylacetamide, with respect to the dipole moment to the square root of the molar amount equal to 0.39 dB/(cm3/g·mol1/2the steam consumption was 0,32 t/t catalyzate reforming, cooling water flow rate was 8.9 m3/t catalyzate reforming. Mixing D1and W2got 0,84 tons of high-octane dibenzopyrans mixture having the octane number on the research method 96,2.

In example 2, as the polar solvent used is N-formylmorpholine relevant dipole moment to the square root of the molar amount equal 0,41 dB/(cm3/g·mol1/2the steam flow rate was 0.33 t/t catalyzate reforming, cooling water consumption amounted to 9 m3/t catalyzate reforming. Mixing D2and W1got 0,88 t high-octane dibenzopyrans mixture, and eUSA octane number by the research method is 95.6.

In example 3, as the polar solvent used methoxypropionitrile relevant dipole moment to the square root of the molar amount equal to at 0.42 dB/(cm3/g·mol1/2the steam consumption was 0,31 t/t catalyzate reforming, cooling water consumption was 8.7 m3/g catalyzate reforming. Mixing D1and W2got 0,84 tons of high-octane dibenzopyrans mixture having the octane number on the research method 96,2.

In example 4, as the polar solvent used N is the organic relation of the dipole moment to the square root of the molar amount equal to at 0.42 dB/(cm3/g·mol1/2the steam consumption amounted to 0.28 t/t catalyzate reforming, cooling water consumption was 5.8 m3/t catalyzate reforming. Mixing D1and W1got 0,81 tons of high-octane dibenzopyrans mixture having the octane number on the research method 96,5.

In example 5, taken for comparison, as the polar solvent used is N,N-dimethylacetamide, with respect to the dipole moment to the square root of the molar amount equal to 0.39 dB/(cm3/g·mol1/2the steam consumption amounted to 0.35 t/t catalyzate reforming, cooling water consumption amounted to 9.3 m3/t catalyzate reform the ha The result was 0.65 t high-octane dibenzopyrans mixture of W1having the octane number on the research method of 98.2. The mixture of W1with D2gives 0.96 tons of a mixture having the octane number on the research method 92.

25
Table 1
Components and parametersExample 1 (1)Example 2 (2)Example 3 (1)
FD1D2W2D3D4W1D2W2D3D4D1D2W2D3D4
Composition, wt%:
hydrocarbons, C2-C46,234,4328,1034,43
hydrocarbons, C58,741,917,109,5438,192,303,5341,917,10at 9.53
nah612,223,3049,3266,2732,7141,7063,9623,3049,3266,20
nah710,017,8510,8023,990,1711,3521,0032,210,2617,8510,8023,970,10
nah8+4,36,69to 6.676,69
including carbohydrates with tKip.>110°C0,0020,0010,002
benzene4,60,3625,720,550,2099,790,301,0034,990,3099,710,3625,720,550,3099,88
toluene18,10,0127,520,0427,430,010,030,0127,520,02
xylenes and ethylbenzene+35,954,4454,2554,44
the polar solvent
Flow, t/t F1,00,180,160,660,120,040,660,220,120,080,040,180,160,660,120,04
The flow of the polar solvent in the extractive distillation column, t/t benzene5,36,05,0
(N.N-dimethylacetamide)(N-formylmorpholine +2,5% H2O)(methoxypropionitrile)
Column 1:
the number of theoretical plates2525
reflux number20,82
Column 2:
the number of theoretical plates353535
reflux number31,53
Column 3:
the number of theoretical plates303030
reflux number111
Column 4:
the number of theoretical plates202020
reflux number1,0 0,40,8

41,64
Table 2.
Components and parametersExample 4 (3)Example 5 (4)
FD1BOW1D3D4W1D1D3D4D5
Composition, wt%:
hydrocarbons, C2-C46,232,988,30of 10.5817,7420,19
hydrocarbons, C58,735,3419,6024,9824,8928,33
nah612,230,1053,060,4034,1638,88
nah710,08,9212,4011,360,149,5210,90KZT 12.390,130,11
non-aromatic C8+4,3to 6.586,76
including carbohydrates with tKip>110°0,0030,0120,020,01
benzene4,61,5821,520,370,0299,790,5112,210,2199,0599,69
toluene18,10,0227,080,0727,770,100,820,20
xylenes and ethylbenzene+35,953,5755,04
the polar solvent
Flow, t/t F1,00,140,190,670,150,040,650,350,310,040,04
The flow of the polar solvent in the extractive distillation column, t/t benzene7,013,0
(N,organic(N,N-dimethylacetamide)
Column 1:
the number of theoretical plates3535
reflux number30,6
Column 3:
the number of theoretical plates3030
reflux number11,0
Column 4:
the number of theoretical plates2020
reflux number0,56,3
Column 5:
the number of theoretical plates-20
reflux number-0,2

1. A method of producing benzene and dibenzocrown high-octane mixture of catalyzate reforming wide gasoline fractions containing more than 2 wt.% benzene, by separation by distillation and extractive distillation with a polar, aprotic solvent having a ratio of the dipole moment to the square root of the molar volume of more than 0.3 dB/(cm3/g·mol1/2preferably more than 0.4 dB/(cm3/g·mol1/2and a boiling point of from 150 to 250°With, trichosis fact, the reforming catalysate separated by distillation into three fractions: boiling fraction containing mainly non-aromatic hydrocarbons With4-C6and not more than 1%, preferably not more than 0.5 wt.% benzene, tagalakis fraction containing mainly aromatic and nonaromatic hydrocarbons, C7and above and less than 1%, preferably not more than 0.5 wt.% benzene, and the benzene fraction, wikipaedia within 70-95°and containing toluene - not more than 0.1 wt.%, preferably not more than 0.02 wt.%, non-aromatic hydrocarbons with a boiling point of more than 110° - not more than 0.02 wt.%, which is directed to the selection of benzene extractive distillation.

2. The method according to claim 1, characterized in that the separation catalyzate reforming the rectification is carried out in the same column with the selection boiling fraction as a distillate, taglocity faction as the cubic product and benzene fraction as a side selection from a point above the point of supply.

3. The method according to claim 2, characterized in that the effectiveness of the zone located between the input power supply in a rectification column and a side selection of benzene fraction is from 5 to 20 (preferably from 10 to 15 theoretical plates.

4. The method according to claim 1 or 2, characterized in that boiling fraction combined with taglocity what Roccia obtaining dibenzopyrans high-octane mixture.



 

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SUBSTANCE: invention relates to chemical processing of petroleum products, notably to the process of producing o-xylene concentrate, high-octane gasoline component with improved environmental characteristics, commercial benzene and toluene from petroleum and gas-condensate feedstock. According to invention, gasoline reforming catalysate is subjected to fractionation on two rectification columns. Top product of the first column is benzene-toluene fraction with output ensuring potential production of sum of ethylbenzene and m- and p-xylenes in the top product equal to 10-45%. Side product is toluene-xylene fraction with output ensuring potential production of toluene in the side product equal to 5-30%. Bottom residue is fraction of aromatic hydrocarbons C9 and higher. Side product bleeding point in the column is selected such that temperature difference between column bottom and this point were within a range of 30-70°C. Benzene-toluene fraction from the first column top is fed into the second rectification column operated under excess pressure 2-5 kg/cm2. Top product of the second column is pre-benzene fraction with output ensuring potential production of non-aromatic C3-C6-hydrocarbons in the top product equal to 65-95%. Side product is benzene concentrate with output ensuring potential production of non-aromatic C7-C8-hydrocarbons in the side product equal to 30-65%. Bottom residue is toluene-xylene fraction. Side product bleeding point is selected such that temperature difference between side bleeding and column top were within a range of 35-75°C. Bottom product of the first column is combined with distillate and bottom residue of the second column thus producing high-octane gasoline component with improved environmental characteristics. Side distillates of the two columns are combined with benzene-toluene reforming catalysate and thus obtained product is consecutively subjected to hydrogenation, extraction with solvent refining agent to form extract, wherefrom commercial benzene, toluene, and o-xylene concentrate are recovered.

EFFECT: enlarged assortment of products, increased production of commercial benzene and toluene meeting State Standard requirements and also high-octane gasoline component with improved environmental characteristics.

2 cl, 15 ex

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