• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
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  • 法律状态
  • 优先权
    • 专利摘要:
    A method for the removal of aromatic hydrocarbon from mixtures containing non-aromatic hydrocarbon by liquid-liquid extraction and extractive distillation is described. Isoenthalpic expansion of the rectification column bottom solvent stream and addition of water to the selective solvent can be used to reduce heat consumption.
    公开号:SU973016A3
    申请号:SU782648852
    申请日:1978-08-09
    公开日:1982-11-07
    发明作者:Монтанари Ромоло；Антонелли Серджо
    申请人:Снампрогетти С.П.А. (Фирма)；
    IPC主号:
    专利说明:

    (5) METHOD FOR ISOLATION OF AROMATIC HYDROCARBONS FROM THEIR MIXTURES WITH NONAROMATIC
    one
    The invention relates to a process for the isolation of aromatic hydrocarbons — mixtures of benzene, toluene, xylenes and Ca aromatic hydrocarbons — from their mixtures with a non-aromatic g combination of solvent extraction and extractive rectification. .
    Methods are known for the separation of aromatic hydrocarbons from their mixtures with non-aromatic by liquid extraction, followed by extractive distillation. At the same time, at the stages of solvent extraction and extractive distillation a high boiling selective solvent is used, and in a mixture with water. The most suitable for these processes are solvents such as morpholine, alkyl and keto-derivatives of morpholine or their mixtures 1 and 2., 20
    The closest to the proposed technical essence and the achieved result is the method of separation of aromatic hydrocarbons from their mixtures with non-aromatic 25
    by two-stage solvent extraction with water-containing N-formylmorpholine.
    The extract withdrawn from the second cTiyneHM is directed to an extractive distillation.  The resulting extractive distillation distilled by two-stage condensation is divided into a higher boiling fraction, which is returned to the first stage of extraction in the zone between the points of entry of the solvent and the raw material, and the fraction with a lower boiling point.  This fraction is injected into a cube by the extraction stage.  VAT residue extractive distillation is subjected to rectification in the presence of water.  The distilled blend of aromatic hydrocarbons and water is separated in a separator.  The separated water is divided into several streams, one of which is returned to the rectification stage as reflux, and the other is fed into the cube of the rectification column. Part of the separated water from the separator is fed to the washing of the raffinate recovered at the first stage of extraction.  Wash water is then sent to the cube of the second stage of extraction. The solvent collected in the bottom residue is returned to the extraction stage.  According to this method, N-formylmorpholine containing up to 30 ppm of water is used. At the first and second stages of extraction, the temperature is maintained at 0-90 ° C. Extractive rectification is carried out at 30-ZOO C, the solvent is distilled off in a distillation column at 50%. 200 N Z.  The disadvantage of this method is the considerable energy consumption for the process associated with greater heat consumption at the stages of extractive rectification and stripping; Thus, after stripping, the solvent returned to the extraction can contain up to 3-5% of water and should contain traces of aromatic hydrocarbons.  The above disadvantage generally increases the cost of the known method. The purpose of the invention is to reduce energy costs. The goal is achieved by the fact that according to the method of separation of aromatic hydrocarbons from their mixtures with non-aromatic and two-step liquid. extraction with a water-containing N-formylmorpholine as a selective solvent to obtain an extract and raffinate and then feeding the extract to an extractive rectification with separation of the distillate obtained by two-step condensation into more.  high boiling fraction returned to the first stage of extraction in the zone between the solvent and the feedstock input points J and the fraction with a lower boiling point returned to the cube of the second stage of extraction, and rectification1: {iy bottoms extractive distillation in the presence of water with distillate bleeding those mixtures of aromatic hydrocarbons with water and separation of the latter into aromatic hydrocarbons and water-, which is returned as a fryugm to the rectification stage and fed to the opening of the resulting raffinate, with blowing the washing water inlet in cubic second extraction stage, and collecting the solvent in the distillation bottoms, the latter keeps so9 3 wt. % water and 2-k weight,% aromatic hydrocarbons, and it is subjected to isenthal expansion to a residual pressure tO160 mm Hg, st.  with the selection of a liquid solvent stream containing 0,, 9 weight.  water and 0.79-2, by weight of aromatic hydrocarbons returned to the first stage of extraction, and a vaporous solvent stream enriched in water and aromatic hydrocarbons, which is subjected to condensation, followed by mixing 4p-80 weight, the resulting condensate with the extract taken from the extraction stage before it is fed to the extractive distillation stage and the remainder of the condensate is fed into the cube of the second stage of extraction.  The extraction is preferably carried out at 15-100 ° C.  Extractive distillation and rectification is preferably carried out at 5P-1bP ° Co. The drawing shows the scheme of the method.  The initial mixture of hydrocarbons is directed through the main line 1 to the lower part of the extractor 2 of the first stage to extract the liquid with a liquid, where countercurrent contact of the mixture to be separated with a stream of solvent is made, which is directed to the upper part of this extractor through line 3.  From the top of the extractor 2, the raffinate is withdrawn, which is sent along line k to the scrubber column 5. This allows to remove all traces of the solvent taken from the raffinate by washing with water under countercurrent conditions. From the top of the column 5, a raffinate freed from the solvent, and through line 6 it is withdrawn from the system. Water, which is recovered from the bottom of column 5, is sent through line 7 to the lower part of the second stage extractor 8 for liquid extraction with liquid. Solvent enriched with aromatic hydrocarbons taken from the lower part of the extractor 2, through line 9 are fed to the upper plate of the extractor 8, and from the upper plate of the extractor 8, the obtained raffinate is fed through line 10 to the lower part of the extractor 2.  This allows recovery of that part 59 of aromatic hydrocarbons, which is still contained in the raffinate,. By the corresponding lines 7 and 11, in the lower honor of the extractor 8, the washing water discharged from the scrubber column 5 after washing the raffinate is fed, and the stream, which consists of hydrocarbons and water obtained in the condenser 12 of the second stage of the condensation of the column 13 of the extractive distillation. The optimum water content in the cube of the extractor 8 is maintained by feeding along part of the stream 15 of the stream 15 obtained by condensation in the condenser 16 from Qdim from the separator 17 vapor phase solvent obtained after isenthalpic expansion of this stream contains primarily water with a small amount of solvent and aromatics.  The extract discharged from the bottom of the extractor 8 through line 18 is sent to a heat exchanger 19, in which it is heated by indirect heat exchange with a solvent discharged from the bottom of the distillation distillation column 20 "Before the extractive distillation is introduced into the column 13, the extract supplements with a water-containing stream obtained in condenser 16, which is fed through line 21, and then the mixture is sent through line 22 to extractive distillation.  The addition of water supplied through line 21 simplifies the separation of non-aromatic hydrocarbons, thus ensuring a high degree of purity of the extract with reduced heat consumption compared with the cases when using a smaller amount of water. Since the N-formylmorpholine used is characterized by a high boiling point , the higher the water content, the lower the boiling point of the mixture.  Therefore, the addition of water causes an additional reduction in heat consumption compared to the known HZ method. In fact, after heating the bottom product of the column 13i consisting of solvent and extracted aromatic hydrocarbons, a substantial amount of heat is saved to a lower temperature, which corresponds to the temperature difference that is characteristic of different levels of content. water.  Moreover, the technical 6 "characteristic of the extractive distillation column remains unchanged.  The head straps of the column 13 are directed through line 23 first to condenser 2k for partial condensation, in which the minimum amount of water condenses along with a fraction of lower boiling aromatic hydrocarbons, high boiling saturated hydrocarbons and monoarrmatic hydrocarbons, which are characterized by anomalous polarity. facilitating their solubility in a solvent: On line 25, the condensate obtained after separation in separator 2b is directed to the appropriate level of extractor 2, supply level exceeds an therein feedstock via line 1, which simplifies the blowing of non-aromatic hydrocarbons in raffinate with anomalous polarity and prevents the accumulation of these compounds both in the course of the cycle, and any reduction in the degree extract frequency.  The vapor phase coming from the separator 26 is subjected to subsequent and complete condensation in the condenser 12, after which it is collected in the separator 27.  The resulting condensate, which consists of water, lighter-boiling aromatic hydrocarbons and low-boiling unsaturated hydrocarbons, is sent to the lower part of extractor B via line 11. Taking into account the amount of water that is added to the base of the extractor through lines 7 and H, non-aromatic The high boiling compounds contained in the extract phase are transferred to the raffinate phase due to their partial replacement in the extract phase by low boiling non-aromatic hydrocarbons.  The latter are more easily separated at the subsequent stage of extractive rectification.  The bottom product of the column 13 is fed through line 28 to a stripping distillation column 20, in which aromatic hydrocarbons are stripped in the presence of water entering the top of the column through line 29.  Discharged from the top of the column through the line 30 CMech aromatic hydrocarbons and water is sent to the condenser 31, and then to the decantation apparatus 32.  The isolated aromatic hydrocarbons are withdrawn via line 33, and the separated water is partially returned via line 29 to distillation column 20 as reflux and through line 3 is fed to the scrubber column 5 for washing the raffinate. Regenerated solvent from the bottom of column 20 is fed through line 35 to a heat exchanger 19 to preheat the extract stream directed to the extractive column 13, and then it is subjected to isenthalpic expansion to achieve a certain degree of vacuum (0-160 mm Hg) by passing through valve 36.  The vacuum depends to a certain extent on the composition of the feedstock fed to the plant, as well as on the water content in the solvent in the lower part of the stripping column 20 °. Conducting the above expansion with the flow enthalpy of flow 35, the temperature of which after heat exchange in heat exchanger 19 is such that allows its further use in the installation, causes the separation of the stream into gaseous 37 and liquid 3 streams. Stream 37 contains a significant K amount of water, in addition to the presence of solvent and aromatic hydrocarbons, while stream 3 is characterized by a significant decrease in the content of water and hydrocarbons in comparison with their content in the stream 35 ". Thus, it is possible to obtain the required stream 3 of solvent, which, thanks to the low content of water and residual hydrocarbons, makes it possible to operate the first stage extractor for liquid extraction by liquid under improved conditions, since the consumption of solvent can be reduced in comparison with its consumption in the implementation of known methods, as a result of which It consumes the body while at the same time achieving increased efficiency in the recovery of aromatic hydrocarbons.  The required stream 15 is obtained by condensation 8, condenser 16, and it is divided into streams T and 21 for use, as indicated above, in order to change the water content in the bottom of the extractor 8 for liquid extraction with liquid 8 and in column 13 of extractive distillation. the separator 17 and the condenser 16 are supported by an ejector. The vacuum depth is closely related to the need to achieve complete condensation (with the exception of non-condensing components) of stream 37, which eliminates the possibility of losses The hydrocarbon-isoenthalpic expansion of the solvent in the lower part of the stripping column is carried out to ensure that the following advantages of the proposed method are possible.  The residual content of aromatic hydrocarbons in stream 35 is much higher than their residual content in stream 3.  This is due to the tem | that in the process of isenthalpic stripping it is possible to separate part of such hydrocarbons in the vapor phase. As a result, the fractionation rate to be achieved in the aromatic hydrocarbon stripper is not so high that it can significantly reduce heat consumption.  Since the content of water and hydrocarbons in the solvent in the lower part of the stripping column is higher than in stream 3, its relative boiling point at constant pressure is lower than the boiling point of stream 3.  So p. In general, it can be used in smaller quantities, which results in a significant amount of heat saving corresponding to the difference in boiling points. possible corrosive effects, so that carbon steel can be used to make the whole installation. Since fractionation and extends less intense, it is possible to exclude the introduction of water vapor in cc stripper by evaporation of the water, which is obtained as a distillate in dekanta Zion apparatus 32.  Since the amount of heat that comes from the heap remains unchanged, reducing the flow rate of 3 distillates to the minimum in accordance with the needs of the raffinate washer allows an operation with a large reflux number, thereby reducing the amount of solvent taken .  The use of isenthalpic broadening allows to obtain a stream 15 which mainly consists of water intended for use in accordance with the needs of the installation, and to use that heat which cannot be used in other cases, while in the implementation of the known methods the water used in the plant, it is obtained by distillation of the solvent, after which it is separated from the hydrocarbons in the separators in the form of head cuts of the extractive distillation column and the column from the aromatic hydrocarbon parks.  The water content in the solvent at the extraction stage in apparatus 2 and 8 is 0.5-12% by weight, mostly 0, weight, in the first stage of extraction and 0.5-12% by weight.  on the second, the water content in the vat residue of the extractive distillation column is maintained at 3, 8 weight D, depending on the temperature of the bottom of the extractive distillation.  Example 1, the process is carried out as described above.  Separated gasoline is subjected to separation, which includes the following components, wt. %: Benzene 10 Toluene 31 Xylenes 21 Compounds with 9 carbon atoms + aromatics 3 Non-aromatic compounds 30 Specified feedstock in an amount of 100 kg / h is fed to the bottom plate of the column 2 for liquid extraction liquid This column is equipped with 60 sieve plates “In the upper part of the column 2 inlet t N-formylmorpholine (2% solution in water, the content of residual hydrocarbon components is approximately 1.2 veg. about%) in the amount of 370 kg / h.  On the 20th plate (the numbering of the plates starts from the bottom), a more heavy fraction is fed through line 25, which is obtained on the first condensation stage in the separator 26 of headstones of the cylon 13 extractive rectification in the amount of 1.5 kg / h, of which 0.25 kg / h is water.  The temperature in column 2 is maintained in the range of 50-60 ° C .; the raffinate is withdrawn from the head of column 2, which, after washing in column 5 in the amount of 31.9 kg / h, is directed outside the territory occupied by the workshop or installation.  WATER is used as wash water, which comes from decanting apparatus 32 and contains no solvent at all in an amount of 2.2 kg / h, after which it is sent to the bottom of extractor 8 for liquid extraction with liquid.  Into the cube of the extractor 8, which contains 20 sieve plates, the lighter fraction of the overhead distillation column in the amount of 28.6 kg / h is directed along the line 11, and 7 kg / h is accounted for by the water in the cube of the extractor 8 Lines H supply part of the stream obtained by condensation in the condenser 16 of the vapor stream of the separator 17 after isenthalpy expansion, in the amount of 7.8 kg / h, 3 kg / h to water and the rest to the share of hydrocarbons and solvent.  In the bottoms stream, which is removed from the extractor 8, the water concentration is 5 wt. % in terms of the total amount of the mixture, whereas the water content in terms of the solvent-water system is weight. .  Before the extractive distillation is introduced into the column 13, the bottoms stream exiting the extractor 8 is supplemented with a water-containing stream fed through line 21 in an amount of kg / h (k3% of stream 15), of which 3.2 kg / h water, the rest - on hydrocarbons and solvent.  At the bottom of the column 13, the temperature C is maintained (y ° C, and the water concentration is weight.  in terms of a mixture, which also includes aromatic hydrocarbons and a solvent, while 11 in terms of one solvent, this concentration reaches 5 ppm D Condensate, half-condensed from condenser 16, is divided into two streams T and 21, at the same time maintaining in the column of extractive distillation, the maximum concentration of water that corresponds to the required amount of it.  The bottoms stream from the extractive distillation columns is directed to a distillation column 20 for stripping aromatic hydrocarbons. As a result, stripping will result in high purity aromatic hydrocarbons.  In fact, the content of non-aromatic hydrocarbons is less than 400 hours. / 1,000,000 m.  At the same time, a high degree of recovery of aromatic hydrocarbons is achieved,%: Benzene 100 Toluene 99.8 Xylenes 97 Compounds with 9 carbon aromatic atoms. Chests 85 6 For washing the raffinate, a water phase distillate is used, which is obtained from decanting apparatus 32.  The temperature of the bottoms in column 20 is maintained at 160 ° C, and the content of residual hydrocarbons in them is 2 wt% and the water content is 3.9 wt%.  With isenthalpy expansion, a solvent is obtained, which is sent via line 3 to extractor 2, containing 1.2 wt. D of residual hydrocarbons and 2 weight of water. In the separator 17, as well as in the condenser 16, a residual pressure of 110 mm is maintained. Hg  In comparison with the cycle, which is carried out according to a known method of a GBZ, without isenthalpic expansion, heat saving in the extractive column is 18%, and in the steam distillation column - 20%.  At the same time, the purity of the aromatic hydrocarbons obtained is the same. The data on the composition of the liquid and vapor phase obtained by carrying out the process under the conditions of Example 1 at different pressures of isental expansion are presented in Table 1.
    +8.53 1.7 53.96 Water 0.9 N-formylmorpholine Benzene Toluene Xylene Aromatic g, 65 and, about 0.85
    Example 2 The process is carried out analogously to example 1, the bottom of the column 13 is maintained. The water concentration in it is maintained at a temperature of 2.5, 1.23, 5.70.
    complies with L, 7 This is achieved by recycling about O weight. of the total amount of vapor phase leaving separator 17 after 1.88-5555 2.21 57.88 6.89 21.56 96.i "2 0.11 1, 35 0i" 0.03 5.96 0.26 0.23 0.97 N, 57 1.07 U, 62
    13973016I
    cooling it in the condenser 16 in terms of the water concentration is 5 wt. D to the pipeline 21.. and the concentration of hydrocarbons is 3 weight D.
    The lower part of the distillation distillation-enthalpy expansion, shown in the column, operates at 152С s in Table 2. 2.57 T5.27 2.25 N-Formylmorph water Under these conditions, the heat consumption in the column 20 is reduced to 18.2 kcal / kg of the original raw materials, and thus provides savings in heat consumption, amounting to about 27 compared with the known method. Example 3 The process is carried out analogously to example 1. At the bottom of the extractive column 13, the temperature is maintained at 136 ° C. The water concentration at the bottom of this column is about 6.3 ppb, which is 3.00 59.68 3.90 59.67 N-Formylmorpholine Benzene Toluene Xylene Aromatic 1.66 20.28 1.92, 20.67
    The results obtained with isotB and 2.7 57; 89 3.12 58.33 provide by recirculation about 80 weight from the total vapor phase leaving separator 17 after cooling in condenser 16 through pipe 21 "Lower part of the steam of distillation column 20 operates at a temperature, the concentration of water is 7 weight, and the concentration of hydrocarbons is about k weight L, the results of the isoenthalpic expansion; the yrenes are presented in table 3. T a b i c 3, 8 59,35, 90 58.99 2.09 20.99 2.22 21.2t 159 Under these conditions, the heat consumption in the steam column 20 decreases to H6.1 kcal / kg of the original raw material, and thus saving in heat consumption is about 38 relative to the known method. Similarly, the process can be carried out with a decrease in the operating temperature of the bottom of the column 20 from to and with an increase in the water content from to 6.3 weight%, claim 1, A method for separating aromatic hydrocarbons from their mixtures with non-aromatic two-step solvent extraction with a water-containing N-formylmorpholine as a selective solvent to obtain an extract and raffinate and then by feeding the extract to an extractive rectification with separation of the distillate obtained by two-step condensation into a higher boiling fraction returned to the first stage of extraction into the zone between the solvent and raw materials, and the fraction with lower boiling point returned to the cube the second stage of the Estraction, and rectification of the vat residue of the extractive distillation in the presence of water with the selection in the distillate of the mixture of aromatic hydrocarbons with water and the separation of the latter into aromatic hydrocarbons and water, which is returned as reflux to the rectification stage and fed to the washing of the obtained raffinate, followed by the introduction of the washing water into the cube of the second extraction stage and with 16 boron in the residue of the rectification of the solvent returned to the extraction stage, characterized in that in order to reduce energy costs, a solvent containing 3.9 7% by weight of water and 2-aromatic hydrocarbons, which is subjected to isental expansion to residual d, is taken to the bottoms at the stage of rectification. detecting 0-160 mmHg with a selection of a liquid solvent stream containing 0,, 9 weight L of water and 0.79-2, weight of aromatic hydrocarbons returned to the first stage of extraction, and a vaporous solvent stream enriched with water and aromatic hydrocarbons, which is subjected to condensation, followed by mixing 40- 80 wt.% Of the condensate obtained with the extract discharged from the extraction stage before it is fed to the extractive distillation stage and feeding the remaining part of the condensate into the second stage extraction cube, 2. The method according to claim 1 is different and Extraction is carried out at 15-100 ° C. 3. The method according to claim 1, characterized in that the extractive distillation and rectification is carried out at 50-160 ° C. Sources of information taken into account during the examination 1. USSR patent number ii85588, cl. C 07 7/10, published 1973. 2. Patent of the USSR ° 563116, cl. From 07 to 7/10, published. 1977. 3. The patent of Great Britain No. 1271596, cl. C 07 S 7/02, published 1972 (prototype) about
    权利要求:
    Claims (3)
    [1]
    Claim
    1, Method for the separation of aromatic 5 hydrocarbons from their mixtures with non-aromatic by two-stage liquid extraction with water-containing N-formylmorpholine as a selective solvent with the production of extract 2 and raffinate and subsequent feeding of the extract for extractive distillation with separation of the obtained distillate by two-stage condensation into a high-boiling fraction 25 is recycled to the first extraction stage into the zone between the entry points of the solvent and feedstock and the fraction with a lower tempo boiling water, returned 30 • to the cube of the second extraction stage, and rectification of the cubic residue of extractive distillation in the presence of water with the selection in the distillate of a mixture of aromatic hydrocarbons with water and separation of the latter into aromatic hydrocarbons and water, which is returned as reflux to the stage rectification and fed to the washing of the obtained raffinate, with 40 the next introduction of washing water into the cube of the second stage of extraction and selection in the bottom residue of the rectification of the solvent returned to the stage, extraction and, characterized in that, in order to reduce energy costs, a solvent containing 3.9 "7 wt.% water and 2-4 wt.% aromatic hydrocarbons, which is isoenthalically expanded to a residual pressure of 40 -1b0 mmHg with the selection of a liquid solvent stream containing 0.94-4.9 wt.% water and 0.79 “2.84 wt.% aromatic carbon. - levodorods returned to the first stage of extraction, and a vaporous stream of solvent enriched in water and aromatic hydrocarbons, which is subjected to condensation, followed by mixing 4 () - 80 wt.% Of the obtained condensate with the extract removed from the extraction stage before being fed to the stage of extractive rectification and feeding the remainder of the condensate into the cube of the second extraction stage,
    [2]
    2. The method of pop., 1, is distinguished by the fact that the extraction is carried out at 15 “10 ° C.
    [3]
    3. The method of pop. 1, characterized in that the extractive rectification and rectification is carried out at 50-1 ° C.
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    同族专利:
    公开号 | 公开日
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    法律状态:
    优先权:
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