Method and device for improved extraction distillation by water steam supply into reboiler, connected with extraction distillation column

FIELD: power engineering.

SUBSTANCE: invention is intended for extraction distillation. Device for extraction distillation of the extract from the flow of raw material comprises the extraction distillation column, raw material flow supply line, solvent supply line, reboiler with internal steam distributor, connected with the extraction distillation column, water steam supply line, connected with the steam distributor, and water steam supply line from the extraction distillation column, connected with the internal steam distributor. The extract is an aromatic hydrocarbon. Reboiler is selected from the group consisting of the kettle boiler, thermosyphon reboiler and reboiler with forced circulation.

EFFECT: improvement of efficiency of extraction distillation.

10 cl, 1 dwg, 1 ex

 

This application claims priority based on provisional patent application U.S. 61/239272 dated 9 September 2009 and patent application U.S. No. 12/706937 from February 17, 2010, each of which is incorporated into this description by reference in its entirety.

The LEVEL of TECHNOLOGY

The supply of steam to the distillation column as a means for steaming usually allows to carry out the distillation at a lower temperature than without the addition of water vapor. Steam can also be submitted to a distillation column which operates as an extractive distillation column. Usually steam is fed directly to the section of the column below the last collector plates.

The inclusion of reboiler in a distillation apparatus for use water vapor as a heat source gives a lot of technological advantages, including the possibility of implementation of the distillation. Although the use of reboilers known in the practice of distillation, the simultaneous use of reboiler as to heat the distillation column, and as a means for steaming in extraction distillation still was not described.

Therefore improved methods and devices for the extraction distillation using reboiler as for heating, and as a means is to steam could provide significant benefits. In addition, improved reboiler, allowing to intensify heat and mass transfer, could provide significant benefits described here are devices and methods extraction distillation.

DISCLOSURE of INVENTIONS

In the present description describes the different variants of the device for the extraction distillation of the extract from the stream of raw materials. This device includes a column extractive distillation, a reboiler connected to the extraction column distillation, and the supply line of the water vapor. The reboiler with a humidifier. Supply line of the water vapor is connected with the interior of the humidifier.

In the present description also describes other variants of the device for the extraction distillation of the extract from the stream of raw materials. The device includes a column extractive distillation boiler reboiler connected to the extraction column distillation, the line of flow of raw materials, the supply line of the solvent, the supply line of the water vapour line drain mixture of distillate and solvent and steam extraction line. In the boiler-the reboiler has an internal humidifier.

In other embodiments, the device for extraction distillation of the extract from the stream of raw materials includes the column extractive distillation, a reboiler connected to the extraction column distillation, and line the filing of water vapor. The reboiler has an internal space and an external surface. Supply line of the water vapor is connected with the inner space of reboiler.

In the following embodiments, there are described methods of extraction distillation of the extract from the stream of raw materials containing at least one hydrocarbon. These methods include (a) extraction of at least one hydrocarbon from the stream of raw material by the solvent to form a mixture of hydrocarbon/solvent b) the supply of water vapor directly into the reboiler, (C) the supply of steam as a coolant tube reboiler, d) mixing the mixture of the hydrocarbon/solvent with steam through the steam may condense inside reboiler, and (e) evaporation of the mixture of the hydrocarbon/solvent. In some embodiments, these methods also include separating at least one hydrocarbon from the mixture of the hydrocarbon/solvent after the stage of evaporation.

Features of the present invention have been described above in General terms for a better understanding of the subsequent detailed description. The following are additional features and advantages of the inventions that are the subject of the formulas presented.

BRIEF DESCRIPTION of DRAWINGS

For a more complete understanding of the present invention and its advantages is the following description in conjunction with the drawing, where urogenitalnye variants of the invention, among them:

the FIGURE 1 shows a diagram of the apparatus of the extraction distillation, in which water vapor is fed directly into the reboiler.

The IMPLEMENTATION of the INVENTION

In the following description shows some details, such as specific quantities, sizes, etc. necessary for a complete understanding of the disclosed here options. However, experts in this field will be obvious that the present invention can be realized without such detail. In many cases, these and other details of such description are not listed because they are not necessary for a full understanding of the present invention and known qualified specialists in the respective field.

In General, it is clear that these drawings are only illustrative description of the specific variants of the invention and not limit it. The scale of the figures in this case are not significant.

While most used terms understandable to experts in this field, however, it should be borne in mind that unless otherwise agreed, these terms should be interpreted in the sense which is accepted by specialists in this field. In cases where the expression could be understood as meaningless or mostly meaningless, its definition should be taken from Webster's Dictionary Webster's Dictionary, 3rd Edition,2009. Do not enter the definition and/or interpretation of other related or unrelated patent applications, patents and publications, unless specifically stated herein or their use is necessary to preserve meaning.

Used herein, the term "aromatic" refers to aromaticity, i.e., the chemical property that provides a stronger stabilization of the coupled-loop containing unsaturated communication, lone-electron pair or vacant orbitals than would be expected if only one pair. Aromaticity can also be viewed as a manifestation of cyclic delocalization and resonance stabilization. Usually it is believed that this effect is due to free electrons in cyclically arranged atoms, which are connected to each other alternating the ordinary and double bonds.

Used herein, the term "aliphatic" refers to compounds with carbon atoms that can connect to each other in unbranched chains, branched chains or rings (in this case they are called alicyclic). They can be connected by single bonds (alkanes), double bonds (alkenes) or triple bonds (alkynes).

In various embodiments, the methods and devices described in this invention increase the efficiency of xtraction distillation, in particular extractive distillation of aromatic compounds. In various devices and methods described herein, to increase the efficiency of use of the steam in the reboiler connected to the extraction column distillation device extraction distillation. Such a device and method used for separation of styrene from raw pyrolysis gasoline. Styrene obtained ways described here and on the proposed apparatus will be called the next GT-styrene. The person skilled in the art it will be important that using the steps described here are methods and devices can be distinguished from the flow of raw materials along with styrene and other hydrocarbons. For example, other hydrocarbons may include VTH (benzene/toluene/xylene), isoprene, butadiene and other vinylaromatic connection.

In the method of extraction distillation GT-styrene flow raw material - average fraction of pyrolysis gasoline, representing the past Hydrotreating hydrocarbons C8, including styrene, refer to the column extractive distillation (EDC). In the system of vapor-liquid solvent selectively extracts styrene, which is directed into the lower part of the column of EDC, and other C8 aromatic hydrocarbons and non-aromatic components (i.e., aliphatic compounds) are sent to the flow of raffinate in the upper part of the column EDC.The solvent can be changed without restriction. In various embodiments, the EDC is a Packed column. In other embodiments, the EDC operates under vacuum. Column EDC is supplied with heat from reboiler, which is used as coolant water vapor. Enriched with styrene solvent away from the bottom of the column EDC and then served in the column regeneration allocation solvent (SRC). Styrene is separated and then the solvent is sent back to the column EDC.

In various embodiments, there is described a device for the extraction distillation of the extract from the stream of raw materials. This device includes a column extractive distillation, a reboiler connected to the extraction column distillation, and the supply line of the water vapor. Inside reboiler have a humidifier. Supply line of the water vapor is connected with the interior of the humidifier.

In other embodiments, the device for extraction distillation of the extract from the stream of raw materials includes the column extractive distillation, a reboiler connected to the extraction column distillation, and the supply line of the water vapor. The reboiler has an internal space and an external surface. Supply line of the water vapor is connected with the inner space of reboiler.

In some embodiments, the device of the extraction column is a system of single-stage evaporation. However, in other embodiments, the condition is device using column extraction distillation can be formed of a two-, three - or multi-stage evaporation.

In some embodiments, the device supply line water vapor is a circuit generating steam. This circuit generation system of water vapor provides a balance of water in this embodiment. For example, the water vapor generated from the system water balance (loop generating steam) is fed into the lower part of the column of EDC to participate in the extractive distillation and the temperature at the bottom of this column. In some embodiments, the flow of water vapor in the lower part of the column of EDC to reduce the temperature combined with vacuum effects. The water is then transferred from the EDC in the raffinate phase is separated and returned as process steam in a closed circuit for further extraction distillation. Described here extractive distillation GT-styrene temperature reduction is especially significant because it prevents or significantly reduces the danger of styrene polymerization in the column EDC.

In various embodiments, the water vapor is fed directly into the lower part of the inner space of reboiler. This way steam has the advantage that it provides the highest efficiency of mass/heat transfer of water vapor. Other methods of supplying water vapor into the interior of reboiler also otec who have the spirit and scope of the present invention. For example, the supply of water vapor below the last column plate EDC (in the absence of reboiler) or above reboiler (lower manifold plates) do not provide such high performance mass/heat transfer. Any other options to improve the efficiency of the method of extraction distillation, for example, to create a differential pressure by using a vacuum or increase the feed rate of water vapor.

In the above embodiments, to facilitate the extraction of aromatic hydrocarbons using steam in the reboiler. In various embodiments, the aromatic hydrocarbon is styrene or other vinylaromatic connection. However, the described methods and devices can be used for extraction distillation other distillates of flows of raw materials because they meet the spirit and scope of the present invention. As indicated above, the devices and methods of the present invention have the advantage that they operate at temperatures that do not contribute to the polymerization vinylaromatic connections.

In various embodiments of the present invention uses a heat-reboiler. However, any person skilled in the art it will be clear that the here described methods and apparatus can be used any type of reboiler. Such alternative reboiler include, for example, thermosiphon R the boilers and reboiler with forced circulation. In embodiments described herein boiler reboiler has the advantage that it provides a large contact time and a small drift in the way of the extraction distillation with the introduction of water vapor directly into the interior of reboiler.

To improve the efficiency of the method of extraction distillation reboiler can be modified by calculating the efficiency of mass - and heat transfer distillate. Although the methods and apparatus of the present invention can be used reboiler of any size, for maximum efficiency it is preferable that the size of reboiler was sufficient to ensure effective contact time with sufficient mass transfer between liquid and gas phases. Effective contact time depends, for example on the composition of the flow of raw materials processed, and the person skilled in the art can easily determine the effective contact time, depending on the specific requirements of the method. In various embodiments, reboiler of the present invention have been modified by the use of internal humidifier, which leads to improved distribution of water vapor in the inner space of reboiler.

In other embodiments, the device for extraction distillation of the extract from the stream of raw materials includes the extraction column distillation boiler rebeu the EP, coupled with the column extractive distillation, the line of flow of raw materials, the supply line of the solvent, the supply line of the water vapour line drain mixture of distillate and solvent and steam extraction line. The boiler has an internal reboiler steam distributor. Supply line of the water vapor is connected with the interior of the humidifier.

In the following embodiments, there are described methods of extraction distillation of the extract from the stream of raw materials containing at least one hydrocarbon. These methods include (a) solvent extraction of at least one hydrocarbon from the stream of raw material with formation of a mixture of the hydrocarbon/solvent b) the supply of water vapor directly into the reboiler, (C) the supply of water vapor to heat the tubes reboiler, d) mixing the mixture of the hydrocarbon/solvent with steam through the steam may condense inside reboiler and (e) evaporation of the mixture of the hydrocarbon/solvent. In some embodiments, these methods also include separating at least one hydrocarbon from the mixture of the hydrocarbon/solvent after the stage of evaporation. In some embodiments, the shell reboiler is a boiler-reboiler.

Experimental example

The following example is offered to more fully illustrate some of the options disclosed above. It should be emphasized for specialists in this about the region, this example represents one of the methods of the invention. Professionals need to understand that, in the light of the present invention in the disclosed specific ways you can make many changes and get the same or similar result without departing from the spirit and scope of the invention.

Example 1: Device extraction distillation with a reboiler. Different variants of the present invention can be better understood with the help of FIGURE 1. The FIGURE 1 shows the diagram of the apparatus of the extraction distillation 1, in which the water vapor is fed directly into the reboiler. As shown in FIGURE 1, the flow of raw materials C8 (containing styrene) after Hydrotreating is the average fraction of pyrolysis gasoline, and it is served in a column extraction distillation 120 along the line of flow of the raw material 101. In this example, the average fraction enriched in C8 styrene (~30 - ~40 wt.%). Column extraction distillation 120 is a Packed column connected to a supply line of flow of the raw material 101 and the supply line of the solvent 102. In various embodiments, the apparatus extraction distillation operates under vacuum. In some embodiments, lean solvent is fed to the extraction column distillation 120 along the line of feed of the solvent 102 at a temperature in the range of about 70°C. - 100°C.

Column extraction distillation 120 is connected with the boiler-what boileroom 135. The heat supplied to the boiler-reboiler 135 on the supply line of the saturated water vapor 106. Saturated water vapor condenses inside the tubes reboiler. In different variants regulate the temperature of the lower part of the column extractive distillation 120 using boiler-reboiler 135 at about 120°C or below. Such temperatures are preferred, because they practically do not cause polymerization of styrene in the lower part of the column.

In various embodiments of the device for the extraction distillation system vapor/liquid solvent to extract the styrene in the lower part of the column extractive distillation 120, displacing the raffinate (other C8 aromatic hydrocarbons and non-aromatic hydrocarbons) in the upper part of the column extractive distillation 120. Vapors from the upper part of the column condense in the refrigerator 127 and sent to separator 130 through line 125. In the separator 130 aqueous phase is removed by phase separation and direct lines of drainage of water 104. Desantiruemye water line water drainage 104 pumped as technical water through the circuit generation system of water vapor (not shown) and is directed back into the reboiler 135. In the reboiler 135 water immediately turn in technological water vapor, which enters the lower part of reboiler 135 along the lines of water vapor 107. In one embodiment, the hydrocarbon fraction (raffinate), remaining in the aparature 130 after water separation, pumped back into the column extractive distillation 120 through the line of phlegmy 105 at reflux the number of about 1. Alternative raffinate can be removed from the system along the line of withdrawal of raffinate 103.

Water vapor is served by lines of water vapor 107 inside reboiler 135 and mixed with the liquid stream 109 from the column extractive distillation 120. After that, the steam flow 108, formed from water vapor inside reboiler 135, sent back to the extraction column distillation 135 lower collector plate 150. Steam flow 108 supplies depleted styrene solvent to continue extraction distillation and, in addition, it heats the column extractive distillation 120. Remaining in the reboiler 135 liquid containing styrene and solvent, direct line reboiler 110 in the form of liquid product in the lower part of the column. There styrene plus solvent is pumped through line 111 to the column selection of the solvent 160.

The reboiler 135 specially designed for methods of extraction distillation according to the present invention, in order to increase its efficiency. As shown above, water vapor is added to the reboiler 135 along the lines of water vapor 107. In the reboiler 135 water vapor is supplied into the internal humidifier 140. Steam reduces the partial pressure of the extracted styrene. After reboil is and 135 styrene together with the solvent is sent in the form of liquid product in line reboiler 110 in the lower part of the column extractive distillation 120.

Styrene together with the solvent in line 111 is sent to the column selection of the solvent 160, where the solvent is separated pure styrene. Then, if necessary, the solvent is returned to the extraction column distillation 120 on line 102.

As is known to the person skilled in the art, the efficiency of the mass transfer of water vapor is determined as follows:

Ev=nandblYudandemaboutepandpCandandlbnaboutedandinlenandeineyewith atinandnandinsxaboutdepandpCandandlbnaboutedandinlenandeineyewith atinandppandpandinnaboutinewith aandand

The efficiency of mass transfer in the reboiler is usually taken as 100% (close to one theoretical Tarek is). However, 100% of the efficiency of mass transfer is not applicable with the introduction of water vapor directly into the reboiler, especially in the case of vertical reboiler, where the contact time in the contact zone (between entering the reboiler steam and liquid phases) is not high enough. It was found that the boiler reboiler described in this embodiment in FIGURE 1, gives the advantage that it leads to a great time of contact (close contact) between the phases. A model was developed to determine/calculate the efficiency, which served as the basis for calculating the mechanical dimensions of reboiler and humidifier.

Based on the above description, the person skilled in the art can easily establish the main characteristics of this invention and, without departing from its spirit and scope, can make various changes and modifications to adapt the description to the various options and applications. Described above are only illustrative and are not intended to limit the scope of the invention, which is defined by the following formula.

1. Device for the extraction distillation of the extract from the flow of raw materials, including:
column extraction distillation;
the reboiler connected to the extraction column distillation;
the reboiler further includes an internal humidifier;
LiveUpdate water vapor, connected to the humidifier, and the extract is an aromatic hydrocarbon; and
the line of liquid flow from the column extractive distillation connected with internal humidifier.

2. The device under item 1, in which the extraction column distillation system includes single-stage evaporation.

3. The device under item 1, in which the aromatic hydrocarbon is a styrene.

4. The device under item 1, in which the reboiler is a boiler-reboiler.

5. The device extraction distillation of the extract from the flow of raw materials, including:
column extraction distillation;
boiler-a reboiler connected to the extraction column distillation;
the boiler reboiler further includes an internal humidifier;
the line of flow of raw materials,
the supply line of the solvent,
the supply line of the water vapor that is connected with the interior of the humidifier,
the line of withdrawal of the mixture of distillate and solvent, and
the line of liquid flow from the column extractive distillation in the interior of the humidifier, and the extract is an aromatic hydrocarbon.

6. The device under item 5, in which the extraction column distillation system includes single-stage evaporation.

7. The device under item 5, in which the aromatic hydrocarbon represented yet a styrene.

8. The device under item 5, in which the supply line pair includes a circuit generating steam.

9. Device for the extraction distillation of the extract from the flow of raw materials, including:
column extraction distillation;
the reboiler connected to the extraction column distillation;
the reboiler includes an internal space and an external surface, and further includes an internal humidifier;
the supply line of the water vapor that is connected with the interior of the humidifier; and
the line of flow of the liquid stream from the column extractive distillation in the interior of the humidifier, and the extract is an aromatic hydrocarbon.

10. The device under item 9, in which the reboiler is chosen from the group consisting of a boiler-reboiler, thermosiphon reboiler and reboiler with forced circulation.



 

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1 tbl

FIELD: chemistry.

SUBSTANCE: invention concerns improved method for obtaining (meth)acrylic acid involving steam phase catalytic oxidation of propylene, propane or isobutylene for production of reaction mix, absorption of oxidised reaction product in water to obtain water solution containing (meth)acrylic acid, concentration of water solution in the presence of azeotropic agent and distillation of obtained (meth)acrylic acid in distillation column to obtaining purified (meth)acrylic acid. During operation of distillation column, including operation interruption and resumption, the column is washed with water, and afterwards azeotropic distillation is performed in the presence of azeotropic agent.

EFFECT: efficient and fast cleaning of distillation column with extraction of valuable substance.

5 cl, 5 dwg, 3 ex

FIELD: chemistry.

SUBSTANCE: method of separation of starting mixture (A) consisting of two or more constituents, by extractive distillation with the selective solvent (S) within dividing wall column (TKW), is proposed. The separation is performed in the dividing wall column (TKW) having a dividing wall aligned in a longitudinal direction (TW) and extending to an upper end of the column and dividing an interior of the column into first region (1), second region (2), and lower combined column region (3). The starting mixture is fed into first region (1), first top stream (B) is taken off from first region (1), and second top stream (C) is taken off from second region (2), with each of the streams having a prescribed specification. The selective solvent (S) is introduced in an upper part of first region (1) and/or in an upper part of second region (2), and flow of solvent (S1) into the first region (1) and/or flow of solvent (S2) into second region (2) are set so that each of the prescribed specifications for top streams (B, C) are met.

EFFECT: invented method of dividing mixtures is more efficient in terms of energy and solvent consumption.

6 cl, 7 dwg, 1 tbl

FIELD: ecology; hydrochemistry; analytical chemistry; methods of extraction of the volatile organic substances from the water medium.

SUBSTANCE: the invention is pertaining to the field of ecology, hydrochemistry, analytical chemistry and may be used for extraction of the organic compounds from the water mediums, in particular, from the mineral waters including sulfide mineral waters. For realization of the method of extraction of the volatile organic substances from the water medium into the organic dissolvent conduct the joint condensation of the extracted substance produced as a result of distillery and the vapor of the dissolvent. For production of the joint condensate they gate the vapor-shaped dissolvent through the water sample or preliminary add it into the water sample with the subsequent distillation. The organic dissolvent is chosen from the following row: ethanol, acetonitrile, acetone, hexane. The method ensures the single-stage extraction of the dissolved organic substances into the dissolvents, the unlimited their mixing with the water, reduction of the thermal action on the researched sample, the increase of the extraction ratio.

EFFECT: the invention ensures the single-stage extraction of the dissolved organic substances into the dissolvents, their unlimited mixing with the water, the reduced the thermal action on the researched sample, the increased extraction ratio.

2 cl, 1 tbl, 5 ex

The invention relates to the separation of 1,1-differetn from vinyl chloride

FIELD: ecology; hydrochemistry; analytical chemistry; methods of extraction of the volatile organic substances from the water medium.

SUBSTANCE: the invention is pertaining to the field of ecology, hydrochemistry, analytical chemistry and may be used for extraction of the organic compounds from the water mediums, in particular, from the mineral waters including sulfide mineral waters. For realization of the method of extraction of the volatile organic substances from the water medium into the organic dissolvent conduct the joint condensation of the extracted substance produced as a result of distillery and the vapor of the dissolvent. For production of the joint condensate they gate the vapor-shaped dissolvent through the water sample or preliminary add it into the water sample with the subsequent distillation. The organic dissolvent is chosen from the following row: ethanol, acetonitrile, acetone, hexane. The method ensures the single-stage extraction of the dissolved organic substances into the dissolvents, the unlimited their mixing with the water, reduction of the thermal action on the researched sample, the increase of the extraction ratio.

EFFECT: the invention ensures the single-stage extraction of the dissolved organic substances into the dissolvents, their unlimited mixing with the water, the reduced the thermal action on the researched sample, the increased extraction ratio.

2 cl, 1 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: method of separation of starting mixture (A) consisting of two or more constituents, by extractive distillation with the selective solvent (S) within dividing wall column (TKW), is proposed. The separation is performed in the dividing wall column (TKW) having a dividing wall aligned in a longitudinal direction (TW) and extending to an upper end of the column and dividing an interior of the column into first region (1), second region (2), and lower combined column region (3). The starting mixture is fed into first region (1), first top stream (B) is taken off from first region (1), and second top stream (C) is taken off from second region (2), with each of the streams having a prescribed specification. The selective solvent (S) is introduced in an upper part of first region (1) and/or in an upper part of second region (2), and flow of solvent (S1) into the first region (1) and/or flow of solvent (S2) into second region (2) are set so that each of the prescribed specifications for top streams (B, C) are met.

EFFECT: invented method of dividing mixtures is more efficient in terms of energy and solvent consumption.

6 cl, 7 dwg, 1 tbl

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