CN218910199U - System for purifying m-dichlorobenzene in mixed dichlorobenzene - Google Patents
System for purifying m-dichlorobenzene in mixed dichlorobenzene Download PDFInfo
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- CN218910199U CN218910199U CN202223357748.6U CN202223357748U CN218910199U CN 218910199 U CN218910199 U CN 218910199U CN 202223357748 U CN202223357748 U CN 202223357748U CN 218910199 U CN218910199 U CN 218910199U
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Abstract
The utility model discloses a system for purifying m-dichlorobenzene in mixed dichlorobenzene. The system for purifying m-dichlorobenzene in mixed dichlorobenzene comprises: the device comprises a meta-position tower A and a meta-position tower B, wherein the tower bottom of the meta-position tower A is connected with the feed inlet of the meta-position tower B, the tower top of the meta-position tower B is connected with the feed inlet of the meta-position tower A, and a meta-position extraction outlet is arranged on the tower top of the meta-position tower A; the meta-position tower A and the meta-position tower B are filler rectifying towers, wherein the filler is high-efficiency silk screen filler, and the theoretical plate numbers of the meta-position tower A and the meta-position tower B are not less than 100. The purification system of the utility model uses simple rectification equipment, the purity of the purified m-dichlorobenzene is high, the product yield is high, and the equipment and operation cost is low.
Description
Technical Field
The utility model relates to a system for purifying m-dichlorobenzene in mixed dichlorobenzene.
Background
M-dichlorobenzene, also known as 1, 3-dichlorobenzene, of formula C 6 H 4 Cl 2 The organic matter is colorless liquid, has pungent smell, is insoluble in water, is soluble in alcohol and ether, can perform chlorination, nitration, sulfonation and hydrolysis reactions, and is an isomer with paradichlorobenzene and orthodichlorobenzene when meeting the severe reaction of aluminum. The m-dichlorobenzene is a very important fine chemical organic chemical raw material, is mainly applied to the production industries of medicines, pigments, dyes, pesticides and the like, is also applied to organic synthesis and organic solvents, and is an indispensable chemical product. In particular, in recent years, the medical field has rapidly developed, and the demand of high-purity m-dichlorobenzene in the market has been increasing, and the market supply and demand at home and abroad have been short. The direct chlorination of benzene and the metathesis of p-dichlorobenzene are the main synthetic methods for preparing m-dichlorobenzene, and the two methods are all mixtures of three isomers. Therefore, how to obtain high-purity m-dichlorobenzene from three isomer mixtures has been a hot problem in the art.
The traditional method for separating m-dichlorobenzene is a method combining crystallization and rectification. The method is that dichlorobenzene isomer mixture is separated out through crystallization, crystallization mother liquor is distilled, o-dichlorobenzene is enriched in distillation residual liquid, distillate is recrystallized, and p-dichlorobenzene is separated out to obtain mother liquor enriched in m-dichlorobenzene. The purity of the m-dichlorobenzene obtained by the method is not high, the separation efficiency is low, and the cost is high; in addition, the purification method combining crystallization and rectification has the advantages of large equipment quantity and high equipment cost. European patent EP451720 proposes the separation of the two isomers by extractive distillation by adding the extractants hexamethylphosphoramide and sulfolane to a mixture of m-dichlorobenzene and p-dichlorobenzene. The disadvantage of this process is that the purity and yield of the m-dichlorobenzene obtained are not optimal.
Disclosure of Invention
The utility model solves the technical problems of low separation purity, low product yield and high equipment cost in the method for purifying m-dichlorobenzene in mixed dichlorobenzene in the prior art, and provides a system for purifying m-dichlorobenzene in mixed dichlorobenzene. The purification system of the utility model uses simple rectification equipment, the purity of the purified m-dichlorobenzene is high, the product yield is high, and the equipment and operation cost are low.
In order to achieve the above purpose, the present utility model adopts the following technical scheme:
the utility model provides a system for purifying m-dichlorobenzene in mixed dichlorobenzene, which comprises the following components: the device comprises a meta-position tower A and a meta-position tower B, wherein the tower bottom of the meta-position tower A is connected with the feed inlet of the meta-position tower B, the tower top of the meta-position tower B is connected with the feed inlet of the meta-position tower A, and a meta-position extraction outlet is arranged on the tower top of the meta-position tower A; the meta-position tower A and the meta-position tower B are both packed rectifying towers, wherein the packing is high-efficiency silk screen packing, the theoretical plate number of the meta-position tower A is not less than 100, and the theoretical plate number of the meta-position tower B is not less than 100.
In the present utility model, the theoretical plate number of the meta-column a is preferably 100 to 120.
In the present utility model, the theoretical plate number of the meta-column B is preferably 100 to 120.
In the present utility model, preferably, the position of the feed inlet of the meta-column a is in the column.
In the utility model, preferably, the tower bottom of the meta-position tower A is also connected with a reboiler A, and the outlet of the reboiler A is connected with the tower bottom of the meta-position tower A.
Wherein the reboiler a is preferably a falling film reboiler.
The liquid phase in the falling film reboiler descends fast due to the action of the gas phase and gravity, so that the residence time is shortened, the pressure drop is reduced, the inlet-outlet temperature difference is reduced, and the falling film reboiler is more suitable for thermosensitive substances.
In the utility model, the meta-position extraction outlet is the m-dichlorobenzene extraction outlet as is conventionally understood by those skilled in the art.
In the utility model, the tower bottom of the meta-position tower B is also connected with a reboiler B, and the outlet of the reboiler B is connected with the tower bottom of the meta-position tower B.
Wherein the reboiler B is preferably a falling film reboiler.
In the present utility model, preferably, the tower bottom of the meta-position tower B is further provided with an ortho-position extraction port.
Wherein the ortho-position extraction outlet is used for extracting general ortho-position toluene, para-xylene and some by-product trichlorotoluene.
In the utility model, the system preferably further comprises a weight removing tower, wherein the top of the weight removing tower is connected with the feed inlet of the meta-position tower A and is used for removing tar, salt and heavy components in the mixed dichlorobenzene.
Wherein the heavy component is typically a material that is not readily vaporized.
Wherein the de-weight column is preferably a packed rectifying column. The filler may be conventional in the art, preferably a plate corrugated structured filler.
Wherein the theoretical plate number of the heavy-duty removal tower can be calculated according to the routine in the art, and is preferably 18-25, more preferably 20
Wherein, the position of the feed inlet of the heavy removal tower is preferably the middle part of the tower.
Wherein, preferably, the tower kettle of the weight removing tower is also connected with a film scraping evaporator or a stirring kettle, preferably, a stirring kettle, and the outlet of the kettle top of the stirring kettle is connected with the tower kettle of the weight removing tower and is used for refluxing the evaporated gas component in the stirring kettle to the tower kettle of the weight removing tower.
Still more preferably, the bottom of the stirring kettle is also connected with a reboiler C, and the outlet of the reboiler C is connected with the tower kettle of the weight removing tower.
Wherein the reboiler C is preferably a falling film reboiler.
Still more preferably, the bottom of the stirring kettle is connected with a heavy component extraction outlet for extracting part of bottom liquid of the stirring kettle.
In the utility model, the system preferably further comprises a light component removing tower, wherein the tower bottom of the light component removing tower is connected with the feed inlet of the meta-position tower A and is used for removing light components in the mixed dichlorobenzene.
Wherein the light component may be a component having a boiling point lower than that of m-dichlorobenzene conventionally present in mixed dichlorobenzene, typically comprising chlorobenzene.
Wherein the light component removing tower is preferably a packed rectifying tower. The filler may be conventional in the art, preferably a plate corrugated structured filler.
Wherein, the theoretical plate number of the light component removing tower can be calculated according to the routine in the field, and is preferably 15-25.
Wherein the location of the feed inlet of the light ends removal column may be conventional in the art, preferably the upper half of the light ends removal column.
Preferably, the tower bottom of the light component removing tower is also connected with a reboiler D, and the outlet of the reboiler D is connected with the tower bottom of the light component removing tower.
Preferably, a light component extraction outlet is arranged at the top of the light component removing tower.
In certain preferred embodiments of the present utility model, the system comprises the heavy-removal column, the light-removal column, the meta-column A and the meta-column B in sequence, wherein the top of the heavy-removal column is connected with the feed inlet of the light-removal column, and the bottom of the light-removal column is connected with the feed inlet of the meta-column A.
In the utility model, the system preferably further comprises an ortho-position tower, wherein the ortho-position tower is a rectifying tower, and a feed inlet of the ortho-position tower is connected with a tower kettle of the meta-position tower B and is used for separating o-dichlorobenzene and p-dichlorobenzene in tower kettle liquid of the meta-position tower B.
Wherein the ortho-column is preferably a packed rectifying column.
The packing in the packed rectifying column is preferably a plate corrugated structured packing.
Wherein the theoretical plate number of the ortho-column is preferably 15 to 25, more preferably 20
Wherein the position of the feed inlet of the ortho-column is preferably the lower half of the ortho-column.
Wherein, the tower kettle of the ortho-position tower is preferably also connected with a reboiler E, and the outlet of the reboiler E is connected with the tower kettle of the ortho-position tower.
Wherein, preferably, the tower bottom of the ortho-position tower is also provided with a trichlorobenzene extraction port.
Preferably, the top of the ortho-position tower is also provided with an ortho-position extraction outlet.
The utility model also provides a method for purifying m-dichlorobenzene in mixed dichlorobenzene, which comprises the following steps: the system for purifying m-dichlorobenzene in the mixed dichlorobenzene is adopted, the mixed dichlorobenzene is fed from a feed inlet of a meta-position tower A, and the purified m-dichlorobenzene is produced from a meta-position extraction outlet; the mixed dichlorobenzenes comprise m-dichlorobenzene, p-dichlorobenzene and o-dichlorobenzene, the pressure drop of the meta-column A is not more than 30mbar, and the pressure drop of the meta-column B is not more than 30mbar.
In the present utility model, the mass percentage of the m-dichlorobenzene in the mixed dichlorobenzene is preferably not less than 45%, more preferably 48%.
In the present utility model, the mass percentage of the paradichlorobenzene in the mixed dichlorobenzene is preferably not more than 25%, for example, 24%.
In the present utility model, the mass percent of the o-dichlorobenzene in the mixed dichlorobenzene may be conventional in the art, preferably not higher than 25%, for example 20%.
In the present utility model, the feeding temperature of the meta-column A is preferably 139.9℃to 145℃and more preferably 139.9 ℃.
In the present utility model, the overhead reflux temperature of meta-column a may be conventional in the art, preferably 50 ℃.
In the present utility model, the reflux at the top of the meta-column A is preferably 10 to 20, more preferably 13 to 17, still more preferably 15.
In the present utility model, the feeding temperature of the meta-column B is preferably 136℃to 145℃and more preferably 142.3 ℃.
In the present utility model, the overhead reflux temperature of the meta-column B may be conventional in the art, preferably 50 ℃.
In the present utility model, the reflux at the top of the meta-column B is preferably 15 to 25, more preferably 20.
In the present utility model, preferably, when the mixed dichlorobenzene further comprises organic salt and heavy components, the system further comprises the weight removing tower, and the mixed dichlorobenzene is fed from a feed inlet of the weight removing tower.
Wherein, the heavy component refers to tar or other components which are difficult to evaporate and are generated in the synthesis process of m-dichlorobenzene.
Wherein the mass percentage of the organic salt and the heavy component in the mixed dichlorobenzene is conventional in the art, and the effect of separation and purification is not greatly influenced.
Wherein the pressure drop of the de-weight column is preferably not more than 10mbar, more preferably 10mbar.
Wherein the feed temperature to the de-heavies column may be conventional in the art, preferably from 110 ℃ to 130 ℃, more preferably from 115 ℃ to 125 ℃, still more preferably 120 ℃.
Wherein, the top reflux temperature of the heavy-duty removal tower is preferably 55-65 ℃, more preferably 60 ℃.
Wherein, the top reflux of the heavy-removal tower is preferably 0.8-1.5, more preferably 1.
In the present utility model, preferably, when the mixed dichlorobenzene further comprises a light component, the system further comprises the light component removal tower, and the mixed dichlorobenzene is fed from a feed inlet of the light component removal tower.
Wherein the light component may be a component having a boiling point lower than that of the m-dichlorobenzene as is conventional in the art, typically comprising chlorobenzene.
Wherein, the weight percentage of the light component to the mixed dichlorobenzene can be conventional in the field, and the separation and purification effect of the m-dichlorobenzene is not greatly influenced.
Wherein the pressure drop of the light ends column is preferably not more than 10mbar, more preferably 10mbar.
Wherein the light ends column feed temperature may be conventional in the art, preferably 139-145 ℃, more preferably 144.5 ℃.
Wherein, the top reflux temperature of the light component removal tower is preferably 45-55 ℃, more preferably 50 ℃.
Wherein, the top reflux of the light component removal tower is preferably 8-15, more preferably 10.
In the present utility model, preferably, when trichlorobenzene is further included in the mixed dichlorobenzene, the system further includes the ortho-column, and the ortho-extraction port of the meta-column B is connected to the feed port of the ortho-column.
Wherein the trichlorobenzene is a byproduct generated in the synthesis process of the m-dichlorobenzene, and is generally 1,2, 4-trichlorobenzene.
Wherein, the mass percentage of the trichlorobenzene to the mixed dichlorobenzene can be conventional in the field, and the effect of separating and purifying the m-dichlorobenzene is not greatly influenced.
Wherein the pressure drop of the ortho-column is preferably not more than 10mbar, more preferably 10mbar.
Wherein the feed temperature to the ortho-column may be conventional in the art, preferably 138-145 ℃, more preferably 143.3 ℃.
Wherein the reflux temperature at the top of the ortho-column is preferably 65-75deg.C, more preferably 70deg.C.
Wherein, the top reflux of the ortho-tower is preferably 1.5-3, more preferably 2.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred examples of the utility model.
The reagents and materials used in the present utility model are commercially available.
The utility model has the positive progress effects that:
(1) The rectification system has simple flow, does not need to adopt a rectification and crystallization composite process, and can achieve the purpose of purifying the m-dichlorobenzene only by rectification by singly relying on high-efficiency packing, so that the purity of the m-dichlorobenzene reaches more than 80 percent;
(2) The primary yield is high, and the yield of m-dichlorobenzene in the rectification process is as high as more than 98wt percent.
Drawings
FIG. 1 is a flow chart of a system for purifying m-dichlorobenzene from mixed dichlorobenzene of example 1.
Reference numerals:
t101-heavy ends removal column, T102-light ends removal column, T103-meta-position column A, T-meta-position column B, T-ortho-position column.
Detailed Description
The utility model is further illustrated by means of the following examples, which are not intended to limit the scope of the utility model. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
Example 1
Referring to fig. 1, the system for purifying m-dichlorobenzene in mixed dichlorobenzene in this embodiment includes a heavy removal column T101, a light removal column T102, a meta column A T103,103, a meta column B T104,104 and an ortho column T105, wherein the top of the heavy removal column T101 is connected to a feed inlet of the light removal column T102, a light component extraction outlet is provided at the top of the light removal column T102, a bottom of the light removal column T102 is connected to a feed inlet of the meta column A T103,103, a bottom of the meta column A T103,103 is connected to a feed inlet of the meta column B T104,104, a top of the meta column B T104,104 is connected to a feed inlet of the meta column A T, and a bottom of the meta column B T104,104 is connected to a feed inlet of the ortho column T105. The tower kettle of the heavy-removal tower T101 is connected with a stirring kettle, a kettle top outlet of the stirring kettle is connected with the tower kettle of the heavy-removal tower T101, a kettle bottom of the stirring kettle is connected with a heavy component extraction outlet and is used for extracting part of stirring kettle bottom liquid, the kettle bottom of the stirring kettle is also connected with a falling film reboiler C, and an outlet of the falling film reboiler C is connected with the tower kettle of the heavy-removal tower T101. The tower bottom of the light component removal tower T102 is connected with the inlet of a falling film reboiler D, the outlet of the falling film reboiler D is connected with the tower bottom of the light component removal tower T102, the tower bottom of the meta-position tower A T103 is connected with the inlet of a falling film reboiler A, and the outlet of the falling film reboiler A is connected with the tower bottom of the meta-position tower A T; the tower kettle of the meta-position tower B T is connected with the inlet of a falling film reboiler B, and the outlet of the falling film reboiler B is connected with the tower kettle of the meta-position tower B T104; the tower kettle of the ortho-position tower T105 is connected with the inlet of the falling film reboiler E, and the outlet of the falling film reboiler E is connected with the tower kettle of the ortho-position tower T105. The top of the light component removing tower T102 is provided with a light component extraction outlet, the top of the meta-position tower A T103 is provided with a meta-position extraction outlet, the top of the ortho-position tower T105 is provided with an ortho-position extraction outlet, and the tower bottom of the ortho-position tower T105 is provided with a trichlorobenzene extraction outlet. The heavy-removal tower T101, the light-removal tower T102, the meta-position tower A T103, the meta-position tower B T and the ortho-position tower T105 are all filler rectifying towers, the fillers of the meta-position tower A T103 and the meta-position tower B T are high-efficiency silk screen fillers, and the fillers of the heavy-removal tower T101, the light-removal tower T102 and the ortho-position tower T105 are plate ripple structured fillers. The theoretical plate numbers and feed positions of each column are shown in Table 1.
The mixed dichlorobenzene comprises 48% of m-dichlorobenzene, 24% of p-dichlorobenzene, 20% of o-dichlorobenzene, 4% of chlorobenzene, 2.9% of 1,2, 4-trichlorobenzene, 1% of heavy component and 0.1% of H 2 O. The mixed dichlorobenzene was fed into the above system from the feed inlet of the weight-removing column T101, and the pressure drop, the reflux ratio at the top of the column and the reflux temperature at the top of the column were shown in Table 1, respectively. Salt and heavy components are extracted from the bottom of a stirring kettle of the heavy component removal tower T101, light components are extracted from the top of the light component removal tower T102, m-dichlorobenzene is extracted from a top meta-position extraction port of a meta-position tower A T103, o-dichlorobenzene and p-dichlorobenzene are extracted from a top ortho-position extraction port of an ortho-position tower T105, and 1,2, 4-trichlorobenzene is extracted from a trichlorobenzene extraction port of a kettle of the ortho-position tower T105. The composition and mass of each stream in FIG. 1 are shown in Table 2, and the temperature, pressure and phase of each stream in FIG. 1 are shown in Table 3.
Table 1 system parameters and process parameters for each column of example 1
TABLE 2 Mass and composition Table for each stream
TABLE 3 various physical phase, temperature and pressure gauges
| Logistics number | Phase state | Temperature/. Degree.C | Pressure/ |
| 101 | Liquid phase | 120.0 | 3000 |
| 102 | Gas phase | 144.5 | 455 |
| 103 | Liquid phase | 80.0 | 3000 |
| 104 | Liquid phase | 139.9 | 3000 |
| 105 | Liquid phase | 93.5 | 3000 |
| 106 | Liquid phase | 142.3 | 3000 |
| 107 | Liquid phase | 131.7 | 3000 |
| 108 | Liquid phase | 143.3 | 3000 |
| 109 | Liquid phase | 131.6 | 3000 |
| 110 | Liquid phase | 139.5 | 3000 |
| 111 | Liquid phase | 102.2 | 3000 |
As can be seen from table 2, the purity of the m-dichlorobenzene separated and purified in this example was as high as 82%, and the total mass extracted from the meta-position extraction port was 747kg, and the recovery rate of m-dichlorobenzene was calculated to be 747×82%/(1300×48%) = 98.16%. The content of chlorobenzene in the light component separated by the light component removing tower is 97.5924 percent, so that high-concentration purification of chlorobenzene is realized; the purity of the trichlorobenzene extracted from the tower bottom of the light component removing tower is up to 99.9474%, the components extracted from the tower top of the light component removing tower are mainly o-dichlorobenzene and p-dichlorobenzene, the concentrations of the o-dichlorobenzene and p-dichlorobenzene are 40.3660% and 58.7847%, and the sum of the concentrations of the o-dichlorobenzene and p-dichlorobenzene reaches 99.1507%. Therefore, the separation system and the separation process realize the purification of the m-dichlorobenzene in the mixed dichlorobenzene with high purity and high yield, and simultaneously realize the recovery of the main impurity components chlorobenzene and trichlorobenzene with high purity and the recovery of the mixture of the o-dichlorobenzene and the p-dichlorobenzene with high purity.
As can be seen from table 3, the gas phase temperatures at the tops of the T103 and T104 are higher than 130 ℃, which can be used for regenerating steam, recovering heat and reducing energy consumption; by adopting the falling film reboiler, the residence time of the materials in the rectification process can be reduced, the heat exchange temperature difference is reduced, the coking phenomenon at high temperature is reduced, and the tar amount in the rectification process is reduced.
Claims (10)
1. A system for purifying m-dichlorobenzene from mixed dichlorobenzene, comprising: the device comprises a meta-position tower A and a meta-position tower B, wherein the tower bottom of the meta-position tower A is connected with the feed inlet of the meta-position tower B, the tower top of the meta-position tower B is connected with the feed inlet of the meta-position tower A, and a meta-position extraction outlet is arranged on the tower top of the meta-position tower A; the meta-position tower A and the meta-position tower B are filler rectifying towers, wherein the filler is high-efficiency silk screen filler, and the theoretical plate numbers of the meta-position tower A and the meta-position tower B are not less than 100.
2. The system for purifying m-dichlorobenzene in mixed dichlorobenzene of claim 1, wherein the theoretical plate number of the meta-column a is 100-120, and the theoretical plate number of the meta-column B is 100-120.
3. The system for purifying m-dichlorobenzene in mixed dichlorobenzene according to claim 1, wherein the feed inlet of meta-column a is positioned in the middle of the column;
and the tower bottom of the meta-position tower A is also connected with a reboiler A, and the outlet of the reboiler A is connected with the tower bottom of the meta-position tower A.
4. The system for purifying m-dichlorobenzene in mixed dichlorobenzene according to claim 1, wherein the feed inlet of meta-column B is positioned in the upper section of the column;
the tower bottom of the meta-position tower B is also connected with a reboiler B, and the outlet of the reboiler B is connected with the tower bottom of the meta-position tower B;
and the tower bottom of the meta-position tower B is also provided with an ortho-position extraction outlet.
5. The system for purifying m-dichlorobenzene in mixed dichlorobenzene as claimed in claim 1, wherein said system further comprises a de-heavies column, the top of said de-heavies column being connected to the feed inlet of said meta-column a.
6. The system for purifying m-dichlorobenzene in mixed dichlorobenzene as claimed in claim 5, wherein said de-weight column is a packed rectifying column with plate ripple structured packing, and the theoretical plate number of said de-weight column is 18-25; the feeding position of the heavy-removal tower is the middle part of the tower; the tower bottom of the weight removing tower is also connected with a film scraping evaporator or a stirring kettle, and a kettle top outlet of the stirring kettle is connected with the tower bottom of the weight removing tower and is used for refluxing the evaporated gas components in the stirring kettle to the tower bottom of the weight removing tower; and the bottom of the stirring kettle is also connected with a reboiler C, and the outlet of the reboiler C is connected with the kettle of the heavy-removal tower.
7. The system for purifying m-dichlorobenzene in mixed dichlorobenzene as claimed in claim 1, wherein said system further comprises a light component removal column, wherein a bottom of said light component removal column is connected to a feed port of said meta-column a for removing light components from mixed dichlorobenzene.
8. The system for purifying m-dichlorobenzene in mixed dichlorobenzene of claim 7, wherein said light ends removal column is a packed rectifying column of plate ripple structured packing; the theoretical plate number of the light component removing tower is 15-25; the position of the feed inlet of the light component removing tower is the upper half section of the light component removing tower.
9. The system for purifying m-dichlorobenzene in mixed dichlorobenzene as claimed in claim 1, wherein said system further comprises an ortho-column, said ortho-column being a rectifying column, and a feed inlet of said ortho-column being connected to a bottom of said meta-column B for separating o-dichlorobenzene and p-dichlorobenzene from a bottom liquid of said meta-column B.
10. The system for purifying m-dichlorobenzene in mixed dichlorobenzene according to claim 9, wherein said ortho-column is a packed rectifying column of plate corrugated structured packing; the theoretical plate number of the ortho-position tower is 15-25; the position of the feed inlet of the ortho-position column is the lower half section of the ortho-position column.
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