CN103432761A - Distillation equipment and method for separating dichlorobenzene isomers - Google Patents

Distillation equipment and method for separating dichlorobenzene isomers Download PDF

Info

Publication number
CN103432761A
CN103432761A CN2013103635257A CN201310363525A CN103432761A CN 103432761 A CN103432761 A CN 103432761A CN 2013103635257 A CN2013103635257 A CN 2013103635257A CN 201310363525 A CN201310363525 A CN 201310363525A CN 103432761 A CN103432761 A CN 103432761A
Authority
CN
China
Prior art keywords
tower
dichlorohenzene
paracide
rectifying
dichlorobenzene
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2013103635257A
Other languages
Chinese (zh)
Other versions
CN103432761B (en
Inventor
李群
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201310363525.7A priority Critical patent/CN103432761B/en
Publication of CN103432761A publication Critical patent/CN103432761A/en
Application granted granted Critical
Publication of CN103432761B publication Critical patent/CN103432761B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses distillation equipment and method for separating dichlorobenzene isomers. The distillation equipment comprises a dividing wall tower, a tower kettle reboiler and a tower top condenser, wherein the dividing wall tower comprises a middle tower region, a tower top distillation section arranged above the middle tower region and used for performing distillation and separation on m-dichlorobenzene and p-dichlorobenzene, and a tower kettle stripping section arranged below the middle tower region and used for stripping and separating m-dichlorobenzene and o-dichlorobenzene; the middle tower region is divided into a pre-separation tower region and a finished product separation tower region by a baffle plate arranged in a longitudinal direction; the pre-separation tower region is parallel to the finished product separation tower region; the pre-separation tower region comprises an upper feeding distillation section and a lower feeding stripping section; the finished product separation tower comprises an upper m-dichlorobenzene/p-dichlorobenzene stripping section and a lower p-dichlorobenzene/o-dichlorobenzene distillation section. According to the distillation equipment, the dichlorobenzene isomers, namely the m-dichlorobenzene, the p-dichlorobenzene and o-dichlorobenzene can be separated in a distillation tower through the dividing wall tower, so that the energy consumption, the equipment investment and the occupied area are reduced.

Description

The rectifying device and the rectificating method that separate the dichloro-benzenes isomer
Technical field
The rectifying that the present invention relates to the dichloro-benzenes isomer separates, and more specifically, relates to a kind of rectifying device and rectificating method that uses partition tower compartment dichloro-benzenes, paracide and o-dichlorohenzene.
Background technology
In the chemical products production process, often invest hugely, the most complicated part is separation and the purification of product mixture after reaction, all can be applied to this unit process of rectifying in nearly all organic chemical industry's production process.Rectifying is very ripe in contemporary chemical process, and application widely.But the energy consumption of distillation process is huge, in general chemical process the energy consumption of 40-70% for separating of product mixture, this wherein rectifying account for more than 90% again.Along with rising steadily of energy prices, the power-saving technology of research distillation process is extremely important, and by the production process of up-to-date Finestill energy-saving technological transformation traditional product, has great economic worth and realistic meaning.
Traditional dichloro-benzenes isomer separates and at least needs two above rectifying columns, and mixture is downward by tower top, and the concentration of intermediate component paracide increases gradually along with the reduction of light component m-dichlorobenzene; Approaching the tower reactor place, the concentration of paracide increases and reduces along with heavy component o-dichlorohenzene concentration.This can cause paracide that air-teturning mixed phenomenon occurs in rectifying column, thereby causes separative efficiency to reduce.In addition, consider that energy consumption is huge, in actual industrial production, the general isomer mixture that adopts rectifying, these three techniques of crystallization and absorption to solve m-dichlorobenzene, paracide and o-dichlorohenzene separates.Invest huge and technical sophistication, and need high number of theoretical plate, cause most of enterprise all can not effectively carry out separating fully of m-dichlorobenzene, paracide and o-dichlorohenzene.
The rectifying device that for this reason, need to be able to improve product purity, reduction energy consumption, minimizing equipment investment and floor space separates the dichloro-benzenes isomer with method.
Summary of the invention
The objective of the invention is to adopt the control parameter of optimizing, complete dichlorobenzene isomer in a partition tower, it is separating of m-dichlorobenzene, paracide and o-dichlorohenzene, under the prerequisite that obtains highly purified m-dichlorobenzene, paracide and o-dichlorohenzene, compare with traditional separating technology and lower energy consumption, minimizing equipment investment and floor space.Therefore separate described three kinds of dichlorobenzene isomers because the present invention adopts the partition tower, there is no the back-mixing of material and improve separative efficiency, thereby realize the separation of three kinds of dichlorobenzene isomers of minimum boiling-point difference.
According to an aspect of the present invention, a kind of rectifying device that separates the dichloro-benzenes isomer is provided, described rectifying device comprises a partition tower, be connected to the partition tower tower reactor the tower reactor reboiler and be connected to the overhead condenser of the tower top of partition tower, wherein the dichloro-benzenes isomer comprises m-dichlorobenzene, paracide and o-dichlorohenzene, and the partition tower comprises:
The inter-chamber tower district, the baffle for separating that described inter-chamber tower district is arranged along the longitudinal direction becomes parallel pre-separation tower district and finished product knockout tower district, pre-separation tower district is comprised of top charging rectifying section and underfeed stripping section, finished product knockout tower district by between top, paracide stripping section and bottom form, o-dichlorohenzene rectifying section;
The tower top rectifying section, described tower top rectifying section is arranged on the top in inter-chamber tower district and for rectifying compartment dichloro-benzenes and paracide; With
The tower reactor stripping section, the tower reactor stripping section is arranged on the below in inter-chamber tower district and for carrying cut from paracide and o-dichlorohenzene.
The theoretical cam curve in pre-separation tower district in the scope of 60-200 piece, a plate between 120 theoretical plates of the 20th theoretical plate to that feedboard is pre-separation tower district.
Between tower top rectifying section and top, the paracide stripping section form between, paracide knockout tower district,, the theoretical cam curve in paracide knockout tower district is in the scope of 100-360 piece.
Further, the theoretical cam curve of tower top rectifying section is in the scope of 50-280 piece.
Bottom forms, o-dichlorohenzene knockout tower district, o-dichlorohenzene rectifying section and tower reactor stripping section, to the theoretical cam curve in, o-dichlorohenzene knockout tower district in the scope of 120-240 piece.
Further, bottom to the theoretical cam curve of, o-dichlorohenzene rectifying section in the scope of 40-150 piece.
Preferably, the overhead reflux liquid distribution ratio of partition tower is in the scope of 20-40%, and tower reactor gas distribution ratio is in the scope of 30-60%, and tower top pressure is in the scope of 10-100kPa, and reflux ratio is in the scope of 7-100.
According to another aspect of the present invention, provide a kind of rectificating method that uses above-mentioned rectifying device to separate the dichloro-benzenes isomer, comprise the following steps:
Compartment dichloro-benzenes and described o-dichlorohenzene in the pre-separation tower district ,Bing top charging rectifying section of the mixture inflow partition tower of dichloro-benzenes isomer and underfeed stripping section;
Between, the mixture of paracide with dew point vapour phase form flow between tower top rectifying section and top, paracide stripping section be separated into m-dichlorobenzene and paracide, the mixture of, o-dichlorohenzene is flowed into tower reactor stripping section and bottom to, o-dichlorohenzene rectifying section and is separated into paracide and o-dichlorohenzene with the bubble point liquid form; With
From the overhead extraction m-dichlorobenzene, from tower reactor extraction o-dichlorohenzene, from finished product knockout tower district's extraction paracide, thereby complete separating of m-dichlorobenzene, paracide and o-dichlorohenzene.
In described rectificating method, between, the separation of the mixture of paracide is further comprising the steps of:, the mixture of paracide is between tower top rectifying section and top, in the paracide stripping section, rectifying separates, the vapor phase stream obtained via overhead condenser condensation rear section as m-dichlorobenzene from overhead extraction, the remainder of vapor phase stream is back in the partition tower.Separation to the mixture of, o-dichlorohenzene is further comprising the steps of: the mixture of, o-dichlorohenzene is separated rectifying in, o-dichlorohenzene rectifying section in tower reactor stripping section and bottom, the liquid phase stream part obtained is as o-dichlorohenzene by from the tower reactor extraction, and via the heating of tower reactor reboiler, vaporization is back in the partition tower remainder of liquid phase stream.The logistics refluxed repeats rectifying and separates in the partition tower, until m-dichlorobenzene, paracide and o-dichlorohenzene all separate.
Preferably, the overhead reflux liquid distribution ratio of partition tower is in the scope of 20-40%, and tower reactor gas distribution ratio is in the scope of 30-60%, and tower top pressure is in the scope of 10-100kPa, and reflux ratio is in the scope of 7-100.
The accompanying drawing explanation
Above-mentioned and other aspect of the present invention and feature will be from presenting the explanation of embodiment is clear below in conjunction with accompanying drawing, in the accompanying drawings:
Fig. 1 is that demonstration is according to the structure of the rectifying device of the embodiment of the present invention and the schematic diagram of rectification process flow process.
The specific embodiment
The present invention separates three kinds of dichloro-benzenes isomers, i.e. m-dichlorobenzene, paracide and o-dichlorohenzene by rectifying.The rectifying separation refers in rectifying column by liquid is constantly vaporized, liquefied, by gas molecule rectifying wherein out, thereby realize the separation of many kinds of substance, wherein rectifying section is the process of the continuous saturated rising of gaseous molecular, and stripping section is the process of the continuous condensation of liquid molecule.Rectifying device according to the present invention is realized separating fully of three kinds of dichloro-benzenes isomers with rectificating method in a partition tower.Describe illustrative of the present invention, non-limiting example in detail hereinafter with reference to Fig. 1, rectifying device according to the present invention and method are further described.
Comprise a partition tower 1, be connected to the tower reactor reboiler 2 of partition tower tower reactor and be connected to the condenser 3 of partition column overhead according to the rectifying device of separation dichloro-benzenes isomer of the present invention.Partition tower 1 comprises the inter-chamber tower district, be arranged on the tower top rectifying section 4 of top, inter-chamber tower district and be arranged on the tower reactor stripping section 5 of below, inter-chamber tower district, wherein tower top rectifying section 4 is for rectifying compartment dichloro-benzenes and paracide, and tower reactor stripping section 5 is for carrying cut from paracide and o-dichlorohenzene.Referring to Fig. 1, the dividing plate 18 that the inter-chamber tower district is arranged along the longitudinal direction is separated into parallel pre-separation tower district and finished product knockout tower district.Pre-separation tower district is comprised of top charging rectifying section 6 and underfeed stripping section 7, with compartment dichloro-benzenes and o-dichlorohenzene.Finished product knockout tower district by between top, paracide stripping section 8 and bottom form, o-dichlorohenzene rectifying section 9.Between tower top rectifying section 4 and top, paracide stripping section 8 form between, paracide knockout tower district, bottom forms, o-dichlorohenzene knockout tower district, o-dichlorohenzene rectifying section 9 and tower reactor stripping section 5.
According to the present invention, the pre-separation tower district , top charging rectifying section 6 that three kinds of dichloro-benzenes admixture of isomeric compound enter partition tower 1 with complete separating of light component m-dichlorobenzene and heavy component o-dichlorohenzene in underfeed stripping section 7.Between containing, the light component of paracide mixture enter between, paracide knockout tower district, and between tower top rectifying section 4 and top, in paracide stripping section 8, complete separating of m-dichlorobenzene and paracide.Contain heavy component to, o-dichlorohenzene mixture enter to, ,Bing bottom, o-dichlorohenzene knockout tower district to, o-dichlorohenzene rectifying section 9 with complete separating of paracide and o-dichlorohenzene in tower reactor stripping section 5.Between, the tower kettle product in paracide knockout tower district and the overhead product in, o-dichlorohenzene knockout tower district is merged to extraction, obtain paracide logistics 12.The tower top vapor phase stream is coagulated rear section as m-dichlorobenzene logistics 11 extraction entirely through condenser 3, and the remainder of vapor phase stream is back in partition tower 1.The tower reactor liquid phase stream is through reboiler 2 parts vaporizations extraction o-dichlorohenzene logistics 13, thereby between completing in a partition tower, to the separation of, three kinds of isomers of o-dichlorohenzene.
The dividing plate that utilization of the present invention arranges along the longitudinal direction in rectifying column is divided into pre-separation district and finished product Disengagement zone by common rectifying column, has realized the separation function of three towers.Separate three kinds of isomers of dichloro-benzenes in a rectifying column, at first between being separated into through pre-separation tower district, the mixture of the mixture of paracide isomers and neighbour, paracide isomers, then in follow-up finished product Disengagement zone between to the finishing column district with carry out rectifying in adjacency pair finishing column district and separate, obtain qualified between, to, o-dichlorohenzene product.Position by each tower section number of theoretical plate, charging and extraction reasonable in design, overhead reflux liquid distribution ratio, tower reactor gas distribution ratio etc., formulate rational process operation parameter, technological parameters such as tower top pressure, tower reactor temperature (rising vapour amount), reflux ratio, use a rectifying column to obtain up-to-standard m-dichlorobenzene product, paracide product and o-dichlorohenzene product simultaneously, and do not need the operations such as crystallization and adsorbing separation.Therefore, the present invention can significantly reduce the energy consumption of separation, reduces equipment investment and floor space, and technique is simple and easy operating.
Particularly, according to the present invention, the theoretical cam curve in pre-separation tower district in the scope of 60-200 piece, a plate between 120 theoretical plates of the 20th theoretical plate to that feedboard is pre-separation tower district.Between, the theoretical cam curve in paracide knockout tower district in the scope of 100-360 piece, wherein the theoretical cam curve of tower top rectifying section 4 is in the scope of 50-280 piece.To the theoretical cam curve in, o-dichlorohenzene knockout tower district in the scope of 120-240 piece, its middle and lower part to the theoretical cam curve of, o-dichlorohenzene rectifying section 9 in the scope of 40-150 piece.In addition, the overhead reflux liquid distribution ratio of partition tower 1 is in the scope of 20-40%, and tower reactor gas distribution ratio is in the scope of 30-60%, and tower top pressure is in the scope of 10-100kPa, and reflux ratio is in the scope of 7-100.By adopting the technological parameter of above-mentioned optimization, can in a partition tower, complete the separation fully of three kinds of dichlorobenzene isomers.
Next, the distillation process that separates the dichloro-benzenes isomer with reference to the above-mentioned rectifying device of Fig. 1 explanation use according to the present invention.
Between containing, the mixing logistics 10 of, o-dichlorohenzene is flowed into to compartment dichloro-benzenes and o-dichlorohenzene in the pre-separation tower district , top charging rectifying section 6 of partition towers 1 and underfeed stripping section 7.The tower top component in pre-separation tower district be between, the mixture of paracide, this mixture with dew point vapour phase form flow between tower top rectifying section 4 and top, paracide stripping section 8.The tower reactor component in pre-separation tower district is the mixture to, o-dichlorohenzene, and this mixture flows into tower reactor stripping section 5 and bottom to, o-dichlorohenzene rectifying section 9 with the bubble point liquid form.
Between, the mixture of paracide between tower top rectifying section 4 and top, in paracide stripping section 8 further rectifying separate.This rectifying separate the vapor phase stream 16 that obtains through overhead condenser 3 condensation rear sections as m-dichlorobenzene finished product extraction logistics 11 from overhead extraction, the remainder of vapor phase stream 16 is back in partition tower 1 as withdrawing fluid 14.Withdrawing fluid 14 is reallocated in the lower end of tower top rectifying section 4, and a part is as the backflow in pre-separation tower district, and another part as between top, the backflow of paracide stripping section 8, and repeat rectifying separate in the partition tower.
To the mixture of, o-dichlorohenzene in tower reactor stripping section 5 and bottom in, o-dichlorohenzene rectifying section 9 further rectifying separate.This rectifying separate liquid phase stream 17 parts that obtain as o-dichlorohenzene finished product logistics 13 by from the tower reactor extraction, the remainder of liquid phase stream 17 rises as vaporization logistics 15 after via 2 heating of tower reactor reboiler.The vaporization logistics 15 risen is back in partition tower 1, through tower reactor stripping section 5 time, be reallocated, a part is as the backflow in pre-separation tower district, and another part as bottom between, o-dichlorohenzene rectifying section 9 and top, the vapour phase of paracide stripping section 8 refluxes.Between top, the backflow of paracide stripping section 8 part as the logistics 12 of paracide finished product between top, paracide stripping section 8 and bottom be to Ta district extraction between, o-dichlorohenzene rectifying section 9, remainder is the backflow to, o-dichlorohenzene rectifying section 9 as bottom.The backflow of flowing back to partition tower 1 repeats as mentioned above rectifying and separates in the partition tower, until m-dichlorobenzene, paracide and o-dichlorohenzene all separate.
Below will illustrate illustratively that described embodiment is only illustration purpose, and does not mean to limit the scope of the invention according to several specific embodiments of the present invention.
The first embodiment
Between adopting partition tower 1 to separate to contain according to the first embodiment of the present invention, to the dichloro-benzenes raw material of, adjacent isomer, described mixture is comprised of 8% m-dichlorobenzene, 46% paracide and 46% o-dichlorohenzene.Between, the mixture of, o-dichlorohenzene is entered to partition tower 1 with the bubble point of 1000kg/hr flow.Pre-separation tower number of theoretical plate is 130, the 82nd theoretical plate that feedboard is pre-separation tower district.Between, the number of theoretical plate in paracide knockout tower district is 280, wherein tower top rectifying section 4 is 206, between top, paracide stripping section 8 is 74.Number of theoretical plate to, o-dichlorohenzene knockout tower district is 130, and its middle and lower part is 50 to, o-dichlorohenzene rectifying section 9, and tower reactor stripping section 5 is 80.Reflux ratio is 43, and tower top pressure is 56kPa, and overhead reflux liquid distribution ratio is 26%, and tower reactor gas distribution ratio is 52%, and the load of reboiler 2 is 548.6kw.Under above-mentioned theory plate number and technological parameter, it is m-dichlorobenzene 99.5%, paracide 99.9% and o-dichlorohenzene 99.9% that rectifying separates the product purity obtained.
The second embodiment
Between adopting according to a second embodiment of the present invention partition tower 1 to separate to contain, to the dichloro-benzenes raw material of, adjacent isomer, described mixture is comprised of 54% m-dichlorobenzene, 24% paracide and 22% o-dichlorohenzene.Between, the mixture of, o-dichlorohenzene is entered to partition tower 1 with the bubble point of 1000kg/hr flow.Pre-separation tower number of theoretical plate is 180, the 69th theoretical plate that feedboard is pre-separation tower district.Between, the number of theoretical plate in paracide knockout tower district is 240, wherein tower top rectifying section 4 is 85, between top, paracide stripping section 8 is 155.Number of theoretical plate to, o-dichlorohenzene knockout tower district is 160, and its middle and lower part is 96 to, o-dichlorohenzene rectifying section 9, and tower reactor stripping section 5 is 64.Reflux ratio is 16.2, and tower top pressure is 12kPa, and overhead reflux liquid distribution ratio is 37%, and tower reactor gas distribution ratio is 45%, and the load of reboiler 2 is 657kw.Under above-mentioned theory plate number and technological parameter, it is m-dichlorobenzene 99.5%, paracide 99.8% and o-dichlorohenzene 99.9% that rectifying separates the product purity obtained.
The 3rd embodiment
Between a third embodiment in accordance with the invention adopts partition tower 1 to separate to contain, to the dichloro-benzenes raw material of, adjacent isomer, described mixture is comprised of 5% m-dichlorobenzene, 60% paracide and 35% o-dichlorohenzene.Between, the mixture of, o-dichlorohenzene is entered to partition tower 1 with the bubble point of 1000kg/hr flow.Pre-separation tower number of theoretical plate is 83, the 58th theoretical plate that feedboard is pre-separation tower district.Between, the number of theoretical plate in paracide knockout tower district is 278, wherein tower top rectifying section 4 is 173, between top, paracide stripping section 8 is 105.Number of theoretical plate to, o-dichlorohenzene knockout tower district is 155, and its middle and lower part is 78 to, o-dichlorohenzene rectifying section 9, and tower reactor stripping section 5 is 77.Reflux ratio is 71, and tower top pressure is 350kPa, and overhead reflux liquid distribution ratio is 24%, and tower reactor gas distribution ratio is 46%, and the load of reboiler 2 is 596kw.Under above-mentioned theory plate number and technological parameter, it is m-dichlorobenzene 99.5%, paracide 99.8% and o-dichlorohenzene 99.8% that rectifying separates the product purity obtained.
Traditional compartment, to the rectifying device of, three kinds of isomers of o-dichlorohenzene, need three rectifying columns to realize the separation of each material, and the present invention has reduced two rectifying columns and subsidiary rectifying column tower top condenser and tower reactor reboiler thereof by adopting the partition tower can in a rectifying column, complete the separation of three kinds of dichloro-benzenes isomers.Therefore, reduced the condensation of a large amount of materials and heated again the energy consumption process of vaporization according to rectifying device of the present invention and method, avoid the back-mixing effect of intermediate component, and reduced feedboard and the different back-mixings that cause of material composition on reclaiming plate, significantly improved rectification efficiency.In addition, due to the auxiliary equipment of the quantity that has reduced rectifying column and rectifying column, significantly reduced the equipment investment expense and reduced floor space.
Although some embodiment of total inventive concept of the present invention are shown and explanation, but those of ordinary skills will be understood that, in the situation that do not deviate from spirit of the present invention and principle can make a change these embodiment, this bright scope claims with and equivalent in limit.

Claims (10)

1. a rectifying device that separates the dichloro-benzenes isomer, comprise a partition tower, be connected to described partition tower tower reactor the tower reactor reboiler and be connected to the overhead condenser of the tower top of described partition tower, wherein said dichloro-benzenes isomer comprises m-dichlorobenzene, paracide and o-dichlorohenzene, and described partition tower comprises:
The inter-chamber tower district, the baffle for separating that described inter-chamber tower district is arranged along the longitudinal direction becomes parallel pre-separation tower district and finished product knockout tower district, described pre-separation tower district is comprised of top charging rectifying section and underfeed stripping section, described finished product knockout tower district by between top, paracide stripping section and bottom form, o-dichlorohenzene rectifying section;
The tower top rectifying section, described tower top rectifying section is arranged on the top in described inter-chamber tower district and for rectifying compartment dichloro-benzenes and paracide; With
The tower reactor stripping section, described tower reactor stripping section is arranged on the below in described inter-chamber tower district and for carrying cut from paracide and o-dichlorohenzene.
2. rectifying device according to claim 1, wherein, the theoretical cam curve in described pre-separation tower district in the scope of 60-200 piece, a plate between 120 theoretical plates of the 20th theoretical plate to that feedboard is described pre-separation tower district.
3. rectifying device according to claim 1, wherein, between described tower top rectifying section and described top, the paracide stripping section form between, paracide knockout tower district, described, the theoretical cam curve in paracide knockout tower district are in the scope of 100-360 piece.
4. rectifying device according to claim 3, wherein, the theoretical cam curve of described tower top rectifying section is in the scope of 50-280 piece.
5. rectifying device according to claim 1, wherein, described bottom forms, o-dichlorohenzene knockout tower district, o-dichlorohenzene rectifying section and described tower reactor stripping section, and the described theoretical cam curve to, o-dichlorohenzene knockout tower district is in the scope of 120-240 piece.
6. rectifying device according to claim 5, wherein, described bottom to the theoretical cam curve of, o-dichlorohenzene rectifying section in the scope of 40-150 piece.
7. rectifying device according to claim 1, wherein, the overhead reflux liquid distribution ratio of described partition tower is in the scope of 20-40%, and tower reactor gas distribution ratio is in the scope of 30-60%, tower top pressure is in the scope of 10-100kPa, and reflux ratio is in the scope of 7-100.
8. a rectificating method that uses rectifying device according to claim 1 to separate the dichloro-benzenes isomer comprises the following steps:
The mixture of dichloro-benzenes isomer flows into the described pre-separation tower district of described partition tower, and separates described m-dichlorobenzene and described o-dichlorohenzene at described top charging rectifying section with in described underfeed stripping section;
Between, the mixture of paracide with dew point vapour phase form flow between described tower top rectifying section and described top, paracide stripping section be separated into m-dichlorobenzene and paracide, the mixture of, o-dichlorohenzene is flowed into described tower reactor stripping section and described bottom to, o-dichlorohenzene rectifying section and is separated into paracide and o-dichlorohenzene with the bubble point liquid form; With
From the overhead extraction m-dichlorobenzene, from tower reactor extraction o-dichlorohenzene, from described finished product knockout tower district's extraction paracide, thereby complete separating of m-dichlorobenzene, paracide and o-dichlorohenzene.
9. rectificating method according to claim 8, wherein:
Described, the separation of the mixture of paracide are further comprising the steps of:
Described, the mixture of paracide are between described tower top rectifying section and described top, in the paracide stripping section, rectifying separates, the vapor phase stream obtained via described overhead condenser condensation rear section as m-dichlorobenzene from overhead extraction, the remainder of described vapor phase stream is back in described partition tower;
The separation of the described mixture to, o-dichlorohenzene is further comprising the steps of:
The described mixture to, o-dichlorohenzene separates rectifying in, o-dichlorohenzene rectifying section in described tower reactor stripping section and described bottom, the liquid phase stream part obtained is as o-dichlorohenzene by from the tower reactor extraction, and via described tower reactor reboiler heating, vaporization is back in described partition tower the remainder of described liquid phase stream; And
The logistics refluxed repeats rectifying and separates in described partition tower, until m-dichlorobenzene, paracide and o-dichlorohenzene all separate.
10. rectificating method according to claim 8, wherein, the overhead reflux liquid distribution ratio of described partition tower is in the scope of 20-40%, and tower reactor gas distribution ratio is in the scope of 30-60%, tower top pressure is in the scope of 10-100kPa, and reflux ratio is in the scope of 7-100.
CN201310363525.7A 2013-08-20 2013-08-20 Be separated the rectificating method of dichloro-benzenes isomer Active CN103432761B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310363525.7A CN103432761B (en) 2013-08-20 2013-08-20 Be separated the rectificating method of dichloro-benzenes isomer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310363525.7A CN103432761B (en) 2013-08-20 2013-08-20 Be separated the rectificating method of dichloro-benzenes isomer

Publications (2)

Publication Number Publication Date
CN103432761A true CN103432761A (en) 2013-12-11
CN103432761B CN103432761B (en) 2015-07-29

Family

ID=49686532

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310363525.7A Active CN103432761B (en) 2013-08-20 2013-08-20 Be separated the rectificating method of dichloro-benzenes isomer

Country Status (1)

Country Link
CN (1) CN103432761B (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107340346A (en) * 2017-08-07 2017-11-10 安徽东至广信农化有限公司 The quick determination method of micro dichloro-benzenes in a kind of chlorination benzaldehyde product
CN109320417A (en) * 2018-11-29 2019-02-12 武汉有机实业有限公司 Utilize the device and method of partition tower purification Ergol
CN109529394A (en) * 2019-01-10 2019-03-29 青海黄河上游水电开发有限责任公司光伏产业技术分公司 Partition wall rectifying device and rectifying method thereof
CN110724029A (en) * 2019-10-25 2020-01-24 福州大学 Equipment and process for recovering and purifying photochemical reaction solvent o-dichlorobenzene
CN111194300A (en) * 2017-09-25 2020-05-22 韩华思路信(株) Dividing wall distillation column and method for purifying vinylidene chloride by using the same
CN111659150A (en) * 2020-06-18 2020-09-15 东华工程科技股份有限公司 Device and method for refining low-carbon alcohol by using dividing wall tower
CN113144655A (en) * 2021-04-28 2021-07-23 安徽金轩科技有限公司 Jiale musk rectification unit and rectification process thereof
WO2022045960A1 (en) * 2020-08-28 2022-03-03 Sui Jianjun Method and device for purification of p-dichlorobenzene

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1467202A (en) * 2002-06-14 2004-01-14 Process for the purification of mixtures of toluenediisocyanate incorporating a dividing-wall distillation column
CN1496978A (en) * 2002-10-22 2004-05-19 Method for purifying toluene vulcabond by recuperative distilling tower for final purifying
CN102224133A (en) * 2008-10-02 2011-10-19 陶氏环球技术有限责任公司 Apparatus, systems, and methods for purification of isocyanate mixtures

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1467202A (en) * 2002-06-14 2004-01-14 Process for the purification of mixtures of toluenediisocyanate incorporating a dividing-wall distillation column
CN1496978A (en) * 2002-10-22 2004-05-19 Method for purifying toluene vulcabond by recuperative distilling tower for final purifying
US20040118672A1 (en) * 2002-10-22 2004-06-24 Grun Marcus Paul Process for the purification of toluenediisocyanate incorporating a dividing-wall distillation column for the final purification
CN102224133A (en) * 2008-10-02 2011-10-19 陶氏环球技术有限责任公司 Apparatus, systems, and methods for purification of isocyanate mixtures

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107340346A (en) * 2017-08-07 2017-11-10 安徽东至广信农化有限公司 The quick determination method of micro dichloro-benzenes in a kind of chlorination benzaldehyde product
CN111194300A (en) * 2017-09-25 2020-05-22 韩华思路信(株) Dividing wall distillation column and method for purifying vinylidene chloride by using the same
CN111194300B (en) * 2017-09-25 2022-09-13 韩华思路信(株) Dividing wall distillation column and method for purifying vinylidene chloride by using the same
US11707697B2 (en) 2017-09-25 2023-07-25 Hanwha Solutions Corporation Dividing wall distillation column and method for refining vinylidene dichloride by using same
CN109320417A (en) * 2018-11-29 2019-02-12 武汉有机实业有限公司 Utilize the device and method of partition tower purification Ergol
CN109529394A (en) * 2019-01-10 2019-03-29 青海黄河上游水电开发有限责任公司光伏产业技术分公司 Partition wall rectifying device and rectifying method thereof
CN110724029A (en) * 2019-10-25 2020-01-24 福州大学 Equipment and process for recovering and purifying photochemical reaction solvent o-dichlorobenzene
CN110724029B (en) * 2019-10-25 2021-05-18 福州大学 Equipment and process for recovering and purifying photochemical reaction solvent o-dichlorobenzene
CN111659150A (en) * 2020-06-18 2020-09-15 东华工程科技股份有限公司 Device and method for refining low-carbon alcohol by using dividing wall tower
WO2022045960A1 (en) * 2020-08-28 2022-03-03 Sui Jianjun Method and device for purification of p-dichlorobenzene
CN113144655A (en) * 2021-04-28 2021-07-23 安徽金轩科技有限公司 Jiale musk rectification unit and rectification process thereof
CN113144655B (en) * 2021-04-28 2022-06-21 安徽金轩科技有限公司 Jiale musk rectification unit and rectification process thereof

Also Published As

Publication number Publication date
CN103432761B (en) 2015-07-29

Similar Documents

Publication Publication Date Title
CN103432761A (en) Distillation equipment and method for separating dichlorobenzene isomers
CN102355928B (en) Dividing wall distillation columns for production of high-purity 2-ethylhexanol and fractionation method using same
US8932434B2 (en) Dividing wall distillation column for producing high purity acrylic acid and fractional distillation method using the same
CN104027995B (en) The method of Separation of Benzene, ethylbenzene, many ethylbenzene, heavy constituent mixing system
JP5783491B2 (en) Separation wall distillation column for producing high purity neopentyl glycol and production method using the same
Zhang et al. A novel multi-effect methanol distillation process
JP2014508736A (en) Separation wall distillation column for producing high purity 2-ethylhexyl acrylate and production method using the same
Gao et al. A combination of pressure-swing and extractive distillation for separating complex binary azeotropic system
CN103813841A (en) Dual-mode dividing wall column
CN103664446A (en) Technology for separating n-hexane-methylcyclopentane through extractive distillation
CN104610022A (en) Method for separating ethanol-propyl acetate azeotrope through continuous extractive rectification
CN103463826B (en) Rectification and separation method
CN103694088A (en) Method for separating ethylene glycol mixture series
CN102807222B (en) Purification method of silicon tetrachloride
KR101632772B1 (en) Distillation device for separating petane mixure and process of separating petane mixture
CN104058913A (en) Method and device for extracting durene from methanol synthetic oil
CN203060873U (en) Continuous rectifying tower for N-methylaniline
CN102285658A (en) Multistage fully thermally coupled rectification production device and process method for preparing ultra-pure trichlorosilane
CN202438166U (en) Separating device with partition wall for purifying tert-butyl acetate
CN104693005A (en) New process for separating methanol-propyl formate azeotrope through extractive distillation
CN105669353A (en) Ethylbenzene and styrene separation method
CN104415567A (en) Novel double-effect rectifying process
CN101787306B (en) Method and device for refining methanol synthetic oil
CN208482029U (en) Butene-1 separator
CN104370704A (en) Mono-ethylene glycol purification and recovery method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant