CN102659506A - Side stream rectification continuous separation method of chlorobenzene and dichlorobenzene - Google Patents
Side stream rectification continuous separation method of chlorobenzene and dichlorobenzene Download PDFInfo
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- CN102659506A CN102659506A CN2012101233048A CN201210123304A CN102659506A CN 102659506 A CN102659506 A CN 102659506A CN 2012101233048 A CN2012101233048 A CN 2012101233048A CN 201210123304 A CN201210123304 A CN 201210123304A CN 102659506 A CN102659506 A CN 102659506A
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Abstract
The invention belongs to the fine chemical engineering field, and relates to a side stream rectification continuous separation method of chlorobenzene and dichlorobenzene. The method includes the particular steps that mixed materials containing chlorobenzene, para-dichlorobenzene, ortho-dichlorobenzene and poly-dichlorobenzene are continuously conveyed to a preheater through a pump to be preheated; the preheated mixed materials enter a rectifying tower from the middle portion of the rectifying tower with side stream withdrawing, and are heated till boiling through a reboiler at the bottom of the tower to perform rectification separation; chlorobenzene with the content over 99.5% is continuously withdrawn from the top of the tower, and the mixed dichlorobenzene with the content over 99.5 % is continuously withdrawn from the rectifying tower lateral line; trichlorobenzene and a small amount of para-dichlorobenzene and ortho-dichlorobenzene are discharged continuously through a tower kettle, and the purpose of chlorobenzene, dichlorobenzene and trichlorobenzene separation is achieved. According to the side stream rectification continuous separation method, the rectification separation method with side stream withdrawing is utilized for one-time separation of chlorobenzene, dichlorobenzene and trichlorobenzene, the content of the obtained chlorobenzene and dichlorobenzene both achieve over 99.5%, three components are creatively separated in a same tower, one tower device is saved, and power consumption is reduced greatly.
Description
Technical field
The invention belongs to field of fine chemical, is to carry out isolating method about a kind of Benzene Chloride, dichlorobenzene continuously through side line rectifying.
Background technology
Adjacent,, three kinds of isomer of santochlor all are the important intermediate in the fine chemistry industry, are widely used in the synthetic of relevant industrial kinds such as medicine, agricultural chemicals, dyestuff, pigment.Orthodichlorobenzene can be used for carbonate synthesis acid anhydride enzyme inhibitor dichlorphenamidum; The control mosquitos and flies; The midbody 3 of the medicament acetofenate of bedbug, nitroquine etc., 4-dichlorobenzaldehyde, the midbody 3 of broad-spectrum de-worming medicine Vermox; 4-two chloro benzophenones, the basic raw material pyrocatechol that the agricultural chemicals furans is red etc.; Santochlor mainly is used as the raw material of thermoplastic engineering plastic polyphenylene sulfide (PPS); As domestic hygiene articles for use (mothproof, mildew-resistant and deodorizer), can also be used to Synthetic 2; 5-dichlorobenzoic acid (midbody of weedicide dinoben); 2,4 dichloro fluorobenzene (starting raw material of quinolone acids antiseptic-germicide), Resorcinol etc.; Meta Dichlorobenzene can be used for synthetic Resorcinol, 3,5-dichlorphenamide bulk powder etc.
The external at present the whole bag of tricks separation dichlorobenzene mixture that proposes, concluding has following separation method:
(1) extractive distillation method (2) molecular sieve adsorption (3) freezing and crystallizing these method ubiquity separation efficiencies of brilliant partition method (4) the chlorination partition method of clinkering together is low; Defectives such as energy consumption height; Particularly general rectifying crystallization processes is usually earlier separated Benzene Chloride, and then is utilized a tower that mixed dichlorobenzene and polystream are separated through a tower and dichlorobenzene and polystream; Whole technology is separated the knockout tower that uses and is reached 5-6; Per minute uses a tower from a component, and the equipment one-time investment is high, and energy consumption is high.
Summary of the invention
The objective of the invention is to propose a kind of Benzene Chloride, dichlorobenzene, polystream and carry out isolating method continuously through the rectifying of single tower side line.
Main technical schemes of the present invention: Benzene Chloride, dichlorobenzene side line rectifying continuous separation method is characterized in that carrying out through the device that under meter, rectifying tower, condensing surface, rectifying still and accessory heating and necessary pipeline by metering turnover tower and tower still constitute; Thick mixed dichlorobenzene is metered in the rectifying still by under meter; Liquid level is at 40-60% in the maintenance rectifying still; Heat temperature raising is treated to begin to begin continuous extraction from overhead, condensing surface and side line pipeline simultaneously after temperature in the tower, the pressure-stabilisation to total reflux, and cat head obtains Benzene Chloride; Side line obtains mixed dichlorobenzene, and polystream is got rid of from the tower still continuously.
Benzene Chloride, dichlorobenzene, polystream side line rectifying continuous separation method; A kind of typical method is: the mixing raw material that will contain Benzene Chloride, santochlor, orthodichlorobenzene and polystream; Deliver to preheater and preheating continuously; Get into the rectifying tower from the rectifying tower middle part that has the side line extraction then, carry out rectifying separation through the reboiler ebuillition of heated at the bottom of the tower, from the continuous extraction content 99.5% (weight percent of cat head; Following per-cent refers to weight percent together) above Benzene Chloride; From the mixed dichlorobenzene of the continuous extraction of rectifying tower side line more than 99.5%, polystream and a spot of is got rid of through the tower still orthodichlorobenzene continuously, reaches the isolating purpose of Benzene Chloride, dichlorobenzene and polystream.
Usually, continuous separation method of the present invention, distillation operation pressure 0.02-0.1Mpa (absolute pressure); The rectifying tower trim the top of column is than being 3-4.
In the said continuous separation method, control preheater preheating temperature is 120 ℃-140 ℃, 122.4～134.9 ℃ of tower top temperatures, 177.6～178.9 ℃ of side stream temperatures, 198.6～201.4 ℃ of tower still temperature.
In the said continuous separation method, the cat head produced quantity is the 15-17% of raw material inlet amount, and the side line produced quantity is the 80-85% of raw material inlet amount.
The present invention adopts disposable Benzene Chloride, dichlorobenzene and the trichlorobenzene isolated of distillation and separation method of band side line extraction; The Benzene Chloride that obtains and the content of dichlorobenzene all reach more than 99.5%; Creatively three components are separated in same tower; Save a tower, reduced energy consumption simultaneously widely.
Description of drawings
Fig. 1 is an embodiment of the invention method flow synoptic diagram.
In the accompanying drawing: 1-under meter, 2-charging, 3-rectifying tower, the extraction of 4-cat head, 5-condensing surface, 6-backflow, the extraction of 7-material, the extraction of 8-side line, the discharging of 9-side line, 10-heating medium advance, 11-rectifying tower still, 12-heating medium go out, the discharging of 13-tower still.
Embodiment
Below in conjunction with embodiment and accompanying drawing the inventive method is described in detail.
This device mainly is made up of under meter 1, rectifying tower 3, condensing surface 5, rectifying still 11 and accessory heating and the necessary pipeline of metering turnover tower and tower still.Thick mixed dichlorobenzene is metered in the rectifying still by under meter 1; Liquid level is at 40-60% in the maintenance rectifying still; Heat temperature raising is treated to begin to begin continuous extraction from overhead 4, condensing surface 5 and side line pipeline 9 simultaneously after temperature in the tower, the pressure-stabilisation to total reflux, and cat head obtains Benzene Chloride; Side line obtains mixed dichlorobenzene, and polystream is got rid of to tower still discharging 13 through pipeline from the tower still continuously
Embodiment 1
The mixed dichlorobenzene raw material that will contain 17.2% Benzene Chloride, 2.54% Meta Dichlorobenzene, 45.79% santochlor, 33.32% orthodichlorobenzene, 0.47% polystream is preheating to 120 ℃ of middle parts from rectifying tower with 1000 kilograms/hour flow through preheater and gets into the tower; 122.4～134.9 ℃ of tower top temperatures of control, 177.6～178.9 ℃ of side stream temperatures, 198.6～201.4 ℃ of tower still temperature; The 15-17% of the about raw material inlet amount of cat head produced quantity; The 80-85% of the about raw material inlet amount of side line produced quantity, the trim the top of column ratio is 3, atmospheric operation; After treating stable operation; Sampling analysis cat head Benzene Chloride content is 99.7%, and side line two cl contenies reach 99.55%, has reached the requirement of three components of disposable separation.
Embodiment 2
Other operational conditions are with embodiment 1, and changing the trim the top of column ratio is 4, treat stable operation after, sampling analysis cat head Benzene Chloride content is 99.9%, side line two cl contenies reach 99.7%.
Embodiment 3
Other operational conditions are with embodiment 1, and changing working pressure (absolute pressure) is 0.02Mpa, treat stable operation after, sampling analysis cat head Benzene Chloride content is 99.65%, side line two cl contenies reach 99.42%.
Claims (6)
1. a Benzene Chloride, dichlorobenzene side line rectifying continuous separation method is characterized in that carrying out through the device that the pipeline by under meter, rectifying tower, condensing surface, rectifying still and accessory heating and necessity of metering turnover tower and tower still constitutes; Thick mixed dichlorobenzene is metered in the rectifying still by under meter; Liquid level is at 40-60% in the maintenance rectifying still; Heat temperature raising is treated to begin to begin continuous extraction from overhead, condensing surface and side line pipeline simultaneously after temperature in the tower, the pressure-stabilisation to total reflux, and cat head obtains Benzene Chloride; Side line obtains mixed dichlorobenzene, and polystream is got rid of from the tower still continuously.
2. the mixing raw material that will contain Benzene Chloride, santochlor, orthodichlorobenzene and polystream according to the described separation method of claim 1; Deliver to preheater and preheating continuously; Get into the rectifying tower from the rectifying tower middle part that has the side line extraction then; Reboiler ebuillition of heated through at the bottom of the tower carries out rectifying separation, from the Benzene Chloride of the continuous extraction mass content of cat head more than 99.5%, from the mixed dichlorobenzene of the continuous extraction mass content of rectifying tower side line more than 99.5%; Polystream and a spot of is got rid of through the tower still orthodichlorobenzene continuously, reaches the isolating purpose of Benzene Chloride, dichlorobenzene and polystream.
3. continuous separation method according to claim 1 is characterized in that distillation operation pressure 0.02-0.1Mpa (absolute pressure).
4. continuous separation method according to claim 1 is characterized in that controlling the preheater preheating temperature and is 120 ℃-140,122.4～134.9 ℃ of tower top temperatures, 177.6～178.9 ℃ of side stream temperatures, 198.6～201.4 ℃ of tower still temperature.
5. continuous separation method according to claim 1 is characterized in that the cat head produced quantity is the 15-17% of raw material inlet amount, and the side line produced quantity is the 80-85% of raw material inlet amount.
6. continuous separation method according to claim 1 is characterized in that the rectifying tower trim the top of column than being 3-4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012101233048A CN102659506A (en) | 2012-04-25 | 2012-04-25 | Side stream rectification continuous separation method of chlorobenzene and dichlorobenzene |
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| CN2012101233048A CN102659506A (en) | 2012-04-25 | 2012-04-25 | Side stream rectification continuous separation method of chlorobenzene and dichlorobenzene |
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Cited By (3)
| 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 |
| CN111116309A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | Industrial method for separating mixed dichlorobenzene |
| CN111978145A (en) * | 2020-08-27 | 2020-11-24 | 上海化工研究院有限公司 | Purification device for low-boiling-point perfluorocarbon and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101270031A (en) * | 2008-04-29 | 2008-09-24 | 南京师范大学 | Method for extracting dichlorobenzene cut fraction in mix chlorobenzene with continuous single-column multi-ply sidetrack discharge fractional distillation |
| CN102188830A (en) * | 2010-03-03 | 2011-09-21 | 中国石油化工股份有限公司 | Reaction distillation method |
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2012
- 2012-04-25 CN CN2012101233048A patent/CN102659506A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101270031A (en) * | 2008-04-29 | 2008-09-24 | 南京师范大学 | Method for extracting dichlorobenzene cut fraction in mix chlorobenzene with continuous single-column multi-ply sidetrack discharge fractional distillation |
| CN102188830A (en) * | 2010-03-03 | 2011-09-21 | 中国石油化工股份有限公司 | Reaction distillation method |
Non-Patent Citations (2)
| Title |
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| CHEN QI ET AL.: "Refining of chlorobenzene from the mixture of chlorobenzene and dichlorobenzene isomer by continuous side-stream distillation", 《COMPUTERS AND APPLIED CHEMISTRY》 * |
| 孙静: "二元混合物连续精馏的研究", 《中国科技信息》 * |
Cited By (4)
| 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 |
| CN111116309A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | Industrial method for separating mixed dichlorobenzene |
| CN111978145A (en) * | 2020-08-27 | 2020-11-24 | 上海化工研究院有限公司 | Purification device for low-boiling-point perfluorocarbon and application thereof |
| CN111978145B (en) * | 2020-08-27 | 2023-03-28 | 上海化工研究院有限公司 | Purification device for low-boiling-point perfluorocarbon and application thereof |
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Application publication date: 20120912 |