CN105218298A - Continuous rectification is separated parachlorotoluene chlorated liquid and purifies to chlorine one benzyl chloride with to chlorine benzyl dichloride method and device - Google Patents
Continuous rectification is separated parachlorotoluene chlorated liquid and purifies to chlorine one benzyl chloride with to chlorine benzyl dichloride method and device Download PDFInfo
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- CN105218298A CN105218298A CN201510664262.2A CN201510664262A CN105218298A CN 105218298 A CN105218298 A CN 105218298A CN 201510664262 A CN201510664262 A CN 201510664262A CN 105218298 A CN105218298 A CN 105218298A
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- Y—GENERAL 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
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Abstract
The invention discloses continuous rectification and be separated the purification of parachlorotoluene chlorated liquid to chlorine one benzyl chloride with to chlorine benzyl dichloride method and device, present method is: (a) parachlorotoluene chlorated liquid enters in tower from de-to the middle part opening for feed of chlorine one benzyl chloride tower continuously after being preheating to, from the de-outlet of the overhead vapor to chlorine one benzyl chloride tower discharge, the first condenser is entered to chlorine one benzyl chloride, condensation to the extraction of chlorine one benzyl chloride part, taking off, a still liquid part of discharging at the bottom of to chlorine one benzyl chloride tower tower is heat vaporized to be returned in tower, and another part extraction is as the raw material of purifying to chlorine benzyl dichloride tower; B () enters tower in from purification to the middle part opening for feed of chlorine benzyl dichloride tower from the de-still liquid to extraction at the bottom of chlorine one benzyl chloride tower tower, from the overhead vapor mouth discharge of purifying to chlorine benzyl dichloride tower, the second condenser is entered to chlorine benzyl dichloride, condensed to the extraction of a chlorine benzyl dichloride part, purifying, a still liquid part of discharging at the bottom of to chlorine benzyl dichloride tower tower returns in tower through heat vaporized, another part extraction.Present method improves separation efficiency.
Description
Technical field
The present invention relates to the purification of a kind of continuous rectification separation parachlorotoluene chlorated liquid and the purification of parachlorotoluene chlorated liquid is separated to chlorine one benzyl chloride with to chlorine benzyl dichloride production equipment with to chlorine benzyl dichloride production method and continuous rectification to chlorine one benzyl chloride.
Background technology
To chlorine benzyl dichloride as a kind of very important industrial chemicals, be widely used in the fields such as agricultural chemicals, medicine, dyestuff and white dyes.Such as, 4-chloro-benzaldehyde can be obtained by hydrolysis by chlorine benzyl dichloride, and the purposes of 4-chloro-benzaldehyde is also very extensive, can be used for synthesis tranquilizer chlomezanone, microbiotic cloxacillin sodium and dibenzylidene sorbitol (DBS) series derivates etc.At present, separating-purifying is to the method for chlorine benzyl dichloride mainly batch fractionating method.Be separated and Fig. 1 is shown in the traditional technology of chlorine benzyl dichloride.4-chlorobenzyl chloride interval flow process: parachlorotoluene chlorated liquid carries out batch distillation in intermittent column, tower reactor heat-conducting oil heating still liquid also makes still liquid vaporize, when the content of tower reactor to chlorine benzyl dichloride acquires a certain degree a still liquid extraction, ensure in still liquid to chlorine benzyl dichloride more than 92%.From above-mentioned flow process, batch fractionating yield is lower, and energy consumption is high, easy green coke, unstable product quality, and is not very high to chlorine benzyl dichloride content in still liquid, and other contained impurity are more, and the yield of next step hydrolysis reaction is restricted.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art, provide a kind of high-recovery, less energy-consumption and the continuous rectification of high purity product are separated parachlorotoluene chlorated liquid and purify to chlorine one benzyl chloride with to chlorine benzyl dichloride method.
It is high that another object of the present invention is to provide a kind of level of automation, and the stable and continuous rectification of safety is separated parachlorotoluene chlorated liquid and purifies to chlorine one benzyl chloride with to chlorine benzyl dichloride production equipment.
In order to achieve the above object, the technical solution used in the present invention is:
Continuous rectification of the present invention is separated parachlorotoluene chlorated liquid and purifies to chlorine one benzyl chloride with to chlorine benzyl dichloride production method, and it comprises the following steps:
A () parachlorotoluene chlorated liquid enters in tower from de-to the middle part opening for feed of chlorine one benzyl chloride tower through being preheating to after 220 ~ 225 DEG C continuously, from the de-outlet of the overhead vapor to chlorine one benzyl chloride tower discharge, the first condenser is entered to chlorine one benzyl chloride, condensation a chlorine one benzyl chloride part is refluxed, part extraction, take off in chlorine one benzyl chloride tower through heat vaporized the returning of the first reboiler in the described still liquid part of discharging at the bottom of to chlorine one benzyl chloride tower tower that takes off, another part extraction is as the raw material of purifying to chlorine benzyl dichloride tower, described de-be 2 ~ 4kPa to the working pressure of chlorine one benzyl chloride tower, tower top and the pressure reduction at the bottom of tower are 2 ~ 4kPa,
B () enters tower in from purification to the middle part opening for feed of chlorine benzyl dichloride tower from the de-still liquid to extraction at the bottom of chlorine one benzyl chloride tower tower, from the overhead vapor mouth discharge of purifying to chlorine benzyl dichloride tower, the second condenser is entered to chlorine benzyl dichloride, condensed to the backflow of a chlorine benzyl dichloride part, part extraction, a still liquid part of discharging at the bottom of described purification is to chlorine benzyl dichloride tower tower is purified in chlorine benzyl dichloride tower through heat vaporized the returning of the second reboiler, another part extraction, the working pressure of described purification to chlorine benzyl dichloride tower is 1 ~ 3kPa, tower top and the pressure reduction at the bottom of tower are 2 ~ 4kPa.
Continuous rectification of the present invention is separated parachlorotoluene chlorated liquid and purifies to chlorine one benzyl chloride with to chlorine benzyl dichloride production equipment, it comprises de-to chlorine one benzyl chloride tower with purify to chlorine benzyl dichloride tower, de-to chlorine one benzyl chloride tower with purify to connect the tower top of chlorine benzyl dichloride tower and be connected with condenser and reflux respectively and described de-to chlorine one benzyl chloride tower with purify and be connected to reboiler to the tower bottom of chlorine benzyl dichloride tower, de-, to the middle part of chlorine benzyl dichloride tower, opening for feed is had to chlorine one benzyl chloride tower and purification, take off and discharge port at the bottom of chlorine one benzyl chloride tower tower is connected chlorine benzyl dichloride tower opening for feed with purification by pipeline.
Compared with prior art, the present invention has following beneficial effect:
Be improved to double tower continuous distillation method of the present invention by traditional batch fractionating separating technology, improve separation efficiency, for follow-up hydrolysis reaction provides highly purified to chlorine benzyl dichloride, reduce the impact of other impurity on hydrolysis reaction.
Accompanying drawing explanation
Fig. 1 is existing 4-chlorobenzyl chloride batch distillation process schema;
Fig. 2 is that continuous rectification of the present invention is separated the purification of parachlorotoluene chlorated liquid to chlorine one benzyl chloride and the schema to chlorine benzyl dichloride production method.
Embodiment
Describe the present invention below in conjunction with specific embodiment.
Continuous rectification of the present invention is separated the purification of parachlorotoluene chlorated liquid and comprises the following steps to chlorine one benzyl chloride with to chlorine benzyl dichloride production method:
A () parachlorotoluene chlorated liquid enters in tower from de-to the middle part opening for feed of chlorine one benzyl chloride tower 1 through being preheating to after 220 ~ 225 DEG C continuously, from the de-outlet of the overhead vapor to chlorine one benzyl chloride tower discharge, the first condenser 2 is entered to chlorine one benzyl chloride, condensation a chlorine one benzyl chloride part is refluxed, part extraction, take off in chlorine one benzyl chloride tower through heat vaporized the returning of the first reboiler 3 in the described still liquid part of discharging at the bottom of to chlorine one benzyl chloride tower tower that takes off, another part extraction is as the raw material of purifying to chlorine benzyl dichloride tower, described de-be 2 ~ 4kPa to the working pressure of chlorine one benzyl chloride tower, tower top and the pressure reduction at the bottom of tower are 2 ~ 4kPa.
B () enters tower in from purification to the middle part opening for feed of chlorine benzyl dichloride tower 4 from the de-still liquid to extraction at the bottom of chlorine one benzyl chloride tower tower, from the overhead vapor mouth discharge of purifying to chlorine benzyl dichloride tower, the second condenser 5 is entered to chlorine benzyl dichloride, condensed to the backflow of a chlorine benzyl dichloride part, part extraction, a still liquid part of discharging at the bottom of described purification is to chlorine benzyl dichloride tower tower is purified in chlorine benzyl dichloride tower through heat vaporized the returning of the second reboiler 6, another part extraction, the working pressure of described purification to chlorine benzyl dichloride tower is 1 ~ 3kPa, tower top and the pressure reduction at the bottom of tower are 2 ~ 4kPa.
Parachlorotoluene chlorated liquid is the chlorated liquid after removing part parachlorotoluene, and its quality composition with percentages is: 1.0 ~ 1.5% parachlorotoluenes, 0.5 ~ 1.0% parachlorobenzoyl chloride, 0.5 ~ 1.0% 4-chloro-benzaldehyde, 50.0 ~ 55.0% pairs of chlorine one benzyl chlorides, 40.0 ~ 44.0% pairs of chlorine benzyl dichlorides and 2.0 ~ 3.5% pairs of chlorine three benzyl chlorides.
Continuous rectification of the present invention is separated parachlorotoluene chlorated liquid and purifies to chlorine one benzyl chloride with to chlorine benzyl dichloride production equipment, it comprises de-to chlorine one benzyl chloride tower 1 with purify to chlorine benzyl dichloride tower 4, de-to chlorine one benzyl chloride tower with purify to connect the tower top of chlorine benzyl dichloride tower and be connected with condenser 2 respectively, 5 and reflux and described de-to chlorine one benzyl chloride tower with purify and be connected to reboiler 3 to the tower bottom of chlorine benzyl dichloride tower, 6, de-, to the middle part of chlorine benzyl dichloride tower, opening for feed is had to chlorine one benzyl chloride tower and purification, take off and discharge port at the bottom of chlorine one benzyl chloride tower tower is connected chlorine benzyl dichloride tower opening for feed with purification by pipeline.
Described de-to chlorine one benzyl chloride tower with to purify to the reflux of chlorine benzyl dichloride tower be external reflux device.
Described taking off is made up of structured packing and liquid distributor the column internals of chlorine benzyl dichloride tower chlorine one benzyl chloride tower and purification, described structured packing can be the one in Mellapak packing, screen waviness packings or ceramic corrugated filler, certainly the random packing of various types is also comprised, or the tower tray being comprised the patterns such as valve tray column, sieve-tray tower, vertical sieve tray by tray column is formed, wherein Mellapak packing is preferred filler.
Embodiment 1
Being passed into 2000kg/h flow by the stock liquid being preheating to 220 DEG C de-ly enters in tower to the middle part opening for feed of chlorine one benzyl chloride tower, described stock liquid consist of 1.5% parachlorotoluene, 0.5% parachlorobenzoyl chloride, 1.0% 4-chloro-benzaldehyde, 55.0% pair of chlorine one benzyl chloride, 40.0% pair of chlorine benzyl dichloride and 2.0% pair of chlorine three benzyl chloride, from the de-outlet of the overhead vapor to chlorine one benzyl chloride tower discharge, the first condenser is entered to chlorine one benzyl chloride, condensation a chlorine one benzyl chloride part is refluxed, part extraction, take off in chlorine one benzyl chloride tower through heat vaporized the returning of the first reboiler in the described still liquid part of discharging at the bottom of to chlorine one benzyl chloride tower tower that takes off, another part extraction is as the raw material of purifying to chlorine benzyl dichloride tower, described de-be 2 ~ 3kPa to the working pressure of chlorine one benzyl chloride tower, tower top and the pressure reduction at the bottom of tower are 2 ~ 3kPa, in tower, temperature is at 92 ~ 124 DEG C.Enter tower in from purification to the middle part opening for feed of chlorine benzyl dichloride tower with 884kg/h flow from the de-still liquid to extraction at the bottom of chlorine one benzyl chloride tower tower, from the overhead vapor mouth discharge of purifying to chlorine benzyl dichloride tower, the second condenser is entered to chlorine benzyl dichloride, condensed to the backflow of a chlorine benzyl dichloride part, part extraction, a still liquid part of discharging at the bottom of described purification is to chlorine benzyl dichloride tower tower is purified in chlorine benzyl dichloride tower through heat vaporized the returning of the second reboiler, another part extraction, the working pressure of described purification to chlorine benzyl dichloride tower is 1 ~ 2kPa, tower top and the pressure reduction at the bottom of tower are 2 ~ 3kPa, in tower, temperature is at 89 ~ 120 DEG C.
After separating-purifying to chlorine one benzyl chloride with to the massfraction of chlorine benzyl dichloride respectively >=95.0% and >=99.0%.
Embodiment 2
Being passed into 2500kg/h flow by the stock liquid being preheating to 221 DEG C de-ly enters in tower to the middle part opening for feed of chlorine one benzyl chloride tower, described stock liquid consist of 1.0% parachlorotoluene, 1.0% parachlorobenzoyl chloride, 0.5% 4-chloro-benzaldehyde, 50.0% pair of chlorine one benzyl chloride, 44.0% pair of chlorine benzyl dichloride and 3.5% pair of chlorine three benzyl chloride, from the de-outlet of the overhead vapor to chlorine one benzyl chloride tower discharge, the first condenser is entered to chlorine one benzyl chloride, condensation a chlorine one benzyl chloride part is refluxed, part extraction, take off in chlorine one benzyl chloride tower through heat vaporized the returning of the first reboiler in the described still liquid part of discharging at the bottom of to chlorine one benzyl chloride tower tower that takes off, another part extraction is as the raw material of purifying to chlorine benzyl dichloride tower, described de-be 3 ~ 4kPa to the working pressure of chlorine one benzyl chloride tower, tower top and the pressure reduction at the bottom of tower are 3 ~ 4kPa, in tower, temperature is at 92 ~ 123 DEG C.Enter tower in from purification to the middle part opening for feed of chlorine benzyl dichloride tower with 1056kg/h flow from the de-still liquid to extraction at the bottom of chlorine one benzyl chloride tower tower, from the overhead vapor mouth discharge of purifying to chlorine benzyl dichloride tower, the second condenser is entered to chlorine benzyl dichloride, condensed to the backflow of a chlorine benzyl dichloride part, part extraction, a still liquid part of discharging at the bottom of described purification is to chlorine benzyl dichloride tower tower is purified in chlorine benzyl dichloride tower through heat vaporized the returning of the second reboiler, another part extraction, the working pressure of described purification to chlorine benzyl dichloride tower is 2 ~ 3kPa, tower top and the pressure reduction at the bottom of tower are 3 ~ 4kPa, in tower, temperature is at 89 ~ 122 DEG C.
After separating-purifying to chlorine one benzyl chloride with to the massfraction of chlorine benzyl dichloride respectively >=95.0% and >=99.0%.
Embodiment 3
Being passed into 2800kg/h flow by the stock liquid being preheating to 225 DEG C de-ly enters in tower to the middle part opening for feed of chlorine one benzyl chloride tower, described stock liquid consist of 1.2% parachlorotoluene, 0.8% parachlorobenzoyl chloride, 0.6% 4-chloro-benzaldehyde, 52.6% pair of chlorine one benzyl chloride, 41.8% pair of chlorine benzyl dichloride and 3.0% pair of chlorine three benzyl chloride, from the de-outlet of the overhead vapor to chlorine one benzyl chloride tower discharge, the first condenser is entered to chlorine one benzyl chloride, condensation a chlorine one benzyl chloride part is refluxed, part extraction, take off in chlorine one benzyl chloride tower through heat vaporized the returning of the first reboiler in the described still liquid part of discharging at the bottom of to chlorine one benzyl chloride tower tower that takes off, another part extraction is as the raw material of purifying to chlorine benzyl dichloride tower, described de-be 2.5 ~ 3.5kPa to the working pressure of chlorine one benzyl chloride tower, tower top and the pressure reduction at the bottom of tower are 2.5 ~ 3.5kPa, in tower, temperature is at 93 ~ 124 DEG C.Enter tower in from purification to the middle part opening for feed of chlorine benzyl dichloride tower with 1223kg/h flow from the de-still liquid to extraction at the bottom of chlorine one benzyl chloride tower tower, from the overhead vapor mouth discharge of purifying to chlorine benzyl dichloride tower, the second condenser is entered to chlorine benzyl dichloride, condensed to the backflow of a chlorine benzyl dichloride part, part extraction, a still liquid part of discharging at the bottom of described purification is to chlorine benzyl dichloride tower tower is purified in chlorine benzyl dichloride tower through heat vaporized the returning of the second reboiler, another part extraction, the working pressure of described purification to chlorine benzyl dichloride tower is 1.5 ~ 2.5kPa, tower top and the pressure reduction at the bottom of tower are 2.5 ~ 3.5kPa, in tower, temperature is at 89 ~ 121 DEG C.
After separating-purifying to chlorine one benzyl chloride with to the massfraction of chlorine benzyl dichloride respectively >=95.0% and >=99.0%.
Claims (6)
1. continuous rectification is separated the purification of parachlorotoluene chlorated liquid to chlorine one benzyl chloride with to chlorine benzyl dichloride production method, and it is characterized in that, it comprises the following steps:
A () parachlorotoluene chlorated liquid enters in tower from de-to the middle part opening for feed of chlorine one benzyl chloride tower through being preheating to after 220 ~ 225 DEG C continuously, from the de-outlet of the overhead vapor to chlorine one benzyl chloride tower discharge, the first condenser is entered to chlorine one benzyl chloride, condensation a chlorine one benzyl chloride part is refluxed, part extraction, take off in chlorine one benzyl chloride tower through heat vaporized the returning of the first reboiler in the described still liquid part of discharging at the bottom of to chlorine one benzyl chloride tower tower that takes off, another part extraction is as the raw material of purifying to chlorine benzyl dichloride tower, described de-be 2 ~ 4kPa to the working pressure of chlorine one benzyl chloride tower, tower top and the pressure reduction at the bottom of tower are 2 ~ 4kPa,
B () enters tower in from purification to the middle part opening for feed of chlorine benzyl dichloride tower from the de-still liquid to extraction at the bottom of chlorine one benzyl chloride tower tower, from the overhead vapor mouth discharge of purifying to chlorine benzyl dichloride tower, the second condenser is entered to chlorine benzyl dichloride, condensed to the backflow of a chlorine benzyl dichloride part, part extraction, a still liquid part of discharging at the bottom of described purification is to chlorine benzyl dichloride tower tower is purified in chlorine benzyl dichloride tower through heat vaporized the returning of the second reboiler, another part extraction, the working pressure of described purification to chlorine benzyl dichloride tower is 1 ~ 3kPa, tower top and the pressure reduction at the bottom of tower are 2 ~ 4kPa.
2. continuous rectification according to claim 1 is separated the purification of parachlorotoluene chlorated liquid to chlorine one benzyl chloride with to chlorine benzyl dichloride production method, it is characterized in that: described parachlorotoluene chlorated liquid is the chlorated liquid after removing part parachlorotoluene, its quality composition with percentages is: 1.0 ~ 1.5% parachlorotoluenes, 0.5 ~ 1.0% parachlorobenzoyl chloride, 0.5 ~ 1.0% 4-chloro-benzaldehyde, 50.0 ~ 55.0% pairs of chlorine one benzyl chlorides, 40.0 ~ 44.0% pairs of chlorine benzyl dichlorides and 2.0 ~ 3.5% pairs of chlorine three benzyl chlorides.
3. one kind realize claim 1 be separated with the continuous rectification of the present invention of 2 methods parachlorotoluene chlorated liquid purify to chlorine one benzyl chloride with to chlorine benzyl dichloride production equipment, it is characterized in that: it comprises de-to chlorine one benzyl chloride tower with purify to chlorine benzyl dichloride tower, de-to chlorine one benzyl chloride tower with purify to connect the tower top of chlorine benzyl dichloride tower and be connected with condenser and reflux respectively and described de-to chlorine one benzyl chloride tower with purify and be connected to reboiler to the tower bottom of chlorine benzyl dichloride tower, de-, to the middle part of chlorine benzyl dichloride tower, opening for feed is had to chlorine one benzyl chloride tower and purification, take off and discharge port at the bottom of chlorine one benzyl chloride tower tower is connected chlorine benzyl dichloride tower opening for feed with purification by pipeline.
4. continuous rectification according to claim 3 is separated parachlorotoluene chlorated liquid and purifies to chlorine one benzyl chloride with to chlorine benzyl dichloride production equipment, it is characterized in that: described de-to chlorine one benzyl chloride tower with to purify to the reflux of chlorine benzyl dichloride tower be external reflux device.
5. continuous rectification according to claim 4 is separated the purification of parachlorotoluene chlorated liquid to chlorine one benzyl chloride with to chlorine benzyl dichloride production equipment, it is characterized in that: described taking off is made up of structured packing and liquid distributor the column internals of chlorine benzyl dichloride tower chlorine one benzyl chloride tower and purification.
6. continuous rectification according to claim 5 is separated the purification of parachlorotoluene chlorated liquid to chlorine one benzyl chloride with to chlorine benzyl dichloride production equipment, it is characterized in that: described structured packing is Mellapak packing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510664262.2A CN105218298A (en) | 2015-10-14 | 2015-10-14 | Continuous rectification is separated parachlorotoluene chlorated liquid and purifies to chlorine one benzyl chloride with to chlorine benzyl dichloride method and device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510664262.2A CN105218298A (en) | 2015-10-14 | 2015-10-14 | Continuous rectification is separated parachlorotoluene chlorated liquid and purifies to chlorine one benzyl chloride with to chlorine benzyl dichloride method and device |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101497552A (en) * | 2009-03-19 | 2009-08-05 | 江苏钟腾化工有限公司 | Method for preparing p-chlorotoluene and o-chlorotoluene by chlorination toluene |
| CN101941885A (en) * | 2009-07-08 | 2011-01-12 | 冯振灿 | Preparation method of o-chlorobenzyl chloride |
| CN103172490A (en) * | 2012-12-20 | 2013-06-26 | 江苏长三角精细化工有限公司 | Method and device for producing chlorobenzyl chloride through continuous rectification |
| CN104211564A (en) * | 2014-09-16 | 2014-12-17 | 天津大学 | Industrial device and continuous rectification method for extracting 1,2-propylene dichloride from chlorohydrin process epoxypropane waste liquid |
-
2015
- 2015-10-14 CN CN201510664262.2A patent/CN105218298A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497552A (en) * | 2009-03-19 | 2009-08-05 | 江苏钟腾化工有限公司 | Method for preparing p-chlorotoluene and o-chlorotoluene by chlorination toluene |
| CN101941885A (en) * | 2009-07-08 | 2011-01-12 | 冯振灿 | Preparation method of o-chlorobenzyl chloride |
| CN103172490A (en) * | 2012-12-20 | 2013-06-26 | 江苏长三角精细化工有限公司 | Method and device for producing chlorobenzyl chloride through continuous rectification |
| CN104211564A (en) * | 2014-09-16 | 2014-12-17 | 天津大学 | Industrial device and continuous rectification method for extracting 1,2-propylene dichloride from chlorohydrin process epoxypropane waste liquid |
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Application publication date: 20160106 |