CN103130639B - Method for rectification and separation of benzoic acid, benzaldehyde, and toluene by single tower sidestream - Google Patents
Method for rectification and separation of benzoic acid, benzaldehyde, and toluene by single tower sidestream Download PDFInfo
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- CN103130639B CN103130639B CN201110374489.5A CN201110374489A CN103130639B CN 103130639 B CN103130639 B CN 103130639B CN 201110374489 A CN201110374489 A CN 201110374489A CN 103130639 B CN103130639 B CN 103130639B
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Abstract
A method for rectification and separation of benzoic acid, benzaldehyde, and toluene by a single tower sidestream comprises the following steps: firstly adding a toluene liquid phase catalytic oxidation reaction solution into a tower kettle of a sidestream rectifying tower, heating when the liquid level reaches1/3-1/2 of the tower kettle height; when the device reaches total reflux, adjusting the temperature at the sidestream D-1 to 110-112 DEG C, the temperature at the sidestream D-2 to 177-180 DEG C, and the temperature at the sidestream D-3 to 249-255 DEG C from up to down; adding a reaction solution after toluene oxidation into the rectifying tower in a continuous intermediate charging mode, adjusting a reflux ratio to 3-5, wherein the sidestream D-1 distillate is toluene, the sidestream D-2 distillate is benzaldehyde, and the sidestream D-3 distillate is benzoic acid. The tower plate number of the rectifying tower is 96 or more than 96, but less than 110, and the raw material of the toluene oxidation reaction solution is preferably charged at the 25th-30th plate; the sidestream D-1 discharging port is the first tower plate, and the sidestream D-2 discharging port is the 40th-45th tower plate; the sidestream D-3 is the tower bottom.
Description
Technical field
The present invention relates to a kind of separation method of toluene oxidation reaction solution, be specifically related to a kind of toluene, phenyl aldehyde, benzoic method extracted from toluene oxidation reaction solution.
Background technology
In conventional art, for benzoic separating-purifying, be used for preparing hexanolactam, toluene is gained 25% left and right (massfraction after catalyzed oxidation, benzoic acid solution down together), 5% left and right phenyl aldehyde, 65% left and right toluene, 3% left and right phenylcarbinol, 5% left and right water, and a small amount of impurity such as methyl phenyl ketone, biphenyl, methyl diphenyl.Along with the market application of phenyl aldehyde is more and more extensive, the utilization ratio of phenyl aldehyde is more and more higher.Therefore, extract the benzoic phenyl aldehyde that simultaneously extracts 5% left and right, increase business economic profit.Comparatively general method mainly adopts two rectifying tower separate benzoic acid, phenyl aldehyde and toluene at present.The light constituents such as first rectifying tower tower top extraction phenyl aldehyde, toluene, at the bottom of tower, extraction phenylformic acid is refined and is prepared hexanolactam; Second rectifying tower tower top extraction toluene is done oxidizing reaction raw material cycling and reutilization, extracts highly purified phenyl aldehyde finished product at the bottom of tower out.Obviously, traditional technique is for obtaining phenylformic acid, phenyl aldehyde, corresponding 2～3 rectifying tower of toluene needs, and facility investment is large, energy consumption is also large, and yield is low, and production cost is corresponding higher.
Summary of the invention
The present invention seeks to: in order to reduce the separating energy consumption of toluene liquid phase catalytic oxidation reaction solution, and obtain high yield and highly purified phenyl aldehyde, phenyl aldehyde, toluene, the present invention will provide the processing method of a kind of single tower side line rectifying separation phenylformic acid, phenyl aldehyde, toluene.
Technical scheme of the present invention is: the method for single tower side line rectifying separation phenylformic acid, phenyl aldehyde, toluene,
The method of extracting phenylformic acid, phenyl aldehyde, toluene from toluene liquid phase catalytic oxidation reaction solution, comprises the steps:
A, start toluene liquid phase catalytic oxidation reaction solution to add side line tower bottom of rectifying tower, when liquid level reaches tower reactor height 1/3～1/2 place, start heating;
B, when device reaches total reflux, regulating side line D-1 place temperature is from top to bottom 110～112 ℃, side line D-2 place temperature is 177～180 ℃, side line D-3 place temperature is 249～255 ℃;
C, adopt continuous intermediate feed mode, in rectifying tower, add the reaction solution after toluene oxidation, regulating reflux ratio is 3～5, and side line D-1 overhead product is toluene, and side line D-2 overhead product is phenyl aldehyde, and side line D-3 overhead product is phenylformic acid;
Described rectifying tower plates number be 96 and more than, be no more than 110, for save energy is preferably 96; Raw material toluene oxidation reaction solution is at rectifying tower preferably in the charging of 25-30 piece plate, and stage number is counted from the top down, and side line D-1 extraction mouth is the 1st block of column plate, and side line D-2 extraction mouth is 40-45 piece plate;
Side line D-1 overhead product is toluene, and side line D-2 overhead product is phenyl aldehyde, and side line D-3 overhead product is phenylformic acid, at the bottom of side line D-3 refers to tower.The load of above-mentioned side line D-1, side line D-2, side line D-3 is respectively 0.50～0.65,0.03～0.04,0.20～0.35 with the ratio (mass ratio) of toluene oxidation reaction solution inlet amount.
D, side line D-1 overhead product toluene are squeezed into oxidation reactor and are made reaction raw materials recycling, and side line D-2 overhead product enters phenyl aldehyde finished pot, and side line D-3 overhead product makes to prepare hexanolactam raw material.
Above-mentioned side line D-1 overhead product is the toluene of mass content 95～98%, and yield is more than 92%.
Above-mentioned side line D-2 overhead product is the phenyl aldehyde of mass content 98～99%, and yield is more than 90%.
Above-mentioned side line D-3 (at the bottom of tower) overhead product is more than 99% phenylformic acid of mass content, and yield is more than 95%.
Above-mentioned rectifying tower plates number is more than 96, for save energy is preferably 96.When stage number is 96, raw material toluene oxidation reaction solution is at rectifying tower preferably the 30th plate charging, and side line D-2 extraction mouth is preferably the 45th block of plate.In the present invention, stage number is counted from the top down.Rectifying tower plates number is 96, and toluene reaction solution is in the 30th plate charging of rectifying tower, and side line D-1 extraction mouth is the 1st block of column plate, and side line D-2 extraction mouth is the 45th block of plate.
More than 99% phenylformic acid of the mass content that aforesaid method obtains, yield is more than 95%.
Beneficial effect of the present invention: the inventive method, by a tower, not only obtains the components such as phenylformic acid, phenyl aldehyde, toluene, and the benzoic mass content of gained is more than 99%, and yield is more than 95%; The mass content 98～99% of phenyl aldehyde, yield is more than 90%; The mass content 95～98% of toluene, yield is more than 92%.Reaction time of the present invention is short, simple to operate, energy consumption is low, yield is high and gained phenylformic acid purity is high, can realize the industrialization of extracting phenylformic acid, phenyl aldehyde, toluene from toluene reaction solution.
Accompanying drawing explanation
Fig. 1 is single tower side line distillation process figure.
Embodiment
Embodiment 1
This experiment toluene oxidation reaction solution is from Sinopec Shijiazhuang refinery branch office, and reaction solution feeding temperature is 25 ℃.Rectifying tower plates number is 96, and toluene reaction solution is in the 25th plate charging of rectifying tower, and side line D-1 extraction mouth is the 1st block of column plate, and side line D-2 extraction mouth is the 40th block of plate.The reaction solution that toluene oxidation is complete adds rectifying tower, when liquid level reaches tower reactor 1/3 place, starts heating; When device reaches total reflux, regulating side line D-1 temperature is from top to bottom 109～111 ℃, and side line D-2 place temperature is 175～178 ℃, and side line D-3 place temperature is 240～245 ℃; Adopt continuous intermediate feed mode, in rectifying tower, add continuously toluene reaction solution, regulating side line D-1 place reflux ratio is 5, side line D-2 place reflux ratio is 2～4, side line D-3 place reflux ratio is 1～3, side line D-1 overhead product is that mass content is 90% toluene, and side line D-2 overhead product is that mass content is 89.7% phenyl aldehyde, and side line D-3 overhead product is that mass content is 95.7% phenylformic acid.
Embodiment 2
This experiment toluene oxidation reaction solution is from Sinopec Shijiazhuang refinery branch office, and reaction solution feeding temperature is 25 ℃.Rectifying tower plates number is 96, and toluene reaction solution is in the 30th plate charging of rectifying tower, and side line D-1 extraction mouth is the 1st block of column plate, and side line D-2 extraction mouth is the 45th block of plate.The reaction solution that toluene oxidation is complete adds rectifying tower, when liquid level reaches tower reactor 1/3 place, starts heating; When device reaches total reflux, regulating side line D-1 temperature is from top to bottom 110～112 ℃, and side line D-2 place temperature is 177～180 ℃, and side line D-3 place temperature is 249～255 ℃; Adopt continuous intermediate feed mode, in rectifying tower, add continuously toluene reaction solution, regulating side line D-1 place reflux ratio is 5, side line D-2 place reflux ratio is 2～4, side line D-3 place reflux ratio is 1～3, side line D-1 overhead product is that mass content is 96% toluene, and side line D-2 overhead product is that mass content is 98.6% phenyl aldehyde, and side line D-3 overhead product is that mass content is 99.5% phenylformic acid; Together with after side line D-1 production toluene fraction mixes with raw material toluene, squeeze into oxidation reaction apparatus and continue reaction, side line D-3 production phenylformic acid is made hexanolactam reaction raw materials.
As shown in Figure 1, single tower side line rectifier unit comprises raw material storage tank 1, single tower side line rectifying tower 2, side line D-1 extraction mouth 3, side line D-2 extraction mouth 4, side line D-3 extraction mouth 5, the first pump 6 and the second pump 7, condenser system 8.Side line rectifying tower be linked in sequence from top to bottom stripping section, the second rectifying section, the first rectifying section, tower top end socket and condenser.Raw material is squeezed into tower reactor from raw material storage tank 1 by the first pump 6, controls the flow of each opening for feed and extraction mouth with spinner-type flowmeter.
Claims (1)
1. from toluene liquid phase catalytic oxidation reaction solution, extract a method for phenylformic acid, phenyl aldehyde, toluene, it is characterized in that comprising the steps:
When a, beginning, toluene liquid phase catalytic oxidation reaction solution is added to side line tower bottom of rectifying tower, when liquid level reaches tower reactor height 1/3 ~ 1/2 place, start heating;
B, when device reaches total reflux, regulating side line D-1 place temperature is from top to bottom 110 ~ 112 ℃, side line D-2 place temperature is 177 ~ 180 ℃, side line D-3 place temperature is 249 ~ 255 ℃;
C, adopt continuous intermediate feed mode, in rectifying tower, add the reaction solution after toluene oxidation, regulating reflux ratio is 3 ~ 5, and side line D-1 overhead product is toluene, and side line D-2 overhead product is phenyl aldehyde, and side line D-3 overhead product is phenylformic acid;
Described rectifying tower plates number is 96 to 110, and raw material toluene oxidation reaction solution is at rectifying tower in the charging of 25-30 piece column plate, and stage number is counted from the top down; Side line D-1 extraction mouth is the 1st block of column plate, and side line D-2 extraction mouth is 40-45 piece column plate; At the bottom of side line D-3 refers to tower;
The load of above-mentioned side line D-1, side line D-2, side line D-3 is that mass ratio is respectively 0.50 ~ 0.65,0.03 ~ 0.04,0.20 ~ 0.35 with the ratio of toluene oxidation reaction solution inlet amount.
2, toluene, phenyl aldehyde, the benzoic method extracted from toluene oxidation reaction solution as claimed in claim 1, is characterized in that side line D-1 overhead product is the toluene of mass content 95 ~ 98%, and yield is more than 92%.
3, toluene, phenyl aldehyde, the benzoic method extracted from toluene oxidation reaction solution as claimed in claim 1, is characterized in that side line D-2 overhead product is the phenyl aldehyde of mass content 98 ~ 99%, and yield is more than 90%.
4, toluene, phenyl aldehyde, the benzoic method extracted from toluene oxidation reaction solution as claimed in claim 1, is characterized in that side line D-3 overhead product is more than 99% phenylformic acid of mass content, and yield is more than 95%.
5, toluene, phenyl aldehyde, the benzoic method extracted from toluene oxidation reaction solution as claimed in claim 1, it is characterized in that side line D-1 overhead product toluene squeezes into oxidation reactor and make reaction raw materials recycling, side line D-2 overhead product enters phenyl aldehyde finished pot, and side line D-3 overhead product makes to prepare hexanolactam raw material.
6, as described in one of claim 1 to 5, from toluene oxidation reaction solution, extract toluene, phenyl aldehyde, benzoic method, it is characterized in that described rectifying tower plates number is 96.
7, a kind of toluene, phenyl aldehyde, benzoic method extracted from toluene oxidation reaction solution as claimed in claim 6, is characterized in that toluene oxidation reaction solution is in the 30th column plate charging of rectifying tower.
8, a kind of toluene, phenyl aldehyde, benzoic method extracted from toluene oxidation reaction solution as claimed in claim 6, is characterized in that side line D-2 extraction mouth is at the 45th block of column plate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110374489.5A CN103130639B (en) | 2011-11-23 | 2011-11-23 | Method for rectification and separation of benzoic acid, benzaldehyde, and toluene by single tower sidestream |
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| CN201110374489.5A CN103130639B (en) | 2011-11-23 | 2011-11-23 | Method for rectification and separation of benzoic acid, benzaldehyde, and toluene by single tower sidestream |
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| CN103130639B true CN103130639B (en) | 2014-12-10 |
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| CN104974034A (en) * | 2014-04-10 | 2015-10-14 | 中国石化扬子石油化工有限公司 | Method of two-column separation of benzoic acid, benzaldehyde and methylbenzene |
| CN105503567B (en) * | 2016-01-15 | 2017-12-29 | 湖南弘润化工科技有限公司 | The device and method of continuous production benzoic acid, by-product benzaldehyde |
| CN110015954A (en) * | 2019-01-31 | 2019-07-16 | 武汉有机实业有限公司 | The production method of food additives sodium benzoate |
| CN111689537B (en) * | 2020-05-18 | 2022-07-29 | 南京工业大学 | Method for treating sodium benzoate or halogenated sodium benzoate wastewater |
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| CN101607867B (en) * | 2009-08-03 | 2012-05-30 | 湖南大学 | Technique for using methylbenzene to prepare benzaldehyde and benzene methanol by multistage oxidation and equipment |
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