CN104844416B - Multitple extraction absorbs dichloromethane and the method for monochloroacetone in MCPA,MCP,methoxone synthesis tail gas - Google Patents
Multitple extraction absorbs dichloromethane and the method for monochloroacetone in MCPA,MCP,methoxone synthesis tail gas Download PDFInfo
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- CN104844416B CN104844416B CN201510137936.3A CN201510137936A CN104844416B CN 104844416 B CN104844416 B CN 104844416B CN 201510137936 A CN201510137936 A CN 201510137936A CN 104844416 B CN104844416 B CN 104844416B
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Abstract
A kind of multitple extraction is used to absorb dichloromethane and the method for monochloroacetone in MCPA,MCP,methoxone synthesis tail gas, with DOP and water for extraction absorbent, tail gas is 1: 0.1～0.15 with the volume ratio of extraction absorbent, the volume of DOP and water is 1: 1.5～2.0, in multitple extraction absorption tower is to tail gas, dichloromethane and monochloroacetone carry out multitple extraction absorption, after extraction absorbs, in the tail gas of extraction top, absorption tower, content of organics is less than 0.0021Kg/m3, extraction absorption tower bottom liquid phases is through Liquid liquid Separation, and lower floor's aqueous phase is containing COD less than 500PPM, and upper organic layer is delivered to side line rectifying column and processed；Side line rectifying tower top extraction >=98.5% dichloromethane, side line rectifying column side take-off >=97.3% monochloroacetone, after side line rectifier bottoms extraction >=99.9%DOP, DOP and Liquid liquid Separation, lower floor's aqueous phase is mixed in proportion Posterior circle and uses as extraction absorbent to extraction absorption tower.
Description
Technical field
The technique that the present invention relates to a kind of pesticide intermediate production process vent gas treatment, particularly relates to a kind of multitple extraction
Absorb organic method in MCPA,MCP,methoxone synthesis tail gas.
Background technology
MCPA,MCP,methoxone, chemical name 2-methyl-4-chlorophenoxyacetic acid, be China produce the most in a large number and use a kind of high
Effect, low toxicity, high selective insecticide and herbicide.In MCPA,MCP,methoxone building-up process, employing monochloroacetone is synthetic,
Cause its synthesis produces containing a certain amount of dichloromethane, monochloroacetone and the tail gas of water.During MCPA,MCP,methoxone is produced
Tail gas, uses pond to absorb in current commercial production, then carry out biochemical treatment, in the tail gas after the absorption of pond containing Organic substance still
The highest, it is easily caused environmental pollution, the water after tail gas absorption carries out biochemical treatment, and processing cost is high, causes tail gas treatment device to throw
Money is high, cost is big.
The present invention proposes a kind of multitple extraction absorption process and processes containing dichloromethane and the tail gas of monochloroacetone, not only makes tail gas
Middle dichloromethane and monochloroacetone remove more thoroughly, and after absorbing, the COD of water is less than 500PPM simultaneously, extraction used in processing procedure
Absorbent and dichloromethane and monochloroacetone can be recycled.
Summary of the invention
It is an object of the invention to provide a kind of multitple extraction and absorb dichloromethane and a chlorine in MCPA,MCP,methoxone synthesis tail gas
The method of acetone, it is possible to effectively dichloromethane and monochloroacetone in removing tail gas, realizes dichloromethane and monochloroacetone simultaneously
Reclaim or recycle, and after absorption, in water, COD is less than 500PPM.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of multitple extraction is used to absorb dichloromethane and the method for monochloroacetone in MCPA,MCP,methoxone synthesis tail gas, its feature
It is, MCPA,MCP,methoxone synthesis tail gas is delivered to the bottom on multitple extraction absorption tower, mix with dioctyl phthalate (DOP) and water
Closing liquid is extraction absorbent, is added from the top on extraction absorption tower by extraction absorbent, tail gas and the volume ratio of extraction absorbent
It is 1: 0.1～0.15, dichloromethane in tail gas and monochloroacetone are carried out multitple extraction absorption；After extraction absorbs, extraction absorbs
In top of tower tail gas, content of organics is less than 0.0021Kg/m3；Extraction absorption tower bottom liquid phases contains through Liquid liquid Separation, lower floor's aqueous phase
COD is less than 500PPM, and upper organic layer is delivered to side line rectifying column and processed；Described organic layer separates through rectification, side line rectifying tower top
Discharging is dichloromethane, recycles as solvent, and side line rectifying column lateral line discharging is monochloroacetone, and side line rectifier bottoms goes out
Material is DOP；Lower floor's aqueous phase after DOP and Liquid liquid Separation is recycled to extraction absorption tower as extraction absorbent after being mixed in proportion and makes
With.
In described method, containing 0.28～0.30Kg/m in described tail gas3Dichloromethane, 0.14～0.16Kg/m3One
Chlroacetone and 0.50～0.52Kg/m3Water.
In described method, in extraction absorbent, the volume ratio of DOP and water is preferably 1: 1.5～2.0, and optimal proportion is 1:
1.5。
In described method, being provided with 5 grades of bubble-cap extraction absorption tower levels in extraction absorption tower, extraction absorption tower level is extraction
With absorption tower level, it it is again the distributor of extraction absorbent.
In described method, tail gas is 1: 0.1～0.15 with the volume ratio of extraction absorbent, and after extraction absorbs, extraction absorbs
In top of tower tail gas, content of organics is less than 0.0021Kg/m3；After bottom liquid phases material is for absorbing dichloromethane and monochloroacetone
Extraction absorbent, through Liquid liquid Separation, lower water layer is containing COD less than 500PPM, and top organic layer dioctyl phthalate is again
Send into side line rectifying column to process, control rectification condition, tower top, the end and side line extraction content >=98.5% dichloromethane respectively, >=
97.3% monochloroacetone and >=99.9%DOP.
Described side line rectifying column operation pressure 0.306 × 105N/m2, reflux ratio 1～2, control tower top temperature 49.2～
51.3 DEG C, side stream temperature 73.9～74.8 DEG C, column bottom temperature 110.5～113.9 DEG C.
The described preferred number of plates of side line rectifying column is 62, feed entrance point 51, lateral line discharging position 32.
Beneficial effect: the multitple extraction of the present invention absorbs dichloromethane and the side of monochloroacetone in MCPA,MCP,methoxone synthesis tail gas
Method, can effectively extract dichloromethane and monochloroacetone in absorption MCPA,MCP,methoxone synthesis tail gas, uses bubble-cap extraction absorption tower level, extraction
Take absorption tower level and not only play the effect that extraction absorbs, simultaneously work as extracting the distributed effect of absorbent.After extraction absorbs, extraction is inhaled
Receive in top of tower tail gas and be less than 0.0021Kg/m containing Organic substance3, extraction absorption tower bottom liquid phases is layered through liquid liquid, and lower water layer contains
COD be less than 500PPM, upper organic layer (DOP) deliver to side line rectifying column process, respectively obtain dichloromethane, monochloroacetone and
DOP, suitably under conditions of, their content is dichloromethane >=98.5%, monochloroacetone >=97.3% and >=DOP99.9%.
Water after DOP and Liquid liquid Separation is mixed in proportion Posterior circle and uses as extraction absorbent to extraction absorption tower.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not to be embodied as
Mode is limited, but is defined in the claims.
Accompanying drawing explanation
Fig. 1 is the multitple extraction absorption technique flow chart of the present invention；
Wherein: 1 be multitple extraction absorption tower, 2 liquid liquid stand sections, 3 bubble-cap extraction tower levels, 4 extraction absorbent charging apertures, 5
Gas phase stands section, 6 liquid liquid layering tank, 7 side line rectifying columns, 8 side line discharges, 9 side line rectifying tower top condensers, 10 side line rectification
Return tank of top of the tower, 11 side line rectifying column charging apertures, 12 side line rectification tower reactors, 13 MCPA,MCP,methoxone synthesis tail gas, 14 extraction absorption towers
End liquid phase discharging opening, 15 extraction absorb after tail gas, 16 liquid liquid layering tank aqueous phase dischargings, 17 liquid liquid layering tank organic facies dischargings, 18
Side line rectifying tower ejects to go out at the bottom of material, 19 side line rectifying column lateral line dischargings, 20 extraction absorbent chargings, 21 side line rectifying towers
Material.
Fig. 2 is the structure chart of bubble-cap extraction absorption tower level；
Wherein: 22 is bubble-cap extraction absorption tower level, 23 collecting tanks, 24 flanges, 25 bolts, 26 bubble-caps, 27 airways.
Detailed description of the invention
Below by specific embodiment, technical solutions according to the invention are further described in detail, but are necessary
Point out that following example are served only for the description to summary of the invention, be not intended that limiting the scope of the invention.
The multitple extraction that uses of the present invention absorbs dichloromethane, monochloroacetone and the side of water in MCPA,MCP,methoxone synthesis tail gas
Method, uses technological process shown in Fig. 1.With dioctyl phthalate (DOP) and water mixed liquid for extraction absorbent, in tail gas
Dichloromethane and monochloroacetone carry out multitple extraction absorption；Extraction absorbent is after Liquid liquid Separation, and dioctyl phthalate is again
Entering side line rectifying column to process, tower top, the end and side line extraction dichloromethane, monochloroacetone and DOP, DOP respectively are with water in proportion
It is recycled to extract absorption tower as extraction absorbent after mixing.
As it is shown in figure 1, the multitple extraction absorption tower 1 of the present invention is provided with 5 grades of bubble-cap extraction absorption tower levels 3, bubble-cap extraction is inhaled
Receive tower level 3 as shown in Figure 2.It is known to those skilled in the art that the extraction absorption tower 1 upper/lower terminal in bubble-cap extraction absorption tower level 3
Include that liquid liquid stands section 2 and gas phase stands section 5 respectively.
According to MCPA,MCP,methoxone synthesis technique, containing 0.29Kg/m in tail gas described under representative condition3Dichloromethane,
0.15Kg/m3Monochloroacetone and 0.51Kg/m3Water.Will be containing 0.29Kg/m3Dichloromethane, 0.15Kg/m3Monochloroacetone and
0.51Kg/m3The tail gas 13 of water delivers to extract the bottom (liquid liquid stand section 2 above) on absorption tower 1, with DOP and water mixed liquid for extraction
The ratio taking absorbent, DOP and water is 1: 1.5, and from the top on extraction absorption tower 1, (gas phase stands section 5 extraction absorbent 20
Just) charging aperture 4 adds, and extraction absorbent 20 is 1: 0.1 with the volume ratio of tail gas 13, the 5 grades of bubbles set in extraction absorption tower 1
Cover extraction tower level 3, carries out multitple extraction absorption to dichloromethane in tail gas 13 and monochloroacetone, and extraction absorption tower 1 operates temperature
It it is 20.0～30.0 DEG C.After extraction absorbs, containing Organic substance less than 0.0021Kg/m in extraction top, absorption tower tail gas 153, extraction
Absorption tower bottom liquid phases 14 enters liquid liquid layering tank 6, and after Liquid liquid Separation, lower water layer 16 is containing COD less than 500PPM, and upper strata has
Machine layer 17 is delivered to side line rectifying column 7 and is processed.It is dichloromethane that side line rectifying column 7 ejects material 18, recycles as solvent；Side line
Rectifying column lateral line discharging 19 is monochloroacetone, and side line rectifier bottoms discharging 21 is that DOP, DOP are layered tank 6 lower floor aqueous phase with liquid liquid
Recycle as extraction absorbent 20 after 1: 1.5 ratio mixing by volume.
The condition shown in table 1 of employing, in MCPA,MCP,methoxone synthesis tail gas, dichloromethane and monochloroacetone extraction absorption result are shown in
Shown in table 2.
Said method obtains result shown in table 2, processes 1m3Containing 0.29Kg/m3Dichloromethane, 0.15Kg/m3One chlorine third
Ketone and 0.51Kg/m3The tail gas of water, after extraction absorbs, is less than containing Organic substance in the overhead of extraction absorption tower 1
0.0021Kg/m3, side line rectifying column 7 respectively obtain more than 98% dichloroethanes, 97% monochloroacetone and 99.9%DOP, DOP with
Liquid liquid layering tank 6 lower layer of water 1: 1.5 ratio by volume is recycled to extraction absorption tower and uses.
Table 1 multitple extraction absorption technique condition
Table 2 multitple extraction absorption and separation result
Claims (8)
1. using multitple extraction to absorb dichloromethane and a method for monochloroacetone in MCPA,MCP,methoxone synthesis tail gas, its feature exists
In, MCPA,MCP,methoxone synthesis tail gas is delivered to the bottom on multitple extraction absorption tower, with dioctyl phthalate and the mixed liquor of water
For extraction absorbent, being added from the top on extraction absorption tower by extraction absorbent, tail gas is 1 with the volume ratio of extraction absorbent:
0.1～0.15, dichloromethane in tail gas and monochloroacetone are carried out multitple extraction absorption；After extraction absorbs, extraction absorbs tower top
In portion's tail gas, content of organics is less than 0.0021Kg/m3；Extraction absorption tower bottom liquid phases contains COD through Liquid liquid Separation, lower floor's aqueous phase
Less than 500PPM, upper organic layer is delivered to side line rectifying column and is processed；Described organic layer separates through rectification, side line rectifying tower top extraction
Dichloromethane, side line rectifying column side take-off monochloroacetone, extraction dioctyl phthalate, O-phthalic at the bottom of side line rectifying column
Lower floor's aqueous phase after dioctyl phthalate and Liquid liquid Separation recycles as extraction absorbent after being mixed in proportion.
Employing multitple extraction the most according to claim 1 absorbs dichloromethane and monochloroacetone in MCPA,MCP,methoxone synthesis tail gas
Method, it is characterised in that in described extraction absorbent, the volume ratio of dioctyl phthalate and water be 1: 1.5～
2.0。
Employing multitple extraction the most according to claim 2 absorbs dichloromethane and monochloroacetone in MCPA,MCP,methoxone synthesis tail gas
Method, it is characterised in that in described extraction absorbent, the volume ratio of dioctyl phthalate and water is 1: 1.5.
Employing multitple extraction the most according to claim 1 and 2 absorbs dichloromethane and a chlorine in MCPA,MCP,methoxone synthesis tail gas
The method of acetone, it is characterised in that in described method, containing 0.28～0.30Kg/m in described tail gas3Dichloromethane,
0.14～0.16Kg/m3Monochloroacetone and 0.50～0.52Kg/m3The gas of water.
Employing multitple extraction the most according to claim 1 and 2 absorbs dichloromethane and a chlorine in MCPA,MCP,methoxone synthesis tail gas
The method of acetone, it is characterised in that be provided with 5 grades of bubble-cap extraction absorption tower levels in described extraction absorption tower.
Employing multitple extraction the most according to claim 1 and 2 absorbs dichloromethane and a chlorine in MCPA,MCP,methoxone synthesis tail gas
The method of acetone, it is characterised in that in described method, side line rectifying column tower top, the end and side line extraction content respectively >=
The dichloromethane of 98.5%, the monochloroacetone of content >=97.3% and the dioctyl phthalate of content >=99.9%.
Employing multitple extraction the most according to claim 6 absorbs dichloromethane and monochloroacetone in MCPA,MCP,methoxone synthesis tail gas
Method, it is characterised in that described side line rectifying column operation pressure 0.306 × 105N/m2, reflux ratio 1～2, control tower top temperature
Spend 49.2～51.3 DEG C, side stream temperature 73.9～74.8 DEG C, column bottom temperature 110.5～113.9 DEG C.
8. absorb dichloromethane and monochloroacetone in MCPA,MCP,methoxone synthesis tail gas according to the employing multitple extraction described in claim 6
Method, it is characterised in that described side line rectifying tower plates number is 62, feed entrance point 51, lateral line discharging position 32.
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| CN109867585A (en) * | 2017-12-01 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of chloropropene prepares epichlorohydrin reaction process waste gas processing method |
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Inventor after: Dong Liangsheng Inventor after: Lu Jingsong Inventor after: Du Ying Inventor before: Gu Zhenggui Inventor before: Sun Hao |
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Effective date of registration: 20170511 Address after: 223800 Suqian eco chemical science and Technology Industrial Park, Jiangsu, Huaian Province, No. five, No. 1 Patentee after: Jiangsu Jiangu Chemical Industry Co., Ltd. Address before: Ninghai Gulou District of Nanjing city of Jiangsu Province, No. 122 210097 Patentee before: Nanjing Normal University |
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Address after: 223800 Suqian ecological chemical industry science and Technology Industrial Park, 1, No. five road, Suqian, Jiangsu Patentee after: Jiangsu Jiangu Chemical Industry Co., Ltd. Address before: 223800 Suqian ecological chemical industry science and Technology Industrial Park, 1, No. five road, Huaian, Jiangsu Patentee before: Jiangsu Jiangu Chemical Industry Co., Ltd. |