CN104844416A - Method for multistage extracting and absorpting dichloromethane and monochloroacetone in MCPa synthetic tail gas - Google Patents
Method for multistage extracting and absorpting dichloromethane and monochloroacetone in MCPa synthetic tail gas Download PDFInfo
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- CN104844416A CN104844416A CN201510137936.3A CN201510137936A CN104844416A CN 104844416 A CN104844416 A CN 104844416A CN 201510137936 A CN201510137936 A CN 201510137936A CN 104844416 A CN104844416 A CN 104844416A
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Abstract
A method for multistage extracting and absorpting dichloromethane and monochloroacetone in MCPa synthetic tail gas is provided. Multistage extraction absorption is performed on dichloromethane and monochloroacetone in the tail gas in a multistage extraction absorption tower by using DOP and water as an extraction absorption agent, wherein a volume ratio of the tail gas to the extraction absorption agent is 1: 0.1 to 0.15, and a volume ratio of DOP to water is 1: 1.5 to 2.0; after extraction absorption, organic matter content in the tail gas on the top of the extraction absorption tower is lower than 0.0021 kg/m<3>, content of COD of a lower water phase is lower than 500 PPM through liquid-liquid separation of a liquid phase at the bottom of the extraction absorption tower, and an upper organic layer is sent to a side rectifying tower for treatment; and >=98.5% dichloromethane is extracted on the top of the side rectifying tower, >=97.3% monochloroacetone is extracted on the side of the side rectifying tower, >=99.9% DOP is extracted at the bottom of the side rectifying tower, and DOP is recycled to the extraction absorption tower and used as the extraction absorption agent after being proportionally mixed with the lower water phase after liquid-liquid separation.
Description
Technical field
The present invention relates to a kind of technique of pesticide intermediate production process vent gas treatment, particularly relate to a kind of multi-stage solvent extraction and absorb organic method in methoxone synthesis tail gas.
Background technology
Methoxone, chemical name 2-methyl-4-chlorophenoxyacetic acid is that China produces and the sterilant of a kind of efficient, low toxicity, highly selective that uses and weedicide in recent years in a large number.In methoxone building-up process, employing Mono Chloro acetone is synthetic, causes the tail gas produced in its synthesis containing a certain amount of methylene dichloride, Mono Chloro acetone and water.Tail gas during methoxone is produced, pond is adopted to absorb in current industrial production, then biochemical treatment is carried out, still very high containing organism in tail gas after pond absorbs, easily cause environmental pollution, water after tail gas absorption carries out biochemical treatment, and processing costs is high, cause tail gas treatment device invest high, cost is large.
The present invention proposes the tail gas that the process of a kind of multi-stage solvent extraction absorption process contains methylene dichloride and Mono Chloro acetone, methylene dichloride and Mono Chloro acetone in tail gas is not only made to remove more thorough, after simultaneously stability, the COD of water is lower than 500PPM, and in treating processes, extraction absorption agent used and methylene dichloride and Mono Chloro acetone can be recycled.
Summary of the invention
A kind of multi-stage solvent extraction is the object of the present invention is to provide to absorb the method for methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, can methylene dichloride and Mono Chloro acetone in effective elimination tail gas, realize recovery or the recycle of methylene dichloride and Mono Chloro acetone simultaneously, and after absorbing in water COD lower than 500PPM.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method adopting multi-stage solvent extraction to absorb methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, it is characterized in that, methoxone synthesis tail gas is delivered to the bottom on multi-stage solvent extraction absorption tower, with dioctyl phthalate (DOP) (DOP) and water mixed liquid for extraction absorption agent, the top of extraction absorption agent from extraction absorption tower is added, tail gas is 1: 0.1 ~ 0.15 with the volume ratio of extraction absorption agent, carries out multi-stage solvent extraction absorption to methylene dichloride in tail gas and Mono Chloro acetone; After extraction absorbs, in the tail gas of extraction top, absorption tower, organic content is lower than 0.0021Kg/m
3; Extraction absorption tower bottom liquid phases is through Liquid liquid Separation, and lower floor's aqueous phase is containing COD lower than 500PPM, and upper organic layer delivers to the process of side line rectifying tower; Described organic layer is through rectifying separation, and the discharging of side line rectifying tower top is methylene dichloride, and use as solvent cycle, side line rectifying tower lateral line discharging is Mono Chloro acetone, and the discharging of side line rectifier bottoms is DOP; Lower floor's aqueous phase after DOP and Liquid liquid Separation is mixed in proportion and is circulated to and extracts absorption tower as extracting absorption agent and use afterwards.
In described method, containing 0.28 ~ 0.30Kg/m in described tail gas
3methylene dichloride, 0.14 ~ 0.16Kg/m
3mono Chloro acetone and 0.50 ~ 0.52Kg/m
3water.
In described method, in extraction absorption agent, the volume ratio of DOP and water is preferably 1: 1.5 ~ 2.0, and optimum proportion is 1:1.5.
In described method, be provided with 5 grades of bubble-cap extraction absorption tower levels in extraction absorption tower, extraction absorption tower level is extraction and absorption tower level, is again the sparger of extraction absorption agent.
In described method, tail gas is 1: 0.1 ~ 0.15 with the volume ratio of extraction absorption agent, and in the tail gas of extraction absorption rear extraction top, absorption tower, organic content is lower than 0.0021Kg/m
3; Bottom liquid phases material is the extraction absorption agent after absorbing methylene dichloride and Mono Chloro acetone, through Liquid liquid Separation, lower water layer contains COD lower than 500PPM, top organic layer dioctyl phthalate (DOP) sends into the process of side line rectifying tower again, control rectifying condition, tower top, the end and side line be extraction content>=98.5% methylene dichloride,>=97.3% Mono Chloro acetone and>=99.9%DOP respectively.
Described side line rectifying tower working pressure 0.306 × 10
5n/m
2, reflux ratio 1 ~ 2, controls 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 stage number of side line rectifying tower is 62, feed entrance point 51, lateral line discharging position 32.
Beneficial effect: multi-stage solvent extraction of the present invention absorbs the method for methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, effectively can extract and absorb methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, adopt bubble-cap extraction absorption tower level, extraction absorption tower level not only plays the effect that extraction absorbs, and plays the distributed effect of extraction absorption agent simultaneously.After extraction absorbs, in the tail gas of extraction top, absorption tower, contain organism lower than 0.0021Kg/m
3extraction absorption tower bottom liquid phases is through the layering of liquid liquid, lower water layer contains COD lower than 500PPM, upper organic layer (DOP) delivers to the process of side line rectifying tower, obtain methylene dichloride, Mono Chloro acetone and DOP respectively, under suitable condition, their content is methylene dichloride>=98.5%, Mono Chloro acetone>=97.3% and>=DOP99.9%.Water after DOP and Liquid liquid Separation is mixed in proportion Posterior circle and uses as extracting absorption agent to extracting absorption tower.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not limited with embodiment, but is limited by claim.
Accompanying drawing explanation
Fig. 1 is multi-stage solvent extraction absorption technique schema of the present invention;
Wherein: 1 is multi-stage solvent extraction absorption tower, the 2 liquid liquid sections of leaving standstill, 3 bubble-cap extraction tower levels, 4 extraction absorption agent opening for feeds, the 5 gas phase sections of leaving standstill, 6 liquid liquid layering tanks, 7 side line rectifying tower, 8 side line discharges, 9 side line rectifying tower top condensers, 10 side line rectifying tower top return tanks, 11 side line rectifying tower opening for feeds, 12 side line rectifying tower reactors, 13 methoxone synthesis tail gas, liquid phase discharge port at the bottom of 14 extraction absorption towers, tail gas after 15 extractions absorb, 16 liquid liquid layering tank aqueous phase dischargings, 17 liquid liquid layering tank organic phase dischargings, 18 side line rectifying towers eject material, 19 side line rectifying tower lateral line dischargings, 20 extraction absorption agent chargings, discharging at the bottom of 21 side line rectifying towers.
Fig. 2 is the structure iron of bubble-cap extraction absorption tower level;
Wherein: 22 is bubble-cap extraction absorption tower level, 23 receiving tanks, 24 flanges, 25 bolts, 26 bubble-caps, 27 airways.
Embodiment
Below by specific embodiment, technical solutions according to the invention are further described in detail, but are necessary to point out that following examples are only for the description to summary of the invention, do not form limiting the scope of the invention.
Employing multi-stage solvent extraction of the present invention absorbs the method for methylene dichloride, Mono Chloro acetone and water in methoxone synthesis tail gas, adopts technical process shown in Fig. 1.With dioctyl phthalate (DOP) (DOP) and water mixed liquid for extraction absorption agent, multi-stage solvent extraction absorption is carried out to methylene dichloride in tail gas and Mono Chloro acetone; Extraction absorption agent is after Liquid liquid Separation, and dioctyl phthalate (DOP) enters the process of side line rectifying tower again, and tower top, the end and side line respectively extraction methylene dichloride, Mono Chloro acetone and DOP, DOP and water are mixed in proportion and are recycled to extract absorption tower as extracting absorption agent afterwards.
As shown in Figure 1, multi-stage solvent extraction absorption tower 1 of the present invention is provided with 5 grades of bubble-cap extraction absorption tower levels 3, and bubble-cap extraction absorption tower level 3 as shown in Figure 2.It is known to those skilled in the art that extraction absorption tower 1 comprises the liquid liquid section of leaving standstill 2 and the gas phase section of leaving standstill 5 respectively at the upper/lower terminal of bubble-cap extraction absorption tower level 3.
According to methoxone synthesis technique, containing 0.29Kg/m in tail gas described under representative condition
3methylene dichloride, 0.15Kg/m
3mono Chloro acetone and 0.51Kg/m
3water.Will containing 0.29Kg/m
3methylene dichloride, 0.15Kg/m
3mono Chloro acetone and 0.51Kg/m
3the tail gas 13 of water delivers to the bottom (above the liquid liquid section of leaving standstill 2) on extraction absorption tower 1, with DOP and water mixed liquid for extraction absorption agent, the ratio of DOP and water is 1: 1.5, extraction absorption agent 20 adds from top (above the gas phase section of the leaving standstill 5) opening for feed 4 on extraction absorption tower 1, extraction absorption agent 20 is 1: 0.1 with the volume ratio of tail gas 13,5 grades of bubble-cap extraction tower levels 3 of establishing in extraction absorption tower 1, carry out multi-stage solvent extraction absorption to methylene dichloride in tail gas 13 and Mono Chloro acetone, extraction absorption tower 1 service temperature is 20.0 ~ 30.0 DEG C.After extraction absorbs, in extraction top, absorption tower tail gas 15, contain organism lower than 0.0021Kg/m
3, 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 lower than 500PPM, and upper organic layer 17 is delivered to side line rectifying tower 7 and processed.Side line rectifying tower 7 ejects material 18 for methylene dichloride, uses as solvent cycle; Side line rectifying tower lateral line discharging 19 is Mono Chloro acetone, side line rectifier bottoms discharging 21 be DOP, DOP with liquid liquid layering tank 6 lower floor aqueous phase by volume 1: 1.5 ratio recycle as extracting absorption agent 20 after mixing.
The condition shown in table 1 of employing, in methoxone synthesis tail gas, methylene dichloride and Mono Chloro acetone extraction absorption the results are shown in Table shown in 2.
Aforesaid method obtains result shown in table 2, process 1m
3containing 0.29Kg/m
3methylene dichloride, 0.15Kg/m
3mono Chloro acetone and 0.51Kg/m
3the tail gas of water, after extraction absorbs, contains organism lower than 0.0021Kg/m in the overhead of extraction absorption tower 1
3, side line rectifying tower 7 obtain respectively more than 98% ethylene dichloride, 97% Mono Chloro acetone and 99.9%DOP, DOP and liquid liquid layering tank 6 lower layer of water by volume 1: 1.5 ratio be circulated to and extract absorption tower and use.
Table 1 multi-stage solvent extraction absorption technique condition
Table 2 multi-stage solvent extraction absorption extraction result
Claims (8)
1. the method adopting multi-stage solvent extraction to absorb methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, it is characterized in that, methoxone synthesis tail gas is delivered to the bottom on multi-stage solvent extraction absorption tower, with the mixed solution of dioctyl phthalate (DOP) and water for extraction absorption agent, the top of extraction absorption agent from extraction absorption tower is added, tail gas is 1: 0.1 ~ 0.15 with the volume ratio of extraction absorption agent, carries out multi-stage solvent extraction absorption to methylene dichloride in tail gas and Mono Chloro acetone; After extraction absorbs, in the tail gas of extraction top, absorption tower, organic content is lower than 0.0021Kg/m
3; Extraction absorption tower bottom liquid phases is through Liquid liquid Separation, and lower floor's aqueous phase is containing COD lower than 500PPM, and upper organic layer delivers to the process of side line rectifying tower; Described organic layer is through rectifying separation, side line rectifying tower top extraction methylene dichloride, side line rectifying tower side take-off Mono Chloro acetone, extraction dioctyl phthalate (DOP) at the bottom of side line rectifying tower, the lower floor's aqueous phase after dioctyl phthalate (DOP) and Liquid liquid Separation is mixed in proportion and recycles as extracting absorption agent afterwards.
2. employing multi-stage solvent extraction according to claim 1 absorbs the method for methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, and it is characterized in that, in described extraction absorption agent, the volume ratio of dioctyl phthalate (DOP) and water is 1: 1.5 ~ 2.0.
3. employing multi-stage solvent extraction according to claim 2 absorbs the method for methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, and it is characterized in that, in described extraction absorption agent, the volume ratio of dioctyl phthalate (DOP) and water is 1: 1.5.
4. employing multi-stage solvent extraction according to claim 1 and 2 absorbs the method for methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, it is characterized in that, in described method, containing 0.28 ~ 0.30Kg/m in described tail gas
3methylene dichloride, 0.14 ~ 0.16Kg/m
3mono Chloro acetone and 0.50 ~ 0.52Kg/m
3the gas of water.
5. employing multi-stage solvent extraction according to claim 1 and 2 absorbs the method for methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, it is characterized in that, is provided with 5 grades of bubble-cap extraction absorption tower levels in described extraction absorption tower.
6. employing multi-stage solvent extraction according to claim 1 and 2 absorbs the method for methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, it is characterized in that, in described method, side line rectifying tower tower top, the end and side line be extraction methylene dichloride content >=98.5%, Mono Chloro acetone content >=97.3% and dioctyl phthalate (DOP) content >=99.9% respectively.
7. employing multi-stage solvent extraction according to claim 6 absorbs the method for methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas, it is characterized in that, described side line rectifying tower working pressure 0.306 × 10
5n/m
2, reflux ratio 1 ~ 2, controls 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.
8. absorb the method for methylene dichloride and Mono Chloro acetone in methoxone synthesis tail gas according to employing multi-stage solvent extraction according to claim 6, it is characterized in that, described side line rectifying tower plates number is 62, feed entrance point 51, lateral line discharging position 32.
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| CN201510137936.3A CN104844416B (en) | 2015-03-26 | 2015-03-26 | Multitple extraction absorbs dichloromethane and the method for monochloroacetone in MCPA,MCP,methoxone synthesis tail gas |
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| CN201510137936.3A CN104844416B (en) | 2015-03-26 | 2015-03-26 | Multitple extraction absorbs dichloromethane and the method for monochloroacetone in MCPA,MCP,methoxone synthesis tail gas |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN110545895A (en) * | 2017-04-14 | 2019-12-06 | 山东爱地高分子材料有限公司 | Process for recovering dichloromethane in waste gas |
| CN113350976A (en) * | 2021-06-07 | 2021-09-07 | 南京师范大学 | Tail gas treatment and recovery method |
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| CN1403382A (en) * | 2002-10-21 | 2003-03-19 | 南京大学 | Method of treating phenol-containing effluent and recovering resource in 2-methyl-4-chlorophenoxyacetic acid producing process |
| CN102674607A (en) * | 2012-05-03 | 2012-09-19 | 江苏健谷化工有限公司 | Method for treating acid wastewater of 2-methyl-4-chlorophenoxyacetic acid through extraction, neutralization and distillation integration |
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| CN1403382A (en) * | 2002-10-21 | 2003-03-19 | 南京大学 | Method of treating phenol-containing effluent and recovering resource in 2-methyl-4-chlorophenoxyacetic acid producing process |
| CN102674607A (en) * | 2012-05-03 | 2012-09-19 | 江苏健谷化工有限公司 | Method for treating acid wastewater of 2-methyl-4-chlorophenoxyacetic acid through extraction, neutralization and distillation integration |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110545895A (en) * | 2017-04-14 | 2019-12-06 | 山东爱地高分子材料有限公司 | Process for recovering dichloromethane in waste gas |
| 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 |
| CN113350976A (en) * | 2021-06-07 | 2021-09-07 | 南京师范大学 | Tail gas treatment and recovery method |
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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. |
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