CN102500193B - Recovery and utilization method for tail gas in DMF (Dimethyfumarate) synthetic tower and device - Google Patents
Recovery and utilization method for tail gas in DMF (Dimethyfumarate) synthetic tower and device Download PDFInfo
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- CN102500193B CN102500193B CN201110374062.5A CN201110374062A CN102500193B CN 102500193 B CN102500193 B CN 102500193B CN 201110374062 A CN201110374062 A CN 201110374062A CN 102500193 B CN102500193 B CN 102500193B
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Abstract
The invention relates to a recovery and utilization method for tail gas in a DMF (Dimethyfumarate) synthetic tower, which comprises the following steps of: firstly cooling the mixed tail gas flowing out of the DMF synthetic tower with circulating water and then cooling in frozen brine of 10 below zero-0 DEG C; and leading into the bottom part of a methanol absorption tower for absorption, entering a methanol tank for storage and emptying the other part of tail gas subjected to water absorption or directly emptying. The invention also discloses a recovery device for realizing the recovery and the utilization of the tail gas. The recovery and utilization method has the beneficial effects that the recovery and utilization rate of the tail gas is high; the recovery and the reutilization of methanol, dimethylamine and the like are realized; and more importantly, the pollution to environment is avoided to bring the gospel to the environmental improvement.
Description
Technical field
The present invention relates to a kind of gas recovery techniques and device, relate in particular to a kind of recoverying and utilizing method and device for DMF synthetic tower tail gas.
Background technology
DMF formal name used at school is dimethyl formamide, good polar solvent that a kind of stable chemical nature, boiling point and flash-point are high and important industrial chemicals, also can be used as the catalyst of chemical reaction, it is widely used in the industries such as process hides, electronics, staple fibre, pharmacy, petrochemical industry, rubber.So DMF demand and development space are huge.
It is all the reaction of follow-upization of synthesis of methylamines that general industryization is produced DMF, take methyl alcohol and ammonia produces monomethyl amine, dimethylamine, trimethylamine etc. as initiation material, then dimethylamine and carbon monoxide are added in reactor, then add catalyst, through separated, obtain DMF product.But after DMF is synthetic, there is a large amount of tail gas, be mainly dimethylamine, methyl alcohol, CO and part inert gas H2, N2 etc., to environment, wherein dimethylamine combustion, form explosive mixture with air mixing energy, contact fierce reaction with oxidant, can be diffused in lower place quite far away.Existing processing method is tail gas to be entered to surge tank after recirculated water and-10~0 ℃ of chilled brine are cooling carry out gas-liquid separation mostly, part is sent into the utilization of synthetic tower secondary and is used after compressor pressurization makes its pressure be greater than synthetic tower pressure, emptying on the spot after another part tail gas send water sealed tank to absorb.
But this kind of method has following shortcoming: the one, when technological fluctuation, when particularly synthetic tower material does not react, emptying amount increases and causes entrained liquid suddenly, damages compressor; The 2nd, after vent gas treatment, CO content is lower under normal circumstances, and inert gas is higher, and value is very low; The 3rd, this kind of technique produces a large amount of water sealed tank waste water and emptying end gas, causes waste water and exhaust emission.
Summary of the invention
Object of the present invention will solve above-mentioned deficiency exactly, and a kind of recoverying and utilizing method that tail gas can be made full use of, reduce the safe tail gas of pollution is provided, and another object of the present invention is to provide a kind of retracting device of realizing the method.
In order to achieve the above object, the invention provides a kind of recoverying and utilizing method for DMF synthetic tower tail gas, comprise the following steps:
(1) by DMF synthetic tower mixed tail gas out after circulating water cooling, then enter-10~0 ℃ of chilled brines and carry out cooling;
(2) methyl alcohol in cooling rear tail gas, dimethylamine etc. are passed into bottom methyl alcohol absorption tower, another part tail gas enters after water sealed tank absorbs and carries out emptying again;
(3) dimethylamine is absorbed by methanol solution, enters methyl alcohol groove and stores, and as the initiation material of synthesis of methylamines, other inert gases carry out emptying.
For dimethylamine can be absorbed fully, on described top, methyl alcohol absorption tower, through methanol pump, the methyl alcohol in methyl alcohol groove is squeezed into methyl alcohol absorption tower, form shape spray, the methyl alcohol absorbing after dimethylamine flows back in methyl alcohol groove again, forms a circulation.
Like this, carry out DMF when synthetic, after from DMF synthetic tower tail gas out, through recirculated water and-10~0 ℃ of chilled brine, dual cooling is processed, exhaust temperature is down to 0 ℃ of left and right, at this moment from chilled brine condenser dimethylamine and methyl alcohol out, be liquid, utilize self gravitation effect, from pipeline, enter the bottom on methyl alcohol absorption tower, the spray of methanol solution is arranged at top, methyl alcohol absorption tower, the dimethylamine that enters methyl alcohol absorption tower is absorbed by methanol solution completely, then enter together methyl alcohol groove and store, as the synthetic reaction raw materials of methylamine.Other tail gas CO, H2, N2 etc. absorb rear emptying by water sealed tank or from the top emptying of methyl alcohol absorption tower, substantially air, water source etc. are not polluted.
In order to realize tail gas recycle of the present invention, utilize method, device for recovering tail gas of the present invention, comprise condenser, water sealed tank, control valve and gate valve, in the middle of described control valve and gate valve, be provided with a pipeline, described pipeline accesses the bottom on a methyl alcohol absorption tower, and described bottom, methyl alcohol absorption tower and methyl alcohol groove join.
Described top, methyl alcohol absorption tower is connected with a pump housing, and the described pump housing other end and methyl alcohol groove join.
Described pipeline is provided with gate valve, and described top, methyl alcohol absorption tower is provided with evacuation port.
Adopt after above-mentioned retracting device, owing to being provided with methyl alcohol absorption tower, environmentally harmful methyl alcohol and dimethylamine can be absorbed as synthesis material use, both there is no the pollution that causes environment in air or water because being discharged into, can also be as synthesis material, the production cost greatly reducing.And in this device, there is no compressor, reduced maintenance cost.And because tail gas after dual cooling is processed through recirculated water and-10~0 ℃ of chilled brine, exhaust temperature is down to 0 ℃ of left and right, at this moment from chilled brine condenser dimethylamine and methyl alcohol out, be liquid, utilize self gravitation to enter in methyl alcohol absorption tower, if tail gas amount is too much, lower boiling gas carries out emptying processing as N2, H2 etc. just enters water sealed tank by gate valve, even if there is micro-dimethylamine gas not enter methyl alcohol absorption tower, also can be absorbed by the water in water sealed tank.Like this, substantially, dimethylamine, methyl alcohol etc. can not endanger environment generation task.After also having the lower boiling gas of part to enter methyl alcohol absorption tower, also can discharge from the evacuation port on top, methyl alcohol absorption tower.
Beneficial effect of the present invention has:
1, method for recovering tail gas of the present invention is simple;
2, method for recovering tail gas of the present invention can make Tail Gas dimethylamine, methyl alcohol etc. be recovered completely to use, reduced the pollution to environment, can also make synthesis material, reduced production cost.
3, retracting device of the present invention is to transform on original device, and cost investment is few, but the effect reclaiming is remarkable.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the process chart that tail gas recycle of the present invention is utilized method;
Fig. 2 realizes the retracting device signal that tail gas recycle of the present invention is utilized method.
In figure: 1-synthetic tower, 2-water condenser, 3-refrigerated brine condenser, 4-water sealed tank, 5-methyl alcohol absorption tower, 6-methyl alcohol groove, 7-pump, 8-control valve, 9-gate valve, 10-evacuation port.
The specific embodiment
Embodiment mono-:
Tail gas recycle shown in Fig. 1 is utilized in the process chart of method, first DMF synthetic tower mixed tail gas is out lowered the temperature after processing through recirculated water and-10~0 ℃ of dual condenser of chilled brine, exhaust temperature is down to 0 ℃ of left and right, at this moment from chilled brine condenser dimethylamine and methyl alcohol out, be liquid, utilize self gravitation effect, from pipeline, enter the bottom on methyl alcohol absorption tower.Part gas turns back to DMF synthetic tower and participates in further reaction, and another part gas enters water sealed tank, emptying after being absorbed by water.The spray of methanol solution is arranged at top, methyl alcohol absorption tower, and the dimethylamine that enters methyl alcohol absorption tower is absorbed by methanol solution completely, then enters together methyl alcohol groove and stores, as the synthetic reaction raw materials of methylamine.Partial tail gas CO, H2, N2 etc. are from the top emptying of methyl alcohol absorption tower, the useful tail gas producing from DMF synthetic tower has like this been absorbed and used substantially entirely, and air, water source etc. is not had to the gas polluting with regard to emptying, environmentally safe, prepared using is abundant, be conducive to reduce production costs, and reduce the cost to environmental improvement.
Embodiment bis-:
Shown in Fig. 2 is mixed tail gas retracting device of the present invention, comprise recirculated water cooling condenser 2, refrigerated brine condenser 3, water sealed tank 4, control valve 8 and gate valve 9, in the middle of described control valve 8 and gate valve 9, be provided with a pipeline 11, the bottom on described pipeline 11 access one methyl alcohol absorption towers 5, described 5 bottoms, methyl alcohol absorption tower and methyl alcohol groove 6 join, 5 tops, methyl alcohol absorption tower are connected with a pump housing 7, and the pump housing 7 other ends and methyl alcohol groove 6 join.Pipeline 11 is provided with gate valve 9, and described top, methyl alcohol absorption tower is provided with evacuation port 10.
Adopt after above-mentioned retracting device, owing to being provided with methyl alcohol absorption tower, environmentally harmful methyl alcohol and dimethylamine can be absorbed as synthesis material use, both there is no the pollution that causes environment in air or water because being discharged into, can also be as synthesis material, the production cost greatly reducing.And in this device, there is no compressor, reduced maintenance cost.And after because of tail gas, through recirculated water cooling condenser and-10~chilled brine condenser, dual cooling is processed, exhaust temperature is down to 0 ℃ of left and right, at this moment from chilled brine condenser dimethylamine and methyl alcohol out, be liquid, utilize self gravitation to enter in methyl alcohol absorption tower, if tail gas amount is too much, lower boiling gas carries out emptying processing as N2, H2 etc. just enters water sealed tank by gate valve, even if there is micro-dimethylamine gas not enter methyl alcohol absorption tower, also can be absorbed by the water in water sealed tank.Like this, substantially, dimethylamine, methyl alcohol etc. can not endanger environment generation task.After also having the lower boiling gas of part to enter methyl alcohol absorption tower, also can discharge from the evacuation port on top, methyl alcohol absorption tower.
Above embodiment is not limited only to protection scope of the present invention, all based on basic thought of the present invention and all belonging in protection scope of the present invention of modifying or change.
Claims (4)
1. for a recoverying and utilizing method for DMF synthetic tower tail gas, it is characterized in that: described method comprises the following steps:
(1) by DMF synthetic tower mixed tail gas out through after recirculated water cooling condenser cooling, then enter-10~0 ℃ of chilled brine condensers and carry out cooling;
(2) methyl alcohol, dimethylamine in cooling rear tail gas are passed into bottom, methyl alcohol absorption tower, top, described methyl alcohol absorption tower spray methanol solution, flows back in methyl alcohol groove after absorption dimethylamine again; Another part tail gas enters after water sealed tank absorbs and carries out emptying again;
(3) after dimethylamine is absorbed completely by methanol solution, enter methyl alcohol groove and store, as the initiation material of synthesis of methylamines, other inert gases carry out emptying.
2. realize the retracting device that utilizes method for DMF synthetic tower tail gas recycle as claimed in claim 1 for one kind, comprise water condenser, water sealed tank, control valve and gate valve, it is characterized in that: in the middle of described control valve and gate valve, be provided with a pipeline, described pipeline accesses the bottom on a methyl alcohol absorption tower, and described bottom, methyl alcohol absorption tower and methyl alcohol groove join.
3. retracting device according to claim 2, is characterized in that: described top, methyl alcohol absorption tower is connected with a pump housing, and the described pump housing other end and methyl alcohol groove join.
4. retracting device according to claim 2, is characterized in that: described pipeline is provided with gate valve, and described top, methyl alcohol absorption tower is provided with evacuation port.
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CN111056920B (en) * | 2019-12-17 | 2022-09-09 | 陕西渭河煤化工集团有限责任公司 | Recovery method of volatile gas-phase methanol in methanol storage tank |
CN113797716B (en) * | 2021-10-27 | 2023-11-24 | 聊城鲁西甲胺化工有限公司 | Tail gas treatment system, process and application of DMF production device |
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CN1803256A (en) * | 2005-12-06 | 2006-07-19 | 浙江禾欣实业集团股份有限公司 | Dimethyl formamide effluent gases recovering and processing method for dry method synthetic leather |
CN101050183A (en) * | 2006-04-07 | 2007-10-10 | 山东华鲁恒升化工股份有限公司 | New type production system for methylamine, and new technique for producing methylamine by using the system |
CN202427318U (en) * | 2011-11-23 | 2012-09-12 | 安徽淮化股份有限公司 | Waste gas recycling device of dimethyl formamide (DMF) synthetic tower |
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JP2002136827A (en) * | 2000-11-07 | 2002-05-14 | Fuji Photo Film Co Ltd | Gas-liquid contact device and gas-liquid contact method |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN1803256A (en) * | 2005-12-06 | 2006-07-19 | 浙江禾欣实业集团股份有限公司 | Dimethyl formamide effluent gases recovering and processing method for dry method synthetic leather |
CN101050183A (en) * | 2006-04-07 | 2007-10-10 | 山东华鲁恒升化工股份有限公司 | New type production system for methylamine, and new technique for producing methylamine by using the system |
CN202427318U (en) * | 2011-11-23 | 2012-09-12 | 安徽淮化股份有限公司 | Waste gas recycling device of dimethyl formamide (DMF) synthetic tower |
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JP特开2002-136827A 2002.05.14 |
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