CN102500193A - 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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- CN102500193A CN102500193A CN2011103740625A CN201110374062A CN102500193A CN 102500193 A CN102500193 A CN 102500193A CN 2011103740625 A CN2011103740625 A CN 2011103740625A CN 201110374062 A CN201110374062 A CN 201110374062A CN 102500193 A CN102500193 A CN 102500193A
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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
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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 of the DMF of being used for synthetic tower tail gas.
Background technology
The DMF formal name used at school is a dimethyl formamide; Be that a kind of chemical property is stable, boiling point and high good polar solvent and the important chemical material of flash-point; Also can be used as the catalyst of chemical reaction, it is widely used in industries such as process hides, electronics, staple fibre, pharmacy, petrochemical industry, rubber.So DMF demand and development space are huge.
General industry production DMF is the reaction of follow-upization of synthesis of methylamines; With methyl alcohol and ammonia is that initiation material is produced monomethyl amine, dimethylamine, trimethylamine etc.; Then dimethylamine and carbon monoxide are added in the agitated reactor, add catalyst again, get the DMF product through separated.But after DMF is synthetic a large amount of tail gas is arranged, be mainly dimethylamine, methyl alcohol, CO and part inert gas H2, N2 etc., environment is polluted; Wherein dimethylamine combustion; Form explosive mixture with the air mixing energy, contact fierce reaction with oxidant, can be diffused into place quite far away in the lower.Existing processing method is tail gas to be got into surge tank through recirculated water with-10～0 ℃ of chilled brine cooling back carry out gas-liquid separation mostly; Part is sent into the synthetic tower second use and is used after compressor pressurizes makes its pressure greater than synthetic tower pressure, emptying on the spot after another part tail gas send water sealed tank to absorb.
But this kind method has following shortcoming: the one, and when technological fluctuation, when particularly the synthetic tower material did not react, emptying amount increase suddenly caused entrained liquid, damages compressor; The 2nd, under the normal condition after the vent gas treatment CO content lower, inert gas is higher, value is very low; The 3rd, this kind technology produces a large amount of water sealed tank waste water and emptying end gas, causes waste water and exhaust emission.
Summary of the invention
The object of the invention will solve above-mentioned deficiency exactly, and a kind of recoverying and utilizing method that can tail gas be made full use of, reduce the safe tail gas of pollution is provided, and another object of the present invention provides a kind of retracting device of realizing this method.
In order to achieve the above object, the present invention provides a kind of recoverying and utilizing method of the DMF of being used for synthetic tower tail gas, may further comprise the steps:
(1) after the mixed tail gas that the DMF synthetic tower is come out passes through circulating water cooling, gets into-10～0 ℃ of chilled brine again and cool off;
(2) will cool off the methyl alcohol of back in the tail gas, dimethylamine etc. and feed bottom, methyl alcohol absorption tower, another part tail gas gets into and carries out emptying again after water sealed tank absorbs;
(3) dimethylamine is absorbed by methanol solution, gets into the 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, through methanol pump the methyl alcohol in the methyl alcohol groove is squeezed into the methyl alcohol absorption tower on top, described methyl alcohol absorption tower, form the spray shape, the methyl alcohol behind the absorption dimethylamine flows back in the methyl alcohol groove again, forms a circulation.
Like this, carry out DMF when synthetic, after handling through recirculated water and-10～0 ℃ of dual cooling of chilled brine from DMF synthetic tower tail gas discharged; Exhaust temperature is reduced to about 0 ℃; At this moment the dimethylamine and the methyl alcohol that come out from the chilled brine condenser are liquid, utilize the self gravitation effect, get into the bottom on methyl alcohol absorption tower from pipeline; The spray of methanol solution is arranged at top, methyl alcohol absorption tower; The dimethylamine that gets into the methyl alcohol absorption tower is absorbed by methanol solution fully, get into the methyl alcohol groove then together and store, as the synthetic reaction raw materials of methylamine.Other tail gas CO, H2, N2 etc. absorb back emptying or the top emptying from the methyl alcohol absorption tower through water sealed tank, basically air, water source etc. are not polluted.
Utilize method in order to realize tail gas recycle of the present invention; 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 inserts the bottom on a methyl alcohol absorption tower, and bottom, described methyl alcohol absorption tower and methyl alcohol groove join.
Top, described 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 top, described methyl alcohol absorption tower is provided with evacuation port.
After adopting above-mentioned retracting device; Owing to be provided with the methyl alcohol absorption tower, can environmentally harmful methyl alcohol and dimethylamine be absorbed as the synthesis material use, both there be not the pollution that causes environment in air or the water because of being discharged into; Can also be as synthesis material, the production cost that significantly reduces.And do not have compressor in this device, reduced maintenance cost.And because tail gas after dual cooling is handled through recirculated water and-10～0 ℃ of chilled brine; Exhaust temperature is reduced to about 0 ℃, and the dimethylamine and the methyl alcohol that at this moment come out from the chilled brine condenser are liquid, utilizes self gravitation to get in the methyl alcohol absorption tower; If the tail gas amount is too much; Lower boiling gas such as N2, H2 etc. just get into water sealed tank through gate valve and carry out the emptying processing, even there is the dimethylamine gas of trace not get into the methyl alcohol absorption tower, also can be absorbed by the water in the water sealed tank.Like this, basically, dimethylamine, methyl alcohol etc. can not endanger environment generation task.Also can discharge after also having the lower boiling gas of part to get into the methyl alcohol absorption tower 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 harmful tail gas dimethylamine, methyl alcohol etc. be recovered fully to use, reduced the pollution to environment, can also make synthetic raw material, reduced production cost.
3, retracting device of the present invention is on original device, to transform, and cost investment is few, but the effect that reclaims is remarkable.
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Description of drawings
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is done further detailed explanation.
Fig. 1 is the process chart that tail gas recycle of the present invention is utilized method;
Fig. 2 is the retracting device signal that realization tail gas recycle of the present invention is utilized method.
Among the 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 one:
Tail gas recycle shown in Figure 1 is utilized in the process chart of method; After the mixed tail gas that at first the DMF synthetic tower is come out is handled through recirculated water and-10～0 ℃ of dual condenser cooling of chilled brine; Exhaust temperature is reduced to about 0 ℃; At this moment the dimethylamine and the methyl alcohol that come out from the chilled brine condenser are liquid, utilize the self gravitation effect, get into the bottom on methyl alcohol absorption tower from pipeline.Part gas turns back to the DMF synthetic tower and participates in further reaction, and another part gas gets into water sealed tank, is absorbed back emptying by water.The spray of methanol solution is arranged at top, methyl alcohol absorption tower, and the dimethylamine that gets into the methyl alcohol absorption tower is absorbed by methanol solution fully, gets into the methyl alcohol groove then together and stores, as the synthetic reaction raw materials of methylamine.The top emptying from the methyl alcohol absorption tower such as part tail gas CO, H2, N2; The useful tail gas that produces from the DMF synthetic tower like this has been absorbed and used basically entirely; And the gas that air, water source etc. is not had to pollute is with regard to emptying, and environmentally safe, prepared using is abundant; Help reducing production costs, and reduce cost environmental improvement.
Embodiment two:
Shown in Figure 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; At described control valve 8 and the gate valve 9 middle pipelines 11 that are provided with, described pipeline 11 inserts the bottom on a methyl alcohol absorption tower 5, and 5 bottoms, described 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 top, described methyl alcohol absorption tower is provided with evacuation port 10.
After adopting above-mentioned retracting device; Owing to be provided with the methyl alcohol absorption tower, can environmentally harmful methyl alcohol and dimethylamine be absorbed as the synthesis material use, both there be not the pollution that causes environment in air or the water because of being discharged into; Can also be as synthesis material, the production cost that significantly reduces.And do not have compressor in this device, reduced maintenance cost.And because after the dual cooling processing of tail gas process recirculated water cooling condenser and-10～chilled brine condenser; Exhaust temperature is reduced to about 0 ℃, and the dimethylamine and the methyl alcohol that at this moment come out from the chilled brine condenser are liquid, utilizes self gravitation to get in the methyl alcohol absorption tower; If the tail gas amount is too much; Lower boiling gas such as N2, H2 etc. just get into water sealed tank through gate valve and carry out the emptying processing, even there is the dimethylamine gas of trace not get into the methyl alcohol absorption tower, also can be absorbed by the water in the water sealed tank.Like this, basically, dimethylamine, methyl alcohol etc. can not endanger environment generation task.Also can discharge after also having the lower boiling gas of part to get into the methyl alcohol absorption tower from the evacuation port on top, methyl alcohol absorption tower.
Above embodiment is not limited only to protection scope of the present invention, and all are based on basic thought of the present invention and all belonging in protection scope of the present invention of making amendment or change.
Claims (5)
1. recoverying and utilizing method that is used for DMF synthetic tower tail gas, it is characterized in that: described method may further comprise the steps:
(1) after the mixed tail gas that the DMF synthetic tower is come out is lowered the temperature through the recirculated water cooling condenser, gets into-10～0 ℃ of chilled brine condenser again and cool off;
Methyl alcohol, the dimethylamine that (2) will cool off in the tail gas of back feed bottom, methyl alcohol absorption tower, and another part tail gas gets into and carries out emptying again after water sealed tank absorbs;
(3) dimethylamine is absorbed by methanol solution fully, gets into the methyl alcohol groove and stores, and as the initiation material of synthesis of methylamines, other inert gases carry out emptying.
2. a kind of recoverying and utilizing method that is used for DMF synthetic tower tail gas according to claim 1 is characterized in that: in the said step (2), the methyl alcohol after top, said methyl alcohol absorption tower spray methanol solution absorbs dimethylamine flows back in the methyl alcohol groove again.
3. realize that above-mentioned tail gas recycle utilizes the retracting device of method for one kind; Comprise condenser, water sealed tank, control valve and gate valve; It is characterized in that: be provided with a pipeline in the middle of described control valve and the gate valve; Described pipeline inserts the bottom on a methyl alcohol absorption tower, and bottom, described methyl alcohol absorption tower and methyl alcohol groove join.
4. retracting device according to claim 3 is characterized in that: top, described methyl alcohol absorption tower is connected with a pump housing, and the described pump housing other end and methyl alcohol groove join.
5. retracting device according to claim 3 is characterized in that: described pipeline is provided with gate valve, and top, described methyl alcohol absorption tower is provided with evacuation port.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110374062.5A CN102500193B (en) | 2011-11-23 | 2011-11-23 | Recovery and utilization method for tail gas in DMF (Dimethyfumarate) synthetic tower and device |
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| CN201110374062.5A CN102500193B (en) | 2011-11-23 | 2011-11-23 | Recovery and utilization method for tail gas in DMF (Dimethyfumarate) synthetic tower and device |
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| CN102500193A true CN102500193A (en) | 2012-06-20 |
| CN102500193B CN102500193B (en) | 2014-03-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111056920A (en) * | 2019-12-17 | 2020-04-24 | 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 |
| CN113797716A (en) * | 2021-10-27 | 2021-12-17 | 聊城鲁西甲胺化工有限公司 | Tail gas treatment system of DMF (dimethyl formamide) production device, process and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| 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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2011
- 2011-11-23 CN CN201110374062.5A patent/CN102500193B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002136827A (en) * | 2000-11-07 | 2002-05-14 | Fuji Photo Film Co Ltd | Gas-liquid contact device and gas-liquid contact method |
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111056920A (en) * | 2019-12-17 | 2020-04-24 | 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 |
| 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 |
| CN113797716A (en) * | 2021-10-27 | 2021-12-17 | 聊城鲁西甲胺化工有限公司 | Tail gas treatment system of DMF (dimethyl formamide) production device, process and application |
| 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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| CN102500193B (en) | 2014-03-12 |
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