CN1459442A - Energy saving separation technology of refining dimethyl ether and recovery carbon dioxide at the same time - Google Patents
Energy saving separation technology of refining dimethyl ether and recovery carbon dioxide at the same time Download PDFInfo
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- CN1459442A CN1459442A CN02119856A CN02119856A CN1459442A CN 1459442 A CN1459442 A CN 1459442A CN 02119856 A CN02119856 A CN 02119856A CN 02119856 A CN02119856 A CN 02119856A CN 1459442 A CN1459442 A CN 1459442A
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Abstract
一种精制二甲醚同时回收二氧化碳的节能分离工艺，由吸收分离单元、精馏分离单元和余热回收制冷单元由三个部分组成。在吸收分离单元中，采用适当溶剂从反应产物尾气中回收DME和CO2。精馏分离单元中第一精馏塔分离出高纯度的CO2，第二精馏塔分离出高纯度的DME。余热回收制冷单元由上述两个精馏塔塔釜采出物的余热回收器以及氨吸收式制冷单元构成，以实现利用系统排弃的余热，驱动氨吸收式制冷循环产生冷量，提供作第一精馏塔塔顶冷凝负荷。本发明工艺对反应产物气体的DME回收率可以达到99％以上，纯度达99.9％；CO2浓度达到96％以上，离利用率在18％以上，其余作为循环气与原料混合，重新进入反应器利用。An energy-saving separation process for refining dimethyl ether and simultaneously recovering carbon dioxide, which consists of three parts: an absorption separation unit, a rectification separation unit and a waste heat recovery refrigeration unit. In the absorption separation unit, DME and CO 2 are recovered from the tail gas of the reaction product using a suitable solvent. In the rectification separation unit, the first rectification tower separates high-purity CO 2 , and the second rectification tower separates high-purity DME. The waste heat recovery refrigeration unit is composed of waste heat recoverers for the extracts from the above two rectification towers and the ammonia absorption refrigeration unit, in order to realize the use of the waste heat rejected by the system to drive the ammonia absorption refrigeration cycle to generate cooling capacity, which is used as the first A rectification tower overhead condensation load. The DME recovery rate of the reaction product gas by the process of the present invention can reach more than 99%, and the purity can reach 99.9%; the CO2 concentration can reach more than 96%, and the gas utilization rate can be more than 18%. use.
Description
Technical field
The present invention relates to a kind of method of producing dme (DME), relate in particular to a kind of carbonic acid gas (CO that reclaims when directly producing dme by synthetic gas
2) separating technology.
Background technology
U.S. DOE/PC/90018-T7 has proposed the technology of methanol dewatered DME, and this technical process is made of reactor R, methanol-water separator S1, noncondensable gas separator S2 and CO2-DME separator S3 as shown in Figure 1.The reaction product gas that contains DME leaves after the reactor R, and through the first separator S1 condensation, the first alcohol and water separates from the S1 bottom with the form of liquid phase; Through the further condensation of the second separator S2, unreacting gas CO and H
2Separated, DME and CO
2Form with liquid phase enters the 3rd separator S3; CO
2Finish at S3 with separating finally of DME.
Among the German Patent 4 222 655 disclosed DME preparation methods,,, use the methanol wash gas stream by a gas cleaning unit in order from the recycle gas of high-pressure separator, to isolate DME.Subsequently, wash DME and the CO that underflow contains
2Flow again with product and to combine from the highly pressurised liquid separator.In second washing device, then with methyl alcohol or water washing bonded product stream, so that from product, remove CO
2At last, make the washed product of the DME that contains basic equivalent and methyl alcohol some rectification step of flowing through, obtain highly purified DME product.
Synthetic method based on DME, NKK Corp (NKK) is at Japanese Patent: the spy opens flat 10-182 532, spy and opens that flat 10-182 533, spy open flat 10-182534, the spy opens among flat 10-182535 and the flat 11-152 241 of Te Kai, has proposed the preparation technology of DME.Synthetic, the CO that comprise DME
2And the recovery of unreacting gas, adopt cold energy of liquefied natural gas to utilize technology etc.Its basic procedure is illustrated in Fig. 2.R1 among the figure is a conversion reactor, and R2 is the DME synthesis reactor.As can be seen, its DME separating technology is identical with the U.S. DOE report of above-mentioned Fig. 1 substantially.Its major portion has been applied for Chinese patent (patent No. CN 1 169 888).
Dalian Inst of Chemicophysics, Chinese Academy of Sciences discloses preparation and the separation method of DME in Chinese patent CN 1 215 716A.This patent proposes, synthetic gas is after the DME synthesis reactor is reacted, product gas is through interchanger and the heat exchange of unstripped gas synthetic gas, go out liquid (be mainly and generate water) in gas-liquid separator separates, remove methyl alcohol on the absorption tower, the product D ME in the reaction end gas in extraction tower by under the solution extraction, the compressed machine supercharging of unreacted material synthesis gas with enter reactor again after fresh synthesis gas mixes, the DME that is extracted enters desorb-separation column with solvent and carries out desorb, and further carries dense.The solvent cooling that removes DME is after pump is returned the extraction tower recycle.Carry dense DME product and after water cooler condensation and compressor compresses, send into steel cylinder.
Denmark many Tops of Hall plucked instrument (Topsoe) company is called in name respectively among the international monopoly WO 96,/23 755 and Chinese patent CN 1 172 468A of " preparation method of fuel-grade DME ", has illustrated from the method for the synthesis gas preparation fuel-grade DME that contains hydrogen and oxycarbide.In one or more catalyticreactor, in methyl alcohol is synthetic and in the methanol dehydration, all have in the presence of the active catalyzer, synthetic gas is changed into the hybrid technique gas of DME, first alcohol and water.Cooling mixing process gas, the liquid process that obtains containing methyl alcohol, DME and water mutually, and the gaseous state technology that contains the DME that unconverted synthesis gas and part make is mutually.This patented method comprises the other step of separating gas phase and liquid phase, make liquid phase first water distilling apparatus of process and distill out the top product that contains DME and methyl alcohol and also discharge the bottom product stream that contains the first alcohol and water, make bottoms stream through second water distilling apparatus and distill out the logistics that contains methyl alcohol, this methyl alcohol is changed in the cleaning washing device, in cleaning washing device, mutually and from device, discharge the scrub stream of DME and methyl alcohol with methanol wash gaseous state technology.In catalytic and dehydration reaction,, the part methanol conversion in the scrub stream is become DME and water by contacting with dehydration catalyst.From dehydration reactor, discharge the product stream of DME, water and unconverted methyl alcohol and make and combine, obtain flowing of fuel-grade DME in conjunction with product with product stream from dehydration reactor from the top product of first water distilling apparatus.This technical process only can be reclaimed about 73% DME.
Summary of the invention
The object of the present invention is to provide a kind of refining dimethyl ether to reclaim the energy saving separation technology of carbonic acid gas simultaneously, promptly directly produce the technology that dme reclaims carbonic acid gas simultaneously by synthetic gas, this technology is isolated highly purified DME with the very high rate of recovery, the simultaneously separable CO that goes out higher degree
2, and whole technology has higher energy utilization efficiency.
For achieving the above object, technical process of the present invention is made up of three parts: absorption extraction unit, rectifying separation unit and waste heat recovery refrigeration unit.
In the absorption extraction unit, reaction product absorbs through absorption agent, isolates purpose product D ME and by product CO
2,, from absorption product, obtain purity and be higher than 99% DME and purity and be higher than 96% CO again through the rectifying separation unit
2
Specifically, from the reaction product gas of DME synthesis reactor, mainly contain H
2, CO, CO
2, N
2, CH
4With the DME of 11%～15% (quality %), with 45t.h
-1～55t.h
-1Mass flow rate enter the absorption tower, under 20 ℃～50 ℃, the operational condition of 1.0MPa～3.0MPa, make absorption agent with water, methyl alcohol or ethanol, the H in the reaction gas
2, CO, N
2And CH
4And most of CO
2Separate from overhead stream with the gas phase form.And DME, CO
2With small amount of methanol, H
2, N
2With CO by solvent absorbing, be sent to rectification cell.
Rectification cell comprises two rectifying tower.First rectifying tower is at working pressure 1.0MPa～3.0MPa, tower top temperature-30 ℃～-24 ℃, and 160 ℃～200 ℃ of tower still temperature, reflux ratio is 0.9～1.3 time, cat head is isolated CO
2Concentration can reach more than 96% (the quality %) H wherein
2, N
2With the content of CO be about 5% (quality %).DME, H
2O and small amount of methanol flow out from the tower still, after first waste-heat recoverer (or water cooler) cooling, enter second rectifying tower; At working pressure is 0.4MPa～1.5MPa, and tower top temperature is 20 ℃～50 ℃, and tower still temperature is 140 ℃～180 ℃, reflux ratio is 0.9～2.5 time, the second rectifying tower cat head is isolated liquid phase DME, and mass concentration reaches 99.9%, and the rate of recovery of DME reaches more than 99%.The absorption agent that contains Trace Methanol flows out from the tower still, after second waste-heat recoverer (or water cooler) cooling, for the absorption tower recycle.The heat that first waste-heat recoverer and second waste-heat recoverer are obtained is sent to the ammonia absorption type refrigeration unit, for first rectifying tower provides cold.
Above-mentioned absorption agent can also be the mixture of water-methanol or water-ethanol.
The pressure of described first rectifying tower is 1.5MPa～2.0MPa, tower top temperature-20 ℃～-30 ℃, 180 ℃～200 ℃ of tower still temperature.
The pressure of described second rectifying tower is 0.5MPa～0.7MPa, 20 ℃～30 ℃ of tower top temperatures, 140 ℃～160 ℃ of tower still temperature.
Described refrigeration unit is the ammonia absorption type refrigeration unit.
Description of drawings
Fig. 1 is the process flow diagram of methanol dewatered DME in the background technology.
Fig. 2 is the DME separation process scheme synoptic diagram of Japanese NKK in the background technology.
Fig. 3 is a process flow diagram of the present invention.
Embodiment
Also in conjunction with the accompanying drawings content of the present invention is done nearly detailed explanation of a step below by embodiment.
Embodiment 1: the separating technology of making absorption agent with water
Technical process with reference to Fig. 3 is described, and the product (thing stream number 1) from the DME synthesis reactor mainly contains H
2, CO, CO
2, N
2, CH
4With the DME of 14.4% (quality %),, enter the absorption tower of absorptive unit through reducing valve with the mass flow rate of 51.865t/h.Under 25 ℃, the operational condition of 2.5MPa, make absorption agent with water, the H in the reaction gas
2, CO, N
2, CH
4And most of CO
2Separate (thing stream number 9) with the gas phase form from cat head.And DME, CO
2Absorbed (thing stream number 2) with small amount of methanol by water, be sent to rectification cell.
First rectifying tower is at working pressure 18bar, tower top temperature-25.5 ℃, and 191 ℃ of tower still temperature, reflux ratio is 1.1 times, isolates CO from cat head
2(thing stream number 4), concentration reach 95.9% (quality %), H
2, N
2, CO total content be 4.1% (quality %).DME, H
2O and small amount of methanol after the water cooler cooling, enter second rectifying tower (thing stream number 5) from the extraction of tower still (thing stream number 3).At working pressure is 0.72MPa, and tower top temperature is 21 ℃, and tower still temperature is 153 ℃, under the condition of reflux ratio 1.1, isolates DME (thing stream number 6) from the second rectifying tower cat head, and mass concentration reaches 99.9%.The water that contains Trace Methanol is from tower still (thing stream number 7) extraction, after the water cooler cooling, for absorption tower recycle (thing stream number 8).
The heat that two waste-heat recoverers of waste heat recovery refrigeration unit are discharged first rectifying tower and the second rectifying Tata still production (can stream number 10,11) is sent to ammonia absorption type refrigeration unit refrigeration, for first rectifying tower provides cold (can stream number 12).
The result as shown in Table 1 and Table 2.The DME rate of recovery of this technology is 99.79%, CO
2The rate of recovery is 14.37%.DME and CO
2Concentration can reach 99.9% and 95.9% (quality %) respectively.Two rectifying tower stills of this technology steam-heated cal(l)andria load is about 32.285MW, and the cold of first rectifying tower top (25 ℃ of following temperature) load is about 0.520MW.Press the conversion factor of 1kW steam 0.18kg standard coal/h and 1kW cold 0.19kg standard coal/h and calculate, the separation unit consumption of every kg product DME is the 0.788kg standard coal.Based on the carbon content in the unstripped gas, 72% (mole) is converted into product DME, and 18% (mole) is converted into the CO2 of by-product, and 10% (mole) leaves this separation system and enter the circulation gas logistics.Table 1 is made logistics balance (embodiment 1) the thing stream number unstripped gas 1234679 mass flow rates/th of the separating technology of absorption agent with water
-17.991 51.865 123.072 119.512 3.560 7.500 112.012 39.384 composition/w%:H
213.2 21.7 00 0.7 00 28.5
N
2?????3.1?????10.1?????0.1???????0?????????2.2?????0???????0?????????13.1
CO??????76.2????5.5??????0.0???????0?????????1.2?????0???????0?????????7.1
CO
2????7.4?????45.3?????2.8???????0?????????95.9????0???????0?????????50.9
First 0 0.1 0.0 0 0.0 00 0.0
Alcohol
H
2O????0???????2.8??????90.9??????93.7??????0.0?????0.0?????99.9??????0.3
DME 0 14.5 6.1 6.3 0.0 99.5 00 tables 2 are done the energy consumption and the waste heat recovery (embodiment 1) of the separating technology of absorption agent with water
| Project | Load MW | ||
| Public utility | Steam load | The first rectifying Tata still | 23.132 |
| The second rectifying Tata still | 9.153 | ||
| Low temperature cold load | The first rectifying tower cat head | 0.520 | |
| The water coolant load | The second rectifying tower cat head | 1.801 | |
| The waste heat discharging | The first rectifying Tata reactor distillate water cooler | 15.193 | |
| The second rectifying Tata reactor distillate water cooler | 7.940 | ||
| By-product | 0 | ||
Embodiment 2: make absorption agent and the integrated separating technology of heat is arranged with ethanol
Technical process with reference to Fig. 1 is described, and the product (thing stream number 1) from the DME synthesis reactor mainly contains H
2, CO, CO
2, N
2, CH
4With the DME of 13.6% (quality %),, enter the absorption tower of absorptive unit with the mass flow rate of 51.865t/h.Under 25 ℃, the operational condition of 2.5MPa, make absorption agent with ethanol, the H in the reaction gas
2, CO, N
2, CH
4And most of CO
2Separate from cat head with the gas phase form.And DME, CO
2With small amount of methanol by solvent absorbing (thing stream number 2), be sent to rectification cell.
First rectifying tower is at working pressure 20bar, tower top temperature-25.5 ℃, and 170 ℃ of tower still temperature, reflux ratio is 1.3 times, isolates CO from cat head
2(thing stream number 4), purity reach 96.4% (quality %), H
2, N
2, CO total content be 3.9% (quality %).DME, H
2O and small amount of methanol after the cooling of first waste-heat recoverer, enter second rectifying tower from the extraction of tower still (thing stream number 3).At working pressure is 0.52MPa, and tower top temperature is 21 ℃, and tower still temperature is 126 ℃, under the condition of reflux ratio 2.5, isolates DME (thing stream number 6) from the second rectifying tower cat head, and purity reaches 99.9% (quality %).The water that contains Trace Methanol is from tower still (thing stream number 7) extraction, after the cooling of second waste-heat recoverer, for absorption tower recycle (thing stream number 8).
The heat that two waste-heat recoverers of waste heat recovery refrigeration unit are discharged first rectifying tower and the second rectifying Tata still production (can stream number 10,11) is sent to ammonia absorption type refrigeration unit refrigeration, for first rectifying tower provides cold (can stream number 12).
The result is shown in table 3 and table 4.The DME rate of recovery of this technology is 99.79%, CO
2The rate of recovery is 12.3%.DME and CO
2Concentration can reach 99.9% and 96.4% (quality %) respectively.Two rectifying tower stills of this technology steam load is about 24.372MW.Two waste-heat recoverers are distinguished recovery waste heat 3.697MW and 11.421MW, and the cold that produces-33 ℃ is about 3.780MW.Except the separation that can satisfy 0.403MW with the refrigeration duty, also exportable about 3.377MW temperature is about-33 ℃ cold.Conditions such as the industrial scale of this embodiment are substantially the same manner as Example 1, press the conversion factor of embodiment 1, and the separation unit consumption of the every kgDME of this embodiment is the 0.499kg standard coal, save 36.7% than embodiment 1.Based on the carbon content in the unstripped gas, 72% (mole) is converted into product DME, and 18% (mole) is converted into the CO2 of by-product, and 10% (mole) leaves this separation system and enter the circulation gas logistics.Table 3 is made absorption agent with ethanol and logistics balance (embodiment 2) the thing stream number unstripped gas 1234679 mass flow rates/th of the integrated separating technology of heat is arranged
-17.991 51.865 123.072 119.512 3.560 7.500 112.012 39.384 composition/w%:H
213.2 20.5 00 0.5 00 26.2
N
2?????3.1???????9.7??????0?????????0?????????2.0?????0???????0?????????12.3
CO??????76.2??????5.1??????0?????????0?????????1.1?????0???????0?????????6.5
CO
2????7.4???????47.3?????2.2???????0?????????96.4????0???????0?????????53.1
Methyl alcohol 0 0.1 000000
H
2O????0?????????2.4??????0?????????0.9???????0???????0???????1.0???????0
DME?????0?????????13.6?????5.1???????5.2???????0???????99.9????0?????????0
ETOH 0 1.3 91.7 93.8 0.0 0.0 99.0 1.8 tables 4 are made absorption agent with ethanol and the energy consumption and the waste heat recovery (embodiment 2) of the integrated separating technology of heat are arranged
| Project | Load MW | ||
| Public utility | Steam load | The first rectifying Tata still | 18.257 |
| The second rectifying Tata still | 6.115 | ||
| Low temperature cold load | The first rectifying tower cat head | 0.403 | |
| The water coolant load | The second rectifying tower cat head | 2.995 | |
| Waste heat recovery | The first rectifying Tata reactor distillate water cooler | 11.421 | |
| The second rectifying Tata reactor distillate water cooler | 3.697 | ||
| By-product cold (33 ℃) | 3.780 | ||
Claims (5)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02119856XA CN1190405C (en) | 2002-05-15 | 2002-05-15 | Energy saving separation technology of refining dimethyl ether and recovery carbon dioxide at the same time |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02119856XA CN1190405C (en) | 2002-05-15 | 2002-05-15 | Energy saving separation technology of refining dimethyl ether and recovery carbon dioxide at the same time |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1459442A true CN1459442A (en) | 2003-12-03 |
| CN1190405C CN1190405C (en) | 2005-02-23 |
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ID=29426899
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB02119856XA Expired - Fee Related CN1190405C (en) | 2002-05-15 | 2002-05-15 | Energy saving separation technology of refining dimethyl ether and recovery carbon dioxide at the same time |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101053815B (en) * | 2006-04-13 | 2010-08-11 | 杨国华 | Hot reflux tower for producing carbon-13 |
| CN101318651B (en) * | 2007-06-04 | 2012-06-20 | Posco公司 | Apparatus and method for recovering carbon dioxide from flue gas using ammonia water |
| CN103420397A (en) * | 2012-05-22 | 2013-12-04 | 亚申科技研发中心（上海）有限公司 | Separation and purification method for ammonia and dimethyl ether and system |
| CN105873660A (en) * | 2014-01-07 | 2016-08-17 | 林德股份公司 | Separation processing method for a product stream of a dimethyl ether reactor |
| CN105873661A (en) * | 2014-01-07 | 2016-08-17 | 林德股份公司 | Processing by a separation technique of a gas mixture formed from a product stream of a dimethyl reactor |
| CN109809963A (en) * | 2017-11-22 | 2019-05-28 | 林德股份公司 | The method and apparatus for obtaining dimethyl ether and carbon dioxide |
-
2002
- 2002-05-15 CN CNB02119856XA patent/CN1190405C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101053815B (en) * | 2006-04-13 | 2010-08-11 | 杨国华 | Hot reflux tower for producing carbon-13 |
| CN101318651B (en) * | 2007-06-04 | 2012-06-20 | Posco公司 | Apparatus and method for recovering carbon dioxide from flue gas using ammonia water |
| CN103420397A (en) * | 2012-05-22 | 2013-12-04 | 亚申科技研发中心（上海）有限公司 | Separation and purification method for ammonia and dimethyl ether and system |
| CN105873660A (en) * | 2014-01-07 | 2016-08-17 | 林德股份公司 | Separation processing method for a product stream of a dimethyl ether reactor |
| CN105873661A (en) * | 2014-01-07 | 2016-08-17 | 林德股份公司 | Processing by a separation technique of a gas mixture formed from a product stream of a dimethyl reactor |
| JP2017503802A (en) * | 2014-01-07 | 2017-02-02 | リンデ アクチエンゲゼルシャフトＬｉｎｄｅ Ａｋｔｉｅｎｇｅｓｅｌｌｓｃｈａｆｔ | Separation of product stream of dimethyl ether reactor |
| JP2017505224A (en) * | 2014-01-07 | 2017-02-16 | リンデ アクチエンゲゼルシャフトＬｉｎｄｅ Ａｋｔｉｅｎｇｅｓｅｌｌｓｃｈａｆｔ | Processing of gas mixtures formed from the product stream of a dimethyl reactor by separation techniques. |
| CN105873660B (en) * | 2014-01-07 | 2019-01-11 | 林德股份公司 | The method for separating and processing of product stream for dimethyl ether reactor |
| CN109809963A (en) * | 2017-11-22 | 2019-05-28 | 林德股份公司 | The method and apparatus for obtaining dimethyl ether and carbon dioxide |
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| Publication number | Publication date |
|---|---|
| CN1190405C (en) | 2005-02-23 |
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