CN101270034B - Technique for preparing dimethyl ether - Google Patents
Technique for preparing dimethyl ether Download PDFInfo
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- CN101270034B CN101270034B CN2008100549511A CN200810054951A CN101270034B CN 101270034 B CN101270034 B CN 101270034B CN 2008100549511 A CN2008100549511 A CN 2008100549511A CN 200810054951 A CN200810054951 A CN 200810054951A CN 101270034 B CN101270034 B CN 101270034B
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Abstract
The present invention provides a method used for producing dimethyl enther with methanol gas phase dehydration. In the method, a stripping tower and a heat exchanger are combined delicately so that the reaction heat that is recycled by the heat exchanger is completely used for vaporizing and concentrating the raw material of methanol; the particular recovery process of the methanol can control the differential pressure between a methanol recovery tower and an evaporative condenser when the methanol that can not react is recycled; the condensation heat of the methanol returning to the recovery tower of methanol is completely used for evaporating the raw material of the methanol; at the same time, the concentration of the crude methanol in the raw material and the recycled methanol that can not react can be effectively improved; the transformation ratio of the reaction is improved; the operating pressure higher than the traditional process, which can improve the processing capacity of the equipment on one hand, and increase the condensing temperature of the reaction products on the other hand; a heat recovery device can be used for changing the condensation waste heat into by-product steam. Thus the vapor consumption can be reduced from the current 1.4 to 1.5 tons to 0.85 ton to 1.1 tons; the consumption of circulating water can be reduced from 100 to 130 tons to from 50 to 90 tons; the by-product steam can reach to about 300 to 400Kg; thus the method greatly saves the energy and reduces the production cost.
Description
Technical field
The present invention relates to process for preparing dimethyl ether, relating in particular to a kind of is raw material with methyl alcohol, prepares the production technique of dme with the gas phase catalysis evaporation.
Technical background
Methanol industry is produced and is mainly taked gas-phase catalysis technology, as application number be 88101729.9 and application number be 95113028.5 promptly " to produce the method for pure Dimethyl ether ", included technological process in the disclosed production process of Chinese patent of " by the method for methanol production dme " etc.: material benzenemethanol is all sent into the methanol gas phase dehydration reactive system and is reacted after vaporizer or the heating of vaporization tower, the reaction product of coming out from the dehydration reaction system (contains the resultant of reaction dme, unreacted methanol, water etc.) send the dme rectifying tower to separate, obtain the dme product from dme rectifier or cat head; And the mixture of the components of getting rid of from the tower still such as first alcohol and water send methanol distillation column to carry out rectifying separation by self pressure, returns from the methyl alcohol of methanol distillation column recovered overhead again and does raw material, and discharge system from the water that Methanol Recovery Tata still obtains.One of characteristics of this method are to be provided with methanol distillation column, with the method for rectifying the mixture separation of components such as the methyl alcohol of dme rectifying tower and water is purified, methyl alcohol after the purification returns again does raw material, derives from the moisture that water in the material benzenemethanol and dehydration reaction produce and then discharges system from Methanol Recovery Tata still.Because the methyl alcohol that reclaims obtains from Methanol Recovery column overhead (evaporation back condensation), and needs certain reflux ratio, therefore need to consume a large amount of energy, and the methyl alcohol that reclaims is liquid phase, retrieval system is done raw material also needs the heating vaporization.Another characteristics of this method are the methyl alcohol (comprising the methyl alcohol that methanol distillation column reclaims) as raw material, no matter water content how much, all all vaporize at vaporizer or vaporization tower, moisture is wherein also all vaporized and is entered the gas-phase dehydration system, so not only increased the required heat energy of water vapor, and because water is dewatered product, moisture makes speed of response reduce after entering reactive system, has also reduced the equilibrium conversion of reaction simultaneously.Be that the related production process of 200410022020.5 disclosed " methods of methanol production dme " is as application number in addition: material benzenemethanol enters vaporization and carries the top of heating up in a steamer tower, from the first alcohol and water of dme rectifying tower is that main mixed solution is carried the middle part opening for feed that heats up in a steamer tower in vaporization and entered in the tower, directly entering vaporization with water vapor carries and heats up in a steamer the Tata still or carry the material that heats up in a steamer in the Tata still, the steam dereaction system response of cat head by reboiler indirect heating vaporization.The characteristics of this method are to be provided with to vaporize to carry to heat up in a steamer tower, this tower vaporization material benzenemethanol and the function that has the methyl alcohol in the recovery dme rectifying tower tower bottoms concurrently.Therefore because material benzenemethanol enters as phegma from cat head, the vaporization concentration of carrying the methanol steam that heats up in a steamer column overhead is subjected to the purity tolerances of material benzenemethanol.In addition, this method is all sent material benzenemethanol into vaporization rectifying tower top, and as the phegma of vaporization profit reduction and reserving tower recovery by the methyl alcohol in the dme rectifying tower tower bottoms, the amount of material benzenemethanol is considerably beyond the quantity of reflux that needs phegma.These enter vaporization and put forward the material benzenemethanol evaporation institute heat requirement that exceeds required quantity of reflux of heating up in a steamer tower and all provided by the steam of heating tower bottoms, need to consume a large amount of energy.
Summary of the invention
It is low to the invention provides a kind of energy consumption, reduced investment be the method for raw material production dme with methyl alcohol, to overcome the prior art drawback.
For realizing the object of the invention, its feature of this process for preparing dimethyl ether may further comprise the steps:
A. the liquid methanol raw material part after preheating is gone into gas stripping column, and the methanol steam of vaporization enters the dme reactive system, and Qi Hua methanol solution does not enter methanol distillation column middle and upper part inlet via the gas stripping column bottom;
B. another part liquid methanol raw material after preheating is gone into vaporizer-condenser and is partly vaporized, and the methanol steam of vaporization goes out the vaporizer-condenser top exit, and Qi Hua methanol solution is not gone into methanol distillation column middle and upper part inlet via the vaporizer-condenser outlet at bottom;
C. the methanol steam that goes out the methanol distillation column tower top outlet is divided into two-way, and one the tunnel enters the vaporizer-condenser condensation, and phlegma is gone into the top inlet of methanol distillation column; Another road methanol steam with enter heat exchanger after the methanol steam that goes out the vaporizer-condenser top exit in the b step mixes;
D. a part of methanol steam that goes out heat exchanger stimulates the menstrual flow and is mixed into the dme reactive system with another part methanol steam after gas stripping column gas is carried material benzenemethanol;
E. the dme mixed gas that contains that goes out the dme reactive system stimulates the menstrual flow heat exchanger heat exchange and reboiler respectively after preheating material methyl alcohol, the thick dme of preheating, water cooling, go into the rectifying of dme rectifying tower then, tower bottoms is gone into the methanol distillation column centre entrance via the tower bottom outlet, and the methanol distillation column tower bottoms drains into Sewage treatment systems.
When adopting the working pressure higher than traditional technology, dme mixed gas behind described stimulate the menstrual flow heat exchanger and the reboiler can be gone into waste heat recoverer earlier and be reclaimed heat with byproduct steam, goes into the rectifying of dme rectifying tower then after preheating material methyl alcohol, the thick dme of preheating, water-cooled.
The heating steam pressure of described methanol distillation column tower bottoms is 0.5～2.5MPa, and steam directly enters Methanol Recovery Tata still and heats wherein material, or adopts thermal source by reboiler indirect heating tower still material, and discharge from the tower still residual night.
Pressure in the described methanol distillation column is higher than the pressure of evaporation side in the vaporizer-condenser, the pressure reduction of control vaporizer-condenser and methanol distillation column, and the heat of condensation with the condensation of methanol distillation column cat head part methanol steam is used for the evaporation of part material methanol solution; The methanol solution of vaporization not in vaporizer-condenser is sent into the middle and upper part of methanol distillation column after the pressurization; The methyl alcohol of not vaporizing in gas stripping column enters the middle and upper part of methanol distillation column simultaneously; Also have the tower bottoms that comes by the dme rectifying tower to enter the middle part of methanol distillation column simultaneously, utilize in the vaporizer-condenser methanol solution of condensation to do backflow, the methanol solution that enters in the methanol distillation column material is proposed dense recovery.Tower tray or filler with separating power is set in the methanol distillation column.
The technical progress that the present invention obtains:
(1). have the gas stripping column that reclaims residual heat of reaction vaporization and purification material benzenemethanol dual function concurrently owing to adopt, what make effectively that heat exchanger reclaims is higher than into that the waste heat of reactive system temperature is used for the methanol feedstock evaporation, and the purity of the methanol vapor of evaporation is higher than material benzenemethanol, has played the effect of purification raw material.
(2). because the heat of condensation of Methanol Recovery column overhead methanol steam condensation all is used for the evaporation of methanol feedstock, the heat that provides at the bottom of the Methanol Recovery Tata all is used for the evaporation of methyl alcohol.Obviously, methanol distillation column reclaims the methyl alcohol in the dme tower bottoms and carries the dense not material benzenemethanol of vaporization, and the methanol steam that obtains has been saved the energy than under the high situation of other method purity than existing other technology.
(3) no matter. the purity of material benzenemethanol is how, because the methanol vapor concentration when methanol content always is higher than material benzenemethanol and all evaporates in the gas of gas stripping column and evaporator-condenser, the remaining methanol solution of gas stripping column and vaporizer-condenser a little less than material benzenemethanol concentration, enter into the middle and upper part of methanol distillation column, the methanol solution that utilizes condenser condenses is as phegma, carried the tower bottoms 23 of unevaporated methanol solution 10, vaporizer-condenser 2 remaining methanol solutions 14 and dme rectifying tower 7 in gas stripping column 3 dense; Go out the concentration of the methanol vapor of methanol distillation column, the amount of the steam output of material benzenemethanol adjusting methanol distillation column trim the top of column liquid 16 is controlled in the available vaporizer-condenser 2, make the concentration of the methanol steam of methanol distillation column 1 cat head be higher than the concentration of methanol feedstock methyl alcohol far away, thereby help improving the transformation efficiency of reaction.
(4). the hot mixed gas that utilizes out reactive system has reclaimed the waste heat of reactant to greatest extent through dme rectifying tower reboiler 6, heat exchanger 4 recovery waste heats in parallel.
(5). the present invention adopts the working pressure higher than traditional technology, can improve the device processes ability on the one hand, reduces the device total cost, and the reaction product condensing temperature is improved, and the waste heat recoverer of setting can be used for byproduct steam with the condensation waste heat.
(6). adopt technology ton product dme steam consumption of the present invention to be reduced to 0.85～1.1 ton by 1.4～1.5 tons of present traditional technology; Recirculated water consumption is reduced to 50～90 tons by 100～130 tons; But and byproduct steam 300～400Kg, saved the energy significantly, reduced production cost.
Description of drawings
Below in conjunction with accompanying drawing the present invention is further described.
Fig. 1 is a process flow diagram of the present invention.
Fig. 2 is the another embodiment of the present invention synoptic diagram.
Embodiment
Embodiment 1: as shown in Figure 1, present embodiment is not for having the flow process of waste heat recoverer.
A. the liquid methanol raw material part 9 after preheating is gone into gas stripping column 3 gas and is carried, and its temperature is 135 ℃, flow 304Kg/h, methanol content 93% (wt%), several 4 layers of gas stripping column 3 theoretical tower trays, working pressure 0.64MPA (G).The methanol steam of vaporization goes out gas stripping column 3 tops, and going out gas stripping column 3 overhead gas 26 temperature is 126.9 ℃, flow 1043Kg/h, methanol content 95.8% (wt%).Qi Hua methanol solution does not enter methanol distillation column 1 middle and upper part the 10th layer of tower tray that enter the mouth via gas stripping column 3 bottoms, goes out gas stripping column 3 lower liquid 10 flow 96Kg/h, methanol content 92% (wt%);
B. another part liquid methanol raw material 13 after preheating is gone in the pipe of vaporizer-condenser 2, its pressure 0.65MPA (G), temperature is 135 ℃, flow 1215Kg/h, methanol content 93% (wt%), the methanol steam 17 of vaporization goes out vaporizer-condenser 2 top exits, its flow is 617Kg/h, methanol content 95.1% (wt%), Qi Hua methanol solution 14 is not gone into methanol distillation column 1 middle and upper part the 10th tower tray that enter the mouth via vaporizer-condenser 2 outlet at bottoms, its flow 598Kg/h, methanol content 91% (wt%).
C. methanol distillation column 1 theoretical tower tray number is 40 layers, working pressure 0.8MPA (G), the methanol steam that goes out methanol distillation column 1 tower top outlet is divided into two-way, and one the tunnel 15 enters the shell side condensation of vaporizer-condenser 2, phlegma is gone into the top inlet the first layer tower tray of methanol distillation column 1, its flow 596Kg/h; Flow is that 1009Kg/h, methanol content are 97.3% (wt%); Another road methanol steam 18 with enter heat exchanger 4 after the methanol steam that goes out vaporizer-condenser 2 top exits in the b step mixes.
D. a part of methanol steam 11 that goes out heat exchanger 4 enters gas stripping column 3 lowest layer tower tray bottoms, its temperature is 251 ℃, flow 935Kg/h, gas mixes with another part methanol steam after carrying methyl alcohol, advance the temperature of the methanol steam 12 of reactive system 5 in order to adjusting, the temperature of the methanol steam 12 after the adjusting is 176 ℃, and flow is 1833Kg/h, goes into dme reactive system 5 then.
E. the dme mixed gas 20 that contains that goes out dme reactive system 5 temperature and be 305 ℃, flow and be 1833Kg/h stimulates the menstrual flow respectively after heat exchanger 4 heat exchange and reboiler 6 reclaim heats, after preheating material methyl alcohol, the thick dme of preheating, water-cooled, go into 7 rectifying of dme rectifying tower, tower bottoms 23 is gone into methanol distillation column 1 middle part the 15th tower tray from top to bottom via the tower bottom outlet, its flow 816Kg/h, methanol content 42.6% (wt%).Methanol distillation column 1 tower bottoms 24 drains into Sewage treatment systems, its flow 502Kg/h, methanol content 0.08% (wt%).
Embodiment 2: as shown in Figure 2, the present embodiment difference from Example 1 is:
A. the liquid methanol raw material part 9 after preheating is gone into gas stripping column 3, and its temperature is 165 ℃, flow 760Kg/h, methanol content 93% (wt%), several 4 layers of gas stripping column 3 theoretical tower trays, working pressure 1.34MPA (G).The methanol steam of vaporization goes out gas stripping column 3 tops, and going out gas stripping column 3 overhead gas 26 temperature is 153.1 ℃, flow 1374Kg/h, and, methanol content 95.4% (wt%).Qi Hua methanol solution does not enter methanol distillation column 1 middle and upper part the 10th layer of tower tray that enter the mouth via gas stripping column 3 bottoms, goes out gas stripping column 3 lower liquid 10 flow 467Kg/h, methanol content 91% (wt%);
B. another part liquid methanol raw material 13 after preheating is gone in the pipe of vaporizer-condenser 2, its pressure 1.35MPa (G), temperature is 153.3 ℃, flow 760Kg/h, methanol content 93% (wt%), the methanol steam 17 of vaporization goes out vaporizer-condenser 2 top exits, flow 383Kg/h, methanol content 95% (wt%), Qi Hua methanol solution 14 is not gone into methanol distillation column 1 middle and upper part the 10th tower tray that enter the mouth via vaporizer-condenser 2 outlet at bottoms, its flow 377Kg/h, methanol content 90% (wt%).
C. methanol distillation column 1 theoretical tower tray number is 40 layers, working pressure 1.6MPa (G), the methanol steam that goes out methanol distillation column 1 tower top outlet is divided into two-way, and one the tunnel 15 enters the shell side condensation of vaporizer-condenser 2, phlegma is gone into the top inlet the first layer tower tray of methanol distillation column 1, its flow 353Kg/h; Flow 1171Kg/h, methanol content are 95.3% (wt%); Another road methanol steam 18 with enter heat exchanger 4 after the methanol steam that goes out vaporizer-condenser 2 top exits in the b step mixes.
D. a part of methanol steam 11 that goes out heat exchanger 4 enters gas stripping column 3 lowest layer tower tray bottoms, its temperature is 266 ℃, flow 1081Kg/h, gas mixes with another part methanol steam after carrying methyl alcohol, advance the temperature of the methanol steam of reactive system 5 in order to adjusting, the temperature of regulating back methanol steam 12 is 183 ℃, and flow 1847Kg/h goes into dme reactive system 5 then.
E. the temperature that contains dme mixed gas 20 that goes out dme reactive system 5 is 305 ℃, its flow 1847Kg/h, this mixed gas heat exchanger 4 heat exchange and reboiler 6 that stimulate the menstrual flow respectively reclaims the tube side of going into waste heat recoverer 8 behind the heats and reclaims heat, temperature in is 180 ℃, temperature out is 140 ℃, 75 ℃ of hot water after preheating enter the shell side byproduct steam of waste heat recoverer 8, and vapor pressure is 0.2MPa (G), flow 382Kg/h.The dme mixed gas that goes out waste heat recoverer 8 is gone into 7 rectifying of dme rectifying tower after preheating material methyl alcohol, the thick dme of preheating, water-cooled, tower bottoms 23 is gone into methanol distillation column 1 middle part the 15th tower tray from top to bottom via the tower bottom outlet, its flow 830Kg/h, methanol content 42% (wt%).Discharge raffinate 24 at the bottom of methanol distillation column 1 tower continuously and drain into Sewage treatment systems, its flow 502Kg/h, methanol content 0.03% (wt%).
Claims (5)
1. process for preparing dimethyl ether, its feature may further comprise the steps:
A. the liquid starting material methyl alcohol part after preheating is gone into gas stripping column (3) gas and is carried, and the methanol steam of vaporization enters dme reactive system (5), and Qi Hua methanol solution does not enter methanol distillation column (1) middle and upper part inlet via gas stripping column (3) bottom;
B. another part liquid methanol raw material after preheating is gone into vaporizer-condenser (2), and the methanol steam of vaporization goes out vaporizer-condenser (2) top exit, and Qi Hua methanol solution is not gone into methanol distillation column (1) middle and upper part inlet via vaporizer-condenser (2) outlet at bottom;
C. the methanol steam that goes out methanol distillation column (1) tower top outlet is divided into two-way, and one the tunnel enters vaporizer-condenser (2) condensation, and phlegma is gone into the top inlet of methanol distillation column (1); Another road methanol steam with enter heat exchanger (4) after the methanol steam that goes out vaporizer-condenser (2) top exit in the b step mixes;
D. a part of methanol steam that goes out heat exchanger (4) stimulates the menstrual flow and is mixed into dme reactive system (5) with another part methanol steam after gas stripping column (3) gas is carried material benzenemethanol;
E. the dme mixed gas (20) that contains that goes out dme reactive system (5) stimulates the menstrual flow heat exchanger (4) heat exchange and reboiler (6) respectively after preheating material methyl alcohol, the thick dme of preheating, water cooling, go into dme rectifying tower (7) rectifying then, tower bottoms (23) is gone into methanol distillation column (1) centre entrance via the tower bottom outlet, and methanol distillation column (1) tower bottoms (24) drains into Sewage treatment systems.
2. process for preparing dimethyl ether according to claim 1, it is characterized in that the dme mixed gas behind described heat exchanger that stimulates the menstrual flow (4) and the reboiler (6) goes into waste heat recoverer (8), after preheating material methyl alcohol, the thick dme of preheating, water cooling, go into dme rectifying tower (7) rectifying then.
3. process for preparing dimethyl ether according to claim 1 and 2, the heating steam pressure that it is characterized in that described methanol distillation column tower bottoms is 0.5～2.5MPa.
4. process for preparing dimethyl ether according to claim 3 is characterized in that the pressure in the described methanol distillation column (1) is higher than the interior pressure of vaporizer-condenser (2).
5. process for preparing dimethyl ether according to claim 4 is characterized in that being provided with in the described methanol distillation column (1) tower tray or the filler with separating power.
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| CN2008100549511A CN101270034B (en) | 2008-05-12 | 2008-05-12 | Technique for preparing dimethyl ether |
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| CN2008100549511A CN101270034B (en) | 2008-05-12 | 2008-05-12 | Technique for preparing dimethyl ether |
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| CN101270034B true CN101270034B (en) | 2010-06-02 |
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| CN106866368B (en) * | 2017-01-20 | 2020-04-28 | 常州大学 | Gas field alcohol-containing sewage methanol recovery device and process based on gas stripping method and vacuum membrane distillation method |
| CN111285421A (en) * | 2020-01-16 | 2020-06-16 | 董国亮 | Methanol-to-olefin sewage stripping tower system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0270852A2 (en) * | 1986-11-18 | 1988-06-15 | RWE-DEA Aktiengesellschaft für Mineraloel und Chemie | Process for the preparation of pure dimethyl ether |
| CN1293029C (en) * | 2004-03-15 | 2007-01-03 | 四川天一科技股份有限公司 | Method for producing dimethyl ether from methanol |
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2008
- 2008-05-12 CN CN2008100549511A patent/CN101270034B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0270852A2 (en) * | 1986-11-18 | 1988-06-15 | RWE-DEA Aktiengesellschaft für Mineraloel und Chemie | Process for the preparation of pure dimethyl ether |
| CN1293029C (en) * | 2004-03-15 | 2007-01-03 | 四川天一科技股份有限公司 | Method for producing dimethyl ether from methanol |
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Assignee: Hebei Zhengyuan Yang Coal Chemical Group Co. Ltd. Assignor: Qian Jinhua|Liu Jincheng|Lin Meili Contract record no.: 2010130000048 Denomination of invention: Technique for preparing dimethyl ether Granted publication date: 20100602 License type: Exclusive License Open date: 20080924 Record date: 20100810 |
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Effective date of registration: 20180410 Address after: 050061 Xiang Wing Road, Xinhua District, Shijiazhuang, Hebei Province, No. 6 Patentee after: Hebei Zhengyuan Chemical Engineering Design Co. Ltd. Address before: 050091 Hebei Zhengyuan Investment Co., Ltd. 509, Cang an road, Shijiazhuang, Hebei Co-patentee before: Liu Jincheng Patentee before: Qian Jinhua Co-patentee before: Lin Meili |