CN103449980B - Dimethyl ether preparation method and device by methanol dehydration - Google Patents
Dimethyl ether preparation method and device by methanol dehydration Download PDFInfo
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- CN103449980B CN103449980B CN201310420981.0A CN201310420981A CN103449980B CN 103449980 B CN103449980 B CN 103449980B CN 201310420981 A CN201310420981 A CN 201310420981A CN 103449980 B CN103449980 B CN 103449980B
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Abstract
The invention relates to a method dimethyl ether preparation method by methanol dehydration. The method comprises the following steps of: after preheating methanol, dehydrating the preheated methanol under the action of catalyst and performing gas-liquid separation to the obtained reaction mixture; leading the obtained gas phase directly into a catalytic distillation column; also leading the obtained liquid phase into the catalytic distillation column after removing anions and cations therefrom; loading a solid ion exchange resin catalyst in a reaction zone of the catalytic distillation column and obtaining the qualified dimethyl ether product after condensing the distillate on the top of the catalytic distillation column; obtaining methanol-containing waste water on the bottom of the catalytic distillation column. The invention further relates to a special device of the method. The method has simple technological process; due to reaction of the methanol under the liquid phase state, the method has the advantages of low reaction temperature, high conversion ratio, good selectivity and low energy consumption; additionally, the method removes the caustic anions and cations via an ion exchanger so as to effectively solve corrosion problems of the liquid-phase method.
Description
Technical field
The present invention relates to a kind of production method of chemical products, be specifically related to a kind of method and device of dimethyl ether by methanol dehydration.
Background technology
Dme, also known as methyl ether, is called for short DME.Dme, as a kind of basic chemical raw materials, due to its good easy compression, condensation, vaporizing property, can be widely used in the fields such as industry, agricultural, medical treatment, daily life.Dme will be mainly used in alternative vehicle fuel, oil liquefied gas, town gas etc. future, and market outlook are very wide.
Methanol dehydration method adopts sulfuric acid process to dewater the earliest, and reaction is carried out in the liquid phase, and main drawback is that equipment corrosion is serious, operational condition severe, and environmental pollution is serious.The production method of current dme mainly contains: (1) adopts methanol gas phase dewatering preparing dimethy ether, advantage: dimethyl ether purity can reach 99.9%, shortcoming: Dehydration of methanol temperature is higher, also there are certain requirements the purity of methanol feedstock by general 200 ~ 380 DEG C; (2) simple employing catalytic distillation process preparing dimethy ether, advantage: Dehydration of methanol and product separation carry out simultaneously in a catalytic distillation tower, and shortcoming: stage number is more, facility investment is higher, and turndown ratio is less.
Summary of the invention
The object of the invention is to: method and device that a kind of dimethyl ether by methanol dehydration is provided, can simplification of flowsheet, reduce temperature of reaction and production energy consumption, the purity requirement to methanol feedstock can be reduced simultaneously, improve the per pass conversion of methyl alcohol, the turndown ratio of intensifier, the etching problem of effective solving device.
In order to achieve the above object, the present invention is by the following technical solutions:
A kind of method of methanol dehydration dimethyl ether-preparing is provided, comprises the following steps:
1) methyl alcohol is after preheating reaches 100 ~ 180 DEG C, under catalyst action, at the temperature of the pressure of 0.5 ~ 4.0MPa and 100 ~ 180 DEG C, there is dehydration reaction, obtain the reaction mixture be made up of the dme generated, water byproduct and unreacted methyl alcohol;
2) step 1) reaction mixture that obtains carries out gas-liquid separation at the temperature of the pressure of 0.5 ~ 2.0MPa and 100 ~ 180 DEG C, obtains gas phase and liquid phase;
3) step 2) gas phase that obtains directly enters catalytic distillation tower; Step 2) liquid phase that obtains also enters catalytic distillation tower after first removing anions and canons; Described catalytic distillation tower conversion zone is equipped with solid ion-exchange resin catalyzer, working pressure: 0.5 ~ 2.0MPa, tower top temperature: 40 ~ 80 DEG C, bottom temperature: 100 ~ 200 DEG C, reflux ratio: 0.5 ~ 10, air speed: 0.3 ~ 10h
-; Catalytic distillation tower overhead product obtains qualified dme product after condensation; Obtain at the bottom of catalytic distillation tower tower containing alcohol waste water.
Step 1) described in preheating, be that methyl alcohol has been come through heat exchanger unit and well heater successively in preferred scheme; Further in preferred scheme, described heat exchanger unit is made up of the interchanger of 2 series connection; In most preferred scheme, methyl alcohol enters First Heat Exchanger through feed-pipe, through First Heat Exchanger outlet pipe after heat exchange, temperature is 40 ~ 60 DEG C, enters the second interchanger and carries out heat exchange, through the second heat exchanger exit pipe, temperature is 60 ~ 80 DEG C, enter well heater again, methyl alcohol is through heater outlet pipe, and temperature reaches 100 ~ 180 DEG C.
Step 1) described in dehydration reaction preferably carry out at the temperature of the pressure of 1.2 ~ 2.5MPa and 120 ~ 150 DEG C.
Step 2) described in gas-liquid separation, preferably carry out at the temperature of the pressure of 0.8 ~ 1.5MPa and 120 ~ 150 DEG C.
Step 3) described in catalytic distillation tower operational condition preferred: pressure 1.0 ~ 1.5MPa, tower top temperature 50 ~ 60 DEG C, bottom temperature 150 ~ 200 DEG C, reflux ratio 0.5 ~ 5, air speed 0.5 ~ 1.0h
-.
In a kind of preferred scheme of the present invention, step 3) described in catalytic distillation tower tower at the bottom of obtain enter methanol distillation column containing alcohol waste water, methanol distillation column operational condition is: pressure is 0 ~ 0.1MPa, preferably 0 ~ 0.05MPa; Tower top temperature is 50 ~ 80 DEG C, preferably 60 ~ 75 DEG C; Bottom temperature is 90 ~ 120 DEG C, preferably 95 ~ 115 DEG C; Reflux ratio is 0.5 ~ 10, preferably 0.5 ~ 5.0; Methanol distillation column overhead product obtains methyl alcohol after condensation, returns step 1) recycle; Methanol distillation column tower reactor water returns step 1) for pre-hot methanol.
The present invention also provides the special purpose device of the method for described methanol dehydration dimethyl ether-preparing, which comprises at least interchanger, well heater, dehydration reactor, gas-liquid separator, ion-exchanger and catalytic distillation tower, described interchanger, well heater, dehydration reactor, connected by guiding device between gas-liquid separator and catalytic distillation tower, wherein, described heat exchanger exit is connected with calorifier inlets, described heater outlet is connected with dehydration reactor entrance, described dehydration reactor outlet is connected with gas-liquid separator entrance, described gas-liquid separator gaseous phase outlet is connected with catalytic distillation tower gas phase entrance, described gas-liquid separator liquid-phase outlet is connected with ion-exchanger through interchanger, described ion-exchanger outlet is connected with catalytic distillation tower liquid phase entrance.
In the preferred device of the present invention, described interchanger by First Heat Exchanger and the second interchanger in series; Described gas-liquid separator liquid-phase outlet is connected with ion-exchanger through the second interchanger.
In the further preferred device of the present invention, also comprise the methanol distillation column be connected with wastewater outlet at the bottom of described catalytic distillation tower tower, and described Methanol Recovery tower top is connected with described First Heat Exchanger methanol inlet, wastewater outlet at the bottom of methanol distillation column tower is connected with described First Heat Exchanger waterwater entrance.
The preferred device of the present invention further comprises the catalytic distillation tower condenser be connected with catalytic distillation tower tower top outlet, the catalytic distillation tower reboiler be connected with catalytic distillation tower tower bottom outlet, the methanol distillation column condenser be connected with methanol distillation column tower top outlet, the methanol distillation column reboiler that is connected with methanol distillation column tower bottom outlet.
In the most preferred scheme of the present invention, the special purpose device described in employing, be that raw material dehydration prepares dme with methyl alcohol, concrete grammar is as follows:
As shown in Figure 1, methyl alcohol enters First Heat Exchanger 2 through methanol feeding pipe 1, after heat exchange, methyl alcohol is through First Heat Exchanger outlet pipe 3, temperature is 40 ~ 60 DEG C, enter the second interchanger 4 and carry out heat exchange, methyl alcohol is through the second heat exchanger exit pipe 5, temperature is 60 ~ 80 DEG C, enter well heater 6, methyl alcohol is through heater outlet pipe 7, temperature is 120 ~ 150 DEG C, enter dehydration reactor 8, working pressure: 1.2 ~ 2.5MPa, service temperature: 120 ~ 150, under catalyst action, methanol dehydration generates dme mixture, the reaction mixture generated enters gas-liquid separator 10 through dehydration reactor outlet pipe 9, the working pressure of gas-liquid separator 10: 0.8 ~ 1.5MPa, service temperature: 120 ~ 150 DEG C, be separated the gas phase obtained and directly enter catalytic distillation tower 16 through gas-liquid separator gaseous phase outlet pipe 15, be separated the liquid phase obtained and enter the second interchanger 4 through gas-liquid separator liquid-phase outlet pipe 11, through the liquid phase of heat exchange again through the second interchanger liquid phase mixture outlet pipe 12, temperature is 60 ~ 95 DEG C, enter ion-exchanger 13, remove the moon, positively charged ion, then catalytic distillation tower 16 is entered through ion-exchanger outlet pipe 14, working pressure: 1.0 ~ 1.5MPa, tower top temperature: 50 ~ 60 DEG C, bottom temperature: 150 ~ 200 DEG C, reflux ratio: 0.5 ~ 5, air speed: 0.5 ~ 1.0h
-catalytic distillation tower conversion zone is equipped with solid ion-exchange resin catalyzer, methyl alcohol in reaction mixture reacts further and generates dme and byproduct of reaction water in catalytic distillation tower conversion zone, byproduct of reaction water and a small amount of unreacted methyl alcohol and product dme are through catalytic distillation tower separating-purifying, overhead product is after catalytic distillation tower condenser 17 condensation, obtain qualified dme product, be delivered to outside device through dme product pipe 18, under normal circumstances, can obtain qualified reaching direct emission request containing alcohol waste water at the bottom of catalytic distillation tower tower, tower reactor directly enters after First Heat Exchanger 2 recovery waste heat through catalytic distillation tower waste pipe 21 containing alcohol waste water, is delivered to outside device through wastewater outlet pipe 27, but sometimes due to the impact of start-stop car, fault in production and catalyzer catalyst activity in latter stage, waste water alcohol content can be caused to exceed standard, what catalytic distillation tower tower reactor exceeded standard enters methanol distillation column 22 through catalytic distillation tower to Methanol Recovery pipe 20 containing alcohol waste water, working pressure: 0 ~ 0.05MPa, tower top temperature: 60 ~ 75 DEG C, bottom temperature: 95 ~ 115 DEG C, reflux ratio: 0.5 ~ 5.0, overhead product is after methanol distillation column condenser 23 condensation, obtain qualified methyl alcohol, return methanol feeding pipe 1 through Methanol Recovery column overhead methanol outlet pipe 24 and recycle, methanol distillation column tower reactor water, through Methanol Recovery tower reactor bottom outlet pipe 26, after entering First Heat Exchanger 2 recovery waste heat, is delivered to outside device through wastewater outlet pipe 27.
The method of producing dimethyl ether by dehydrating methanol of the present invention, compared with the prior art, has the following advantages: (1) technical process is simple, and temperature of reaction is low, transformation efficiency is high, selectivity is good, energy consumption is low, reduced investment; (2) purity of device to material benzenemethanol is adaptable, can reduce the purchase cost of material benzenemethanol.(3) device turndown ratio is comparatively large, and in the purity of product dme and waste water, methanol content is convenient to control; (4) by ion-exchange removal, there is corrosive anions and canons, efficiently solve the etching problem of device.
Accompanying drawing explanation
Fig. 1 is the special purpose device schematic diagram of the methanol dehydration dimethyl ether-preparing of the embodiment of the present invention 1.
Fig. 2 is the special purpose device schematic diagram of the dimethyl ether by methanol dehydration of the embodiment of the present invention 2.
Number in the figure is described as follows:
1, methanol feeding pipe; 2, First Heat Exchanger; 3, First Heat Exchanger outlet pipe; 4, the second interchanger; 5, the second heat exchanger exit pipe; 6, well heater; 7, heater outlet pipe; 8, dehydration reactor; 9, dehydration reactor outlet pipe; 10, gas-liquid separator; 11, gas-liquid separator liquid-phase outlet pipe; 12, the second interchanger liquid phase mixture outlet pipe; 13, ion-exchanger; 14, ion-exchanger outlet pipe; 15, gas-liquid separator gaseous phase outlet pipe; 16, catalytic distillation tower; 17, catalytic distillation tower condenser; 18, dme product pipe; 19, catalytic distillation tower reboiler; 20, catalytic distillation tower is to Methanol Recovery pipe; 21, catalytic distillation tower waste pipe; 22, methanol distillation column; 23, methanol distillation column condenser; 24, Methanol Recovery column overhead methanol outlet pipe; 25, methanol distillation column reboiler; 26, Methanol Recovery tower reactor bottom outlet pipe; 27, the second interchanger wastewater outlet pipe.
Embodiment
Embodiment 1
A special purpose device for producing dimethyl ether by dehydrating methanol, as shown in Figure 1, is formed primarily of First Heat Exchanger 2, second interchanger 4, well heater 6, dehydration reactor 8, gas-liquid separator 10, ion-exchanger 13, catalytic distillation tower 16, methanol distillation column 22, wherein, First Heat Exchanger 2 entrance is connected with methanol feeding pipe 1, First Heat Exchanger 2 is connected with the second interchanger 4 entrance through First Heat Exchanger outlet pipe 3, second interchanger 4 exports and is connected with well heater 6 entrance through the second heat exchanger exit pipe 5, well heater 6 exports heater via outlet pipe 7 and is connected with dehydration reactor 8 entrance, dehydration reactor 8 exports and is connected with gas-liquid separator 10 entrance through dehydration reactor outlet pipe 9, gas-liquid separator 10 gaseous phase outlet is connected with catalytic distillation tower 16 gas phase entrance by gas-liquid separator gaseous phase outlet pipe 15, gas-liquid separator 10 liquid-phase outlet is connected with the second interchanger 4 liquid phase mixture entrance by gas-liquid separator liquid-phase outlet pipe 11, second interchanger 4 liquid phase mixture outlet is connected with ion-exchanger 13 entrance through the second interchanger liquid phase mixture outlet pipe 12, ion-exchanger 13 exports and is connected with catalytic distillation tower 16 liquid phase entrance through ion-exchanger outlet pipe 14, catalytic distillation tower 16 tower top connects catalytic distillation tower condenser 17, catalytic distillation tower condenser 17 exports and connects dme product pipe 18, catalytic distillation tower 16 tower reactor connects catalytic distillation tower reboiler 19, catalytic distillation tower tower bottom outlet is connected with First Heat Exchanger 2 waterwater entrance through catalytic distillation tower waste pipe 21.
Embodiment 2
A special purpose device for producing dimethyl ether by dehydrating methanol, as shown in Figure 2, on the device basic of embodiment 1, comprises methanol distillation column 22 further, and catalytic distillation tower is connected with methanol distillation column 22 entrance to Methanol Recovery pipe 20 by catalytic distillation tower; Methanol distillation column 20 tower top outlet connects methanol distillation column condenser 23, be connected with methanol feeding pipe 1 through Methanol Recovery column overhead methanol outlet pipe 24 again, the tower reactor of methanol distillation column 20 connects methanol distillation column reboiler 25, then is connected with the waterwater entrance of First Heat Exchanger 2 through Methanol Recovery tower reactor bottom outlet pipe 26.
Embodiment 3
As shown in Figure 2, content 99.5%(mass ratio) methyl alcohol 500kg/h, enter the special production apparatus of the dimethyl ether by methanol dehydration of embodiment 2 through methanol feeding pipe 1, Dehydration of methanol device 8 working pressure is 1.5 ~ 3.0MPa, service temperature is 140 ~ 150 DEG C, and air speed is 1h
-; Gas-liquid separator 10 working pressure is 0.8 ~ 1.3MPa, and service temperature is 120 ~ 130 DEG C; Ion-exchanger 13 service temperature is 80 ~ 85 DEG C; Catalytic distillation tower 16 working pressure is 1.0 ~ 1.2MPa, and tower top temperature is 50 ~ 60 DEG C, and bottom temperature is 150 ~ 200 DEG C, and reflux ratio is 0.5 ~ 2, and air speed is 1h
-; During device start-stop car, methanol distillation column 22 puts into operation; During normal driving, methanol distillation column 22 is stopped transport, methanol distillation column 22 working pressure is 0 ~ 0.1MPa, tower top temperature is 60 ~ 70 DEG C, bottom temperature is 100 ~ 120 DEG C, and reflux ratio is 0.5 ~ 5, after putting into operation, tower top can obtain the methyl alcohol that purity is greater than 99.5%, and tower reactor obtains the water that purity is greater than 99.9%.Finally obtain at catalytic distillation tower 16 tower top the dme that purity is greater than 99.9%, obtain in catalytic distillation tower 16 tower reactor the water that purity is greater than 99.9%.
Claims (2)
1. a method for methanol dehydration dimethyl ether-preparing, is characterized in that, comprises the following steps:
Methyl alcohol enters First Heat Exchanger (2) through methanol feeding pipe (1), after heat exchange, methyl alcohol is through First Heat Exchanger outlet pipe (3), temperature is 40 ~ 60 DEG C, enter the second interchanger (4) and carry out heat exchange, methyl alcohol is through the second heat exchanger exit pipe (5), temperature is 60 ~ 80 DEG C, enter well heater (6), methyl alcohol is through heater outlet pipe (7), temperature is 120 ~ 150 DEG C, enter dehydration reactor (8), working pressure: 1.2 ~ 2.5MPa, service temperature: 120 ~ 150 DEG C, under catalyst action, methanol dehydration generates dme mixture, the reaction mixture generated enters gas-liquid separator (10) through dehydration reactor outlet pipe (9), the working pressure of gas-liquid separator (10): 0.8 ~ 1.5MPa, service temperature: 120 ~ 150 DEG C, be separated the gas phase obtained and directly enter catalytic distillation tower (16) through gas-liquid separator gaseous phase outlet pipe (15), be separated the liquid phase obtained and enter the second interchanger (4) through gas-liquid separator liquid-phase outlet pipe (11), through the liquid phase of heat exchange again through the second interchanger liquid phase mixture outlet pipe (12), temperature is 60 ~ 95 DEG C, enter ion-exchanger (13), remove the moon, positively charged ion, then catalytic distillation tower (16) is entered through ion-exchanger outlet pipe (14), working pressure: 1.0 ~ 1.5MPa, tower top temperature: 50 ~ 60 DEG C, bottom temperature: 150 ~ 200 DEG C, reflux ratio: 0.5 ~ 5, air speed: 0.5 ~ 1.0h
-1catalytic distillation tower conversion zone is equipped with solid ion-exchange resin catalyzer, methyl alcohol in reaction mixture reacts further and generates dme and byproduct of reaction water in catalytic distillation tower conversion zone, a small amount of unreacted methyl alcohol and product dme are through catalytic distillation tower separating-purifying, overhead product is after catalytic distillation tower condenser (17) condensation, obtain qualified dme product, be delivered to outside device through dme product pipe (18), catalytic distillation tower (16) tower reactor enters methanol distillation column (22) through catalytic distillation tower to Methanol Recovery pipe (20) containing alcohol waste water, working pressure: 0 ~ 0.05MPa, tower top temperature: 60 ~ 75 DEG C, bottom temperature: 95 ~ 115 DEG C, reflux ratio: 0.5 ~ 5.0, overhead product is after methanol distillation column condenser (23) condensation, obtain qualified methyl alcohol, return methanol feeding pipe (1) through methanol distillation column (22) tower top methanol outlet pipe (24) and recycle, methanol distillation column (22) tower reactor water, through Methanol Recovery tower reactor bottom outlet pipe (26), after entering First Heat Exchanger (2) recovery waste heat, is delivered to outside device through wastewater outlet pipe (27).
2. the special purpose device of the method for methanol dehydration dimethyl ether-preparing according to claim 1, it comprises interchanger, well heater, dehydration reactor, gas-liquid separator, ion-exchanger and catalytic distillation tower, described interchanger, well heater, dehydration reactor, connected by guiding device between gas-liquid separator and catalytic distillation tower, wherein, described heat exchanger exit is connected with calorifier inlets, described heater outlet is connected with dehydration reactor entrance, described dehydration reactor outlet is connected with gas-liquid separator entrance, described gas-liquid separator gaseous phase outlet is connected with catalytic distillation tower gas phase entrance, described gas-liquid separator liquid-phase outlet is connected with ion-exchanger through interchanger, described ion-exchanger outlet is connected with catalytic distillation tower liquid phase entrance, described interchanger by First Heat Exchanger and the second interchanger in series, described gas-liquid separator liquid-phase outlet is connected with ion-exchanger through the second interchanger,
Described special purpose device also comprises the methanol distillation column be connected with wastewater outlet at the bottom of described catalytic distillation tower tower, and described Methanol Recovery tower top is connected with described First Heat Exchanger methanol inlet, wastewater outlet at the bottom of methanol distillation column tower is connected with described First Heat Exchanger waterwater entrance;
Described special purpose device further comprises the catalytic distillation tower condenser be connected with catalytic distillation tower tower top outlet, the catalytic distillation tower reboiler be connected with catalytic distillation tower tower bottom outlet, the methanol distillation column condenser be connected with methanol distillation column tower top outlet, the methanol distillation column reboiler that is connected with methanol distillation column tower bottom outlet.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093353A (en) * | 1991-10-04 | 1994-10-12 | Rwe-Dea矿物油化学有限公司 | The preparation method of dme |
| CN1299801A (en) * | 1999-12-13 | 2001-06-20 | 孙业茂 | Multiple-section water circulation resin process of preparing para-butanol |
| CN101434518A (en) * | 2008-12-15 | 2009-05-20 | 上海惠生化工工程有限公司 | Method for producing dimethyl ether with combined fixed bed reactor and catalytic distillation column |
| CN101891597A (en) * | 2010-07-05 | 2010-11-24 | 杨奇申 | Dimethyl ether production method with multi-stage reactions |
| CN102464575A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Method for preparing dimethyl ether by gas phase dehydration of industrial methanol |
-
2013
- 2013-09-16 CN CN201310420981.0A patent/CN103449980B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093353A (en) * | 1991-10-04 | 1994-10-12 | Rwe-Dea矿物油化学有限公司 | The preparation method of dme |
| CN1299801A (en) * | 1999-12-13 | 2001-06-20 | 孙业茂 | Multiple-section water circulation resin process of preparing para-butanol |
| CN101434518A (en) * | 2008-12-15 | 2009-05-20 | 上海惠生化工工程有限公司 | Method for producing dimethyl ether with combined fixed bed reactor and catalytic distillation column |
| CN101891597A (en) * | 2010-07-05 | 2010-11-24 | 杨奇申 | Dimethyl ether production method with multi-stage reactions |
| CN102464575A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Method for preparing dimethyl ether by gas phase dehydration of industrial methanol |
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