CN103880606B - A kind of processing method of Liquid Phase Methanol producing dimethyl ether by dehydrating - Google Patents
A kind of processing method of Liquid Phase Methanol producing dimethyl ether by dehydrating Download PDFInfo
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- CN103880606B CN103880606B CN201410163023.4A CN201410163023A CN103880606B CN 103880606 B CN103880606 B CN 103880606B CN 201410163023 A CN201410163023 A CN 201410163023A CN 103880606 B CN103880606 B CN 103880606B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/09—Preparation of ethers by dehydration of compounds containing hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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Abstract
The invention provides a kind of method of dimethyl ether by methanol dehydration, comprise the following steps: methyl alcohol first reaches 120 ~ 160 DEG C through heating again through two-stage heat exchange, then under catalyst action, dehydration generates the mixture of dme, first alcohol and water; The direct separating-purifying of dme mixture generated, obtains qualified dme product and contains alcohol process water; What obtain contains the direct separating-purifying of alcohol process water, obtains qualified methyl alcohol and qualified waste water; The qualified methyl alcohol obtained is heated to 120 ~ 160 DEG C, again carries out dehydration reaction, and the dme obtained and the mixture of water obtain qualified dme product and qualified waste water through separating-purifying again.Tool of the present invention has the following advantages: (1) technical process is simple, and equipment is few, saves floor space, invests little.(2) temperature of reaction is low, transformation efficiency is high, selectivity is good, low without side reaction, material consumption energy consumption.
Description
Technical field
The present invention relates to chemical production technical field, be specifically related to a kind of processing method of Liquid Phase Methanol producing dimethyl ether by dehydrating.
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) catalytic distillation process preparing dimethy ether is adopted, 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: a kind of method that dimethyl ether by methanol dehydration is provided, can simplification of flowsheet, reduce floor space, reduce investment; Reduce temperature of reaction, reduce energy and material consumption, improve transformation efficiency.
In order to achieve the above object, the present invention is by the following technical solutions:
A kind of method of dimethyl ether by methanol dehydration is provided, comprises the following steps:
1) methyl alcohol first reaches 120 ~ 160 DEG C through heating again through two-stage heat exchange, and then under catalyst action, dehydration generates the mixture of dme, first alcohol and water;
2) step 1) the direct separating-purifying of dme mixture that generates, obtain qualified dme product and containing alcohol process water;
3) step 2) obtain containing the direct separating-purifying of alcohol process water, obtain qualified methyl alcohol and qualified waste water;
4) step 3) the qualified methyl alcohol that obtains is heated to 120 ~ 160 DEG C, and again carry out dehydration reaction, the dme obtained and the mixture of water obtain qualified dme product and qualified waste water through separating-purifying again.
In preferred embodiments of the present invention, step 1) and 4) described in dehydration reaction carry out in two different Dehydration of methanol devices respectively, completely isolatedly between described two different dehydration reactors not to be connected.
In the further preferred a kind of scheme of the present invention, step 1) described in dehydration reaction carry out in Dehydration of methanol device, step 4) described in dehydration reaction carry out in recovery Dehydration of methanol device, described Dehydration of methanol device and described recovery Dehydration of methanol device are installed in turn according to overlying relation in same total tower, and are not completely isolatedly between the two connected.
In the further preferred scheme of the present invention, the working pressure of described Dehydration of methanol device and recovery Dehydration of methanol device is 0.5 ~ 4.0MPa, and service temperature is 120 ~ 160 DEG C, and air speed is 0.3 ~ 10h
-1; Further preferred operations pressure is 1.5 ~ 3.0MPa, and service temperature is 140 ~ 150 DEG C, and air speed is 0.5h
-1.
In another preferred scheme of the present invention, described dme rectifying tower and described methanol distillation column are installed in turn according to overlying relation in same total tower, and are connected by pipeline between the two.
In the further preferred scheme of the present invention, described dme rectifying tower working pressure is 0.5 ~ 1.5MPa, and tower top temperature is 40 ~ 60 DEG C, and bottom temperature is 100 ~ 200 DEG C, and reflux ratio is 0.5 ~ 10; Further preferred operations pressure is 0.8 ~ 1.2MPa, and tower top temperature is 40 ~ 50 DEG C, and bottom temperature is 150 ~ 200 DEG C, and reflux ratio is 0.5 ~ 1.
In the further preferred scheme of the present invention, described methanol distillation column working pressure is 0 ~ 0.1MPa, and tower top temperature is 50 ~ 80 DEG C, and bottom temperature is 90 ~ 120 DEG C, and reflux ratio is 0.5 ~ 10; Further preferred operations pressure is 0 ~ 0.1MPa, and tower top temperature is 60 ~ 70 DEG C, and bottom temperature is 100 ~ 120 DEG C, and reflux ratio is 0.5 ~ 1.
In preferred embodiments of the present invention, step 1) charging methyl alcohol before carrying out heat exchange, be introduced into methanol purification device remove impurity and there is corrosive zwitterion.
The most preferred scheme of the present invention, as shown in Figure 1, comprises the following steps:
Methyl alcohol enters methanol purification device 2 through methanol feeding pipe 1, after purification, methyl alcohol enters First Heat Exchanger 4 through First Heat Exchanger inlet pipe 3, after heat exchange through First Heat Exchanger outlet pipe 5 temperature be 40 ~ 60 DEG C, enter the second interchanger 6 and carry out heat exchange, methyl alcohol is 60 ~ 80 DEG C through the second heat exchanger exit pipe 7 temperature, enter methyl alcohol well heater 8, it is 120 ~ 160 DEG C through methyl alcohol heater outlet pipe 9 temperature, enter Dehydration of methanol device 10, working pressure: 0.5 ~ 4.0MPa, service temperature: 120 ~ 160 DEG C, under catalyst action, methanol dehydration generates dme mixture, the reaction mixture generated, dme rectifying tower 12 is directly entered through dme rectifying tower inlet pipe 11, working pressure: 0.5 ~ 1.5MPa, tower top temperature: 40 ~ 60 DEG C, bottom temperature: 100 ~ 200 DEG C, reflux ratio: 0.5 ~ 10, byproduct of reaction water, a small amount of unreacted methyl alcohol and product dme are through dme rectifying tower separating-purifying, overhead product enters after First Heat Exchanger 4 cooling through dme rectifying tower gaseous phase outlet pipe 13, dme condenser 15 is entered through dme condenser inlet pipe 14, qualified dme product is obtained after condensation, be delivered to outside device through dme product pipe 16, what obtain at the bottom of dme rectifying tower contains alcohol process water, to exist together with dme rectifying tower 12 a total tower and methanol distillation column 18 separating-purifying be positioned at below dme rectifying tower 12 is directly entered through dme rectifying tower technique water pipe 17, working pressure: 0 ~ 0.1MPa, tower top temperature: 50 ~ 80 DEG C, bottom temperature: 90 ~ 120 DEG C, reflux ratio: 0.5 ~ 10, overhead product enters methanol distillation column condenser 20 through methanol distillation column gaseous phase outlet pipe 19, qualified methyl alcohol is obtained after condensation, enter through methanol outlet pipe 21 after pressurization and reclaim methyl alcohol well heater 22, through reclaiming methyl alcohol heater outlet pipe 23, temperature is 120-160 DEG C, enter to exist together with Dehydration of methanol device 10 a total tower and the recovery Dehydration of methanol device 24 be in below Dehydration of methanol device 10, reaction mixture enters dme rectifying tower 12 through dme rectifying tower inlet pipe 11, the qualified waste water of tower reactor, through Methanol Recovery tower reactor bottom outlet pipe 25, after entering the second interchanger 6 recovery waste heat, is delivered to outside device through wastewater outlet pipe 26.
In another preferred version of the present invention, after methanol distillation column overhead condenser 20 product methyl alcohol through and methanol distillation column overhead condenser 20 before gas-phase methanol heat exchange reclaim heat after, then enter and reclaim methyl alcohol well heater 22.
The present invention has the following advantages compared with the prior art:
(1) processing method of the present invention can reduce production cost, particularly have employed Dehydration of methanol device in the present invention and reclaim Dehydration of methanol device " double tower is unified ", and the design of dme rectifying tower and methanol distillation column " double tower is unified ", make technical process simple, equipment is few, save floor space, invest little.
(2) processing method temperature of reaction of the present invention is low, transformation efficiency is high, selectivity good, low without side reaction, material consumption; Gasification is not needed directly to enter reactor reaction energy consumption after charging Methanol Recovery waste heat low.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of Liquid Phase Methanol producing dimethyl ether by dehydrating.
In Fig. 1: 1, methanol feeding pipe; 2, methanol purification device; 3, First Heat Exchanger inlet pipe; 4, First Heat Exchanger; 5, First Heat Exchanger outlet pipe; 6, the second interchanger; 7, the second heat exchanger exit pipe; 8, methyl alcohol well heater; 9, methyl alcohol heater outlet pipe; 10, Dehydration of methanol device; 11, dme rectifying tower inlet pipe; 12, dme rectifying tower; 13, dme rectifying tower gaseous phase outlet pipe; 14, dme condenser inlet pipe; 15, dme condenser; 16, dme product pipe; 17, dme rectifying tower technique water pipe; 18, methanol distillation column; 19, methanol distillation column gaseous phase outlet pipe; 20, methanol distillation column condenser; 21, methanol outlet pipe; 22, methyl alcohol well heater is reclaimed; 23, methyl alcohol heater outlet pipe is reclaimed; 24, Dehydration of methanol device is reclaimed; 25, Methanol Recovery tower reactor bottom outlet pipe; 26, wastewater outlet pipe.
Embodiment
Embodiment 1
Carry out the technique of producing dimethyl ether by dehydrating methanol with the device systems shown in Fig. 1 and technical process, concrete steps are as follows:
The methyl alcohol 500kg/h of content 99.5% (mass ratio), methanol purification device 2 is entered through methanol feeding pipe 1, after purification, methyl alcohol enters First Heat Exchanger 4 through First Heat Exchanger inlet pipe 3, after heat exchange through First Heat Exchanger outlet pipe 5 temperature be 40 ~ 60 DEG C, enter the second interchanger 6 and carry out heat exchange, methyl alcohol is 60 ~ 80 DEG C through the second heat exchanger exit pipe 7 temperature, enter methyl alcohol well heater 8, it is 140 ~ 150 DEG C through methyl alcohol heater outlet pipe 9 temperature, enter Dehydration of methanol device 10, working pressure is 1.5 ~ 3.0MPa, and service temperature is 140 ~ 150 DEG C, and air speed is 0.5h
-1, under catalyst action, methanol dehydration generates dme mixture, the reaction mixture generated, dme rectifying tower 12 is directly entered through dme rectifying tower inlet pipe 11, working pressure is 0.8 ~ 1.2MPa, tower top temperature is 40 ~ 50 DEG C, bottom temperature is 150 ~ 200 DEG C, reflux ratio is 0.5 ~ 1, byproduct of reaction water, a small amount of unreacted methyl alcohol and product dme are through dme rectifying tower separating-purifying, tower top obtains the dme that purity is greater than 99.5%, enter after First Heat Exchanger 4 cooling through dme rectifying tower gaseous phase outlet pipe 13, dme condenser 15 is entered through dme condenser inlet pipe 14, qualified dme product is obtained after condensation, be delivered to outside device through dme product pipe 16, what obtain at the bottom of dme rectifying tower contains alcohol process water, to exist together with dme rectifying tower 12 a total tower and methanol distillation column 18 separating-purifying be positioned at below dme rectifying tower 12 is directly entered through dme rectifying tower technique water pipe 17, working pressure is 0 ~ 0.1MPa, tower top temperature is 60 ~ 70 DEG C, bottom temperature is 100 ~ 120 DEG C, reflux ratio is 0.5 ~ 1, tower top can obtain the methyl alcohol that purity is greater than 99.5%, methanol distillation column 18 overhead product enters methanol distillation column condenser 20 through methanol distillation column gaseous phase outlet pipe 19, qualified methyl alcohol is obtained after condensation, enter through methanol outlet pipe 21 after pressurization and reclaim methyl alcohol well heater 22, through reclaiming methyl alcohol heater outlet pipe 23, temperature is 140-150 DEG C, enter to exist together with Dehydration of methanol device 10 a total tower and the recovery Dehydration of methanol device 24 be in below Dehydration of methanol device 10, reaction mixture enters dme rectifying tower 12 through dme rectifying tower inlet pipe 11, methanol distillation column 18 tower reactor obtains the water that purity is greater than 99.9%, through Methanol Recovery tower reactor bottom outlet pipe 25, after entering the second interchanger 6 recovery waste heat, is delivered to outside device through wastewater outlet pipe 26.
Claims (8)
1. a method for dimethyl ether by methanol dehydration, comprises the following steps:
1) methyl alcohol first reaches 120 ~ 160 DEG C through heating again through two-stage heat exchange, and then under catalyst action, dehydration generates the mixture of dme, first alcohol and water;
2) step 1) the direct separating-purifying of dme mixture that generates, obtain qualified dme product and containing alcohol process water;
3) step 2) obtain containing the direct separating-purifying of alcohol process water, obtain qualified methyl alcohol and qualified waste water;
4) step 3) the qualified methyl alcohol that obtains is heated to 120 ~ 160 DEG C, and again carry out dehydration reaction, the dme obtained and the mixture of water obtain qualified dme product and qualified waste water through separating-purifying again;
Above-mentioned steps specific operation process is:
Methyl alcohol enters methanol purification device (2) through methanol feeding pipe (1), after purification, methyl alcohol enters First Heat Exchanger (4) through First Heat Exchanger inlet pipe (3), after heat exchange through First Heat Exchanger outlet pipe (5) temperature be 40 ~ 60 DEG C, enter the second interchanger (6) and carry out heat exchange, methyl alcohol is 60 ~ 80 DEG C through the second heat exchanger exit pipe (7) temperature, enter methyl alcohol well heater (8), it is 120 ~ 160 DEG C through methyl alcohol heater outlet pipe (9) temperature, enter Dehydration of methanol device (10), working pressure: 0.5 ~ 4.0MPa, service temperature: 120 ~ 160 DEG C, under catalyst action, methanol dehydration generates dme mixture, the reaction mixture generated, dme rectifying tower (12) is directly entered through dme rectifying tower inlet pipe (11), working pressure: 0.5 ~ 1.5MPa, tower top temperature: 40 ~ 60 DEG C, bottom temperature: 100 ~ 200 DEG C, reflux ratio: 0.5 ~ 10, byproduct of reaction water, a small amount of unreacted methyl alcohol and product dme are through dme rectifying tower separating-purifying, overhead product enters after First Heat Exchanger (4) cooling through dme rectifying tower gaseous phase outlet pipe (13), dme condenser (15) is entered through dme condenser inlet pipe (14), qualified dme product is obtained after condensation, be delivered to outside device through dme product pipe (16), what obtain at the bottom of dme rectifying tower contains alcohol process water, methanol distillation column (18) separating-purifying is directly entered through dme rectifying tower technique water pipe (17), working pressure: 0 ~ 0.1MPa, tower top temperature: 50 ~ 80 DEG C, bottom temperature: 90 ~ 120 DEG C, reflux ratio: 0.5 ~ 10, overhead product enters methanol distillation column condenser (20) through methanol distillation column gaseous phase outlet pipe (19), qualified methyl alcohol is obtained after condensation, enter through methanol outlet pipe (21) after pressurization and reclaim methyl alcohol well heater (22), through reclaiming methyl alcohol heater outlet pipe (23), temperature is 120-160 DEG C, enter and reclaim Dehydration of methanol device (24), working pressure: 0.5 ~ 4.0MPa, service temperature: 120 ~ 160 DEG C, reaction mixture enters dme rectifying tower (12) through dme rectifying tower inlet pipe (11), the qualified waste water of tower reactor, through Methanol Recovery tower reactor bottom outlet pipe (25), after entering the second interchanger (6) recovery waste heat, is delivered to outside device through wastewater outlet pipe (26).
2. method according to claim 1, it is characterized in that: step 1) and 4) described in dehydration reaction carry out in two different Dehydration of methanol devices respectively, step 1) described in dehydration reaction carry out in Dehydration of methanol device, step 4) described in dehydration reaction carry out in recovery Dehydration of methanol device, described Dehydration of methanol device and described recovery Dehydration of methanol device are installed in turn according to overlying relation in same total tower, and are not completely isolatedly between the two connected.
3. method according to claim 2, is characterized in that: described Dehydration of methanol device and recovery Dehydration of methanol device working pressure are 0.5 ~ 4.0MPa, and service temperature is 120 ~ 160 DEG C, and air speed is 0.3-10h
-1.
4. method according to claim 3, is characterized in that: described Dehydration of methanol device and recovery Dehydration of methanol device working pressure are 1.5 ~ 3.0MPa, and service temperature is 140 ~ 150 DEG C, and air speed is 0.5h
-1.
5. method according to claim 1, is characterized in that: step 2) described in separating-purifying carry out in dme rectifying tower, step 3) described in separating-purifying carry out in methanol distillation column.
6. method according to claim 5, is characterized in that: described dme rectifying tower and described methanol distillation column are installed in turn according to overlying relation in same total tower, and are connected by pipeline between the two.
7. method according to claim 5, is characterized in that: described dme rectifying tower working pressure is 0.8 ~ 1.2MPa, and tower top temperature is 40 ~ 50 DEG C, and bottom temperature is 150 ~ 200 DEG C, and reflux ratio is 0.5 ~ 1.
8. method according to claim 5, is characterized in that: described methanol distillation column working pressure is 0 ~ 0.1MPa, and tower top temperature is 60 ~ 70 DEG C, and bottom temperature is 100 ~ 120 DEG C, and reflux ratio is 0.5 ~ 1.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5218003A (en) * | 1988-01-14 | 1993-06-08 | Air Products And Chemicals, Inc. | Liquid phase process for dimethyl ether synthesis |
| CN1923780A (en) * | 2006-08-18 | 2007-03-07 | 水煤浆气化及煤化工国家工程研究中心 | Method for preparing dimethyl ether by liquid phase compression |
| CN103435454A (en) * | 2013-09-16 | 2013-12-11 | 凯瑞化工股份有限公司 | Method for preparing dimethyl ether through methanol dehydration |
-
2014
- 2014-04-22 CN CN201410163023.4A patent/CN103880606B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5218003A (en) * | 1988-01-14 | 1993-06-08 | Air Products And Chemicals, Inc. | Liquid phase process for dimethyl ether synthesis |
| CN1923780A (en) * | 2006-08-18 | 2007-03-07 | 水煤浆气化及煤化工国家工程研究中心 | Method for preparing dimethyl ether by liquid phase compression |
| CN103435454A (en) * | 2013-09-16 | 2013-12-11 | 凯瑞化工股份有限公司 | Method for preparing dimethyl ether through methanol dehydration |
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