CN101143807A - Method for producing dimethyl ether by separating heat tube type reactor - Google Patents

Method for producing dimethyl ether by separating heat tube type reactor Download PDF

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Publication number
CN101143807A
CN101143807A CNA2007100536305A CN200710053630A CN101143807A CN 101143807 A CN101143807 A CN 101143807A CN A2007100536305 A CNA2007100536305 A CN A2007100536305A CN 200710053630 A CN200710053630 A CN 200710053630A CN 101143807 A CN101143807 A CN 101143807A
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Prior art keywords
dimethyl ether
dme
methanol
gas
tube type
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CNA2007100536305A
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车维新
薛建设
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Wuhan Sanlian Energy-Saving Environmental Protection Engineering Coltd
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Wuhan Sanlian Energy-Saving Environmental Protection Engineering Coltd
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Abstract

The invention relates to method which utilizes a separate heat pipe type reactor to produce dimethyl ether. The method includes three steps; firstly, after being preheated, methanol material and the reclaimed material are evaporated in an evaporator and then enter into the separate heat pipe type reactor via a gas heat exchanger for catalytic dehydration reaction; secondly, the dehydrated gas ordinally passes through the gas heat exchanger, a methanol preheater and a crude dimethyl ether preheater and is condensed in a crude dimethyl ether condenser; thirdly, crude dimethyl ether is rectified in a tray column or a packed column, and a dimethyl ether product is collected from the top or the collection outlet on the lateral line of the upper part of a rectifying column. The invention ueses a simple methanol evaporator to replace a bulky and complex evaporation column, reaction can reach an optimal state because of the isothermal characteristic of the separate heat pipe type reactor, and the temperature of bed can be easily controlled; the invention sufficiently utilizes reaction heat to reduce the consumption of steam and cooling water; a modular cooling scrubber reclaims the dimethyl ether in the reclaimed incondensable gas, thus ensuring safety, energy saving, environmental protection and emission reduction; the content of the methanol in the residual liquid in a methanol distillation column can be less than or equal to 30PPm.

Description

A kind of method that adopts separating heat tube type reactor to produce dme
Technical field
The present invention relates to a kind of method that adopts separating heat tube type reactor to produce dme.
Background technology
Traditional methanol vapor phase method dewatering preparing dimethy ether adopts heat-insulating (ZL88101729.9), cold shock formula (ZL95113028.5) or cooling pipe type (ZL98113093.3) to produce dme, these three kinds of reactors all are difficult to move in the best condition, make the Dehydration of methanol effect just not reach the best, reaction conversion ratio is just low, and the heat energy consumption is also high.
Summary of the invention
The present invention is in order to overcome the deficiency that above-mentioned prior art exists; a kind of method that adopts separating heat tube type reactor to produce dme is provided; and separating heat tube type reactor makes Dehydration of methanol reach optimum regime; dimethyl ether production method of the present invention moves under lowest energy consumption; reasonable recovery in conjunction with tail gas; take into account safety, environment protection again, total Production Flow Chart is the shortest, that enterprise can obtain is energy-conservation, reduce discharging, effect cheaply.The recovery of dme is to adopt in the packing tower of two sections coolings, two sections washings to finish in the non-condensable gas, and this tower is fitted together with thick dme tank battery, does not contain dme in the discharging gas, and the methanol distillation column residual liquid discharge reaches and contains methyl alcohol≤30PPM.
A kind of method that adopts separating heat tube type reactor to produce dme, this method is to carry out methanol dehydration in 180-280 ℃ of temperature range under catalyst action, with dewatered product rectifying, specifically may further comprise the steps again:
(1) methyl alcohol of material benzenemethanol and recovery through after the preheating in vaporizer carburation by evaporation, enter the separating heat tube type dimethyl ether reactor through gas heat exchanger again, carry out catalytic and dehydration reaction;
(2) dehydration reaction gas is successively by gas heat exchanger, methanol evaporator and thick dme preheater, then condensation in thick dme condenser;
(3) thick dme rectifying in efficient tray column or packing tower, operating reflux ratio is 1: 0.3-3.0, from rectifying tower cat head or tower top side line extraction mouth extraction dme cat head or tower top side line extraction mouth extraction gas of dimethyl ether;
(4) gas of dimethyl ether gets the dme product through the rectifying tower condenser condenses.
Dme adopts two sections coolings, second wash towers to reclaim in the non-condensable gas in the rectifying tower condenser, does not contain dme in dropping a hint.
Pipe external pressure≤the 1.6MPa of separating heat tube type dimethyl ether reactor, pipe internal pressure≤1.0MPa, beds is the HZSM-5 type, its service temperature: 180-240 ℃.
Pipe external pressure≤the 1.6MPa of separating heat tube type dimethyl ether reactor, pipe internal pressure≤1.0MPa, beds is γ-Al 2O 3Type, its service temperature: 220-280 ℃.
Produce the fuel dimethyl ether product, its operating reflux ratio is 1: 0.3-0.8.Producing its operating reflux ratio of chemical dme product is 1: 0.8-3.0.
The recovery that contains dme in the non-condensable gas of dme is to carry out in the washing tower of two sections coolings, two sections washings, and washings adopts cold dilute methanol spray, contain the washing of dme, methyl alcohol, water after solution directly enter thick dme storage tank.
The rectifying tower bottoms can with build the methanol rectifying system coproduction, also can independent supporting methanol distillation column, this tower can be accepted thick methyl alcohol and dme rectifying still liquid simultaneously, and the methanol distillation column raffinate is reached contain methyl alcohol≤30PPM.
The present invention is with the vaporization tower of the huge complexity of simple methanol evaporator replacement, because the isothermal characteristics of separating heat tube type reactor can make reaction reach optimum regime, transformation efficiency can improve 5%, and bed temperature is easy to control; Make full use of the consumption that reaction heat reduces steam and water coolant, hear rate reduces 8%-%10, and emission gases does not contain dme.Knockdown cooling washing tower reclaims dme safety, energy-saving and environmental protection, the reduction of discharging in the non-condensable gas; In the supporting methanol recovery system raffinate methanol content can≤30PPm.
Description of drawings
Fig. 1 process flow diagram of the present invention.
Embodiment
The present invention is a kind of method that adopts the separate heat pipe reactor to make dme, as shown in Figure 1, raw material liq methyl alcohol by pipeline 1. after 2. methanol preheater shows the side preheating, 3. enter 4. carburation by evaporation of methanol evaporator by pipeline, gas methyl alcohol through pipeline 5. to gas heat exchanger 6., 7. transfer to the predetermined temperature in of reactor with the electric furnace that goes into operation when going into operation, 8. advance the separating heat tube type dimethyl ether reactor 9. by pipeline, reaction gas goes out to suck dme, unreacted methanol and water vapor, through 10. 6. shell-side of air inlet body interchanger of pipeline, heat exchange is after pipeline To methanol evaporator heating zone shell-side 4., insufficient section is by the steam reboiler Replenish, gas is then successively through pipeline after the heat exchange
Figure A20071005363000043
, thick dme preheater
Figure A20071005363000044
, pipeline
Figure A20071005363000045
, thick dme condenser
Figure A20071005363000046
, condensation thick dme, methyl alcohol, water mixture is through pipeline
Figure A20071005363000047
To thick dme storage tank Treat rectification process;
The conductive fluid that 9. reactor fills in the heat-exchanging tube bundle is subjected to the reaction heat vaporization through pipeline To 2. shell-side of methanol preheater, the heating methanol conductive fluid is condensed through pipeline
Figure A200710053630000410
, be back to reactor and 9. restrain the closed cycle of interior one-tenth;
Thick dme is successively through pipeline
Figure A200710053630000411
, the rectifying tower fresh feed pump
Figure A200710053630000412
, pipeline
Figure A200710053630000413
To thick dme preheater
Figure A200710053630000414
Preheating is after pipeline in the pipe
Figure A200710053630000415
To rectifying tower
Figure A200710053630000416
The middle part, dme steam is discharged through pipeline by cat head
Figure A200710053630000417
To the rectifying tower condenser
Figure A200710053630000418
, phlegma is by pipeline
Figure A200710053630000419
Flow into return tank
Figure A200710053630000420
, through pipeline
Figure A200710053630000421
, the dme reflux pump
Figure A200710053630000422
, pipeline
Figure A200710053630000423
Return to tower top and do backflow, the product dme is by pipeline
Figure A200710053630000424
Deliver to tank field dme storage tank.
Rectifying tower
Figure A200710053630000425
Heat requirement by the steam boiling device
Figure A200710053630000426
Provide, methanol plus water is then by pipeline in the still liquid
Figure A200710053630000427
Deliver to original methanol rectifying tower of factory or methanol distillation column, methyl alcohol is reached quality standards, make raw material with material benzenemethanol.Methanol concentration≤30PPm in the methanol distillation column raffinate (wt);
The rectifying tower condenser
Figure A200710053630000428
The non-condensable gas of discharging is through pipeline
Figure A200710053630000429
To washing tower , washings is by pipeline The dilute methanol liquid of the 35-45% concentration that cuts from methanol rectifying tower or methanol distillation column.Dme is recovered in the non-condensable gas, the non-condensable gas of contamination-free from cat head through pipeline
Figure A20071005363000051
Drain into atmosphere.Embodiment of the invention 1-6 is all by above-mentioned technical process operation.
Embodiment 1
Methanol feed rate 1500kg/m 3.h, separating heat tube type dimethyl ether reactor beds is the HZSM-5 type, and the working pressure pipe is outward 0.8MPa, is 0.7MPa in the pipe, 180 ℃~240 ℃ of temperature of reaction, transformation efficiency 80%; Dme rectifying tower stage number n=65 piece, operating reflux ratio is 1: 0.3, the purity that obtains dme is 99.5%.
Embodiment 2
Methanol feed rate 1500kg/m 3.h, separating heat tube type dimethyl ether reactor beds is the HZSM-5 type, and the working pressure pipe is outward 0.8MPa, is 0.7MPa in the pipe, 180 ℃~240 ℃ of temperature of reaction; Dme rectifying tower stage number n=65 piece, operating reflux ratio is 1: 3.0, the purity that obtains dme is 99.9%.
Embodiment 3
Methanol feed rate 800kg/m 3.h, separating heat tube type dimethyl ether reactor beds γ-Al 2O 3Type, working pressure pipe are outward 0.8MPa, are 0.8MPa in the pipe, 240 ℃~280 ℃ of temperature of reaction, transformation efficiency 80%.Dme rectifying tower stage number n=65 piece, operating reflux ratio is 1: 0.3, the purity that obtains dme is 99.5%.
Embodiment 4
Methanol feed rate 800kg/m 3.h, separating heat tube type dimethyl ether reactor beds γ-Al 2O 3Type, working pressure pipe are outward 0.8MPa, are 0.8MPa in the pipe, 240 ℃~280 ℃ of temperature of reaction, transformation efficiency 80%.Dme rectifying tower stage number n=65 piece, operating reflux ratio is 1: 3.0, the purity that obtains dme is 99.9%.
Embodiment 5
Methanol feed rate 1200kg/m 3.h, separating heat tube type dimethyl ether reactor beds ball-type γ-Al 2O 3Type, working pressure pipe are outward 0.8MPa, are 0.7MPa in the pipe, 260 ℃ of temperature of reaction, transformation efficiency 82%.Dme rectifying tower stage number n=65 piece, operating reflux ratio is 1: 0.8, the purity that obtains dme is 99.5%.
Embodiment 6
Methanol feed rate 1000kg/m 3.h, separating heat tube type dimethyl ether reactor beds ball-type γ-Al 2O 3Type, working pressure pipe are outward 0.8MPa, are 0.7MPa in the pipe, 260 ℃ of temperature of reaction, transformation efficiency 82%.Dme rectifying tower stage number n=65 piece, operating reflux ratio is 1: 3.0, the purity that obtains dme is 99.9%.

Claims (6)

1. with the method for methanol production dme, this method is to carry out methanol dehydration in 180-280 ℃ of temperature range under catalyst action, with dewatered product rectifying, specifically may further comprise the steps again:
(1) material benzenemethanol and the methyl alcohol that reclaims from the dme rectifying tower through after the preheating in vaporizer carburation by evaporation, enter the separating heat tube type dimethyl ether reactor through gas heat exchanger again, carry out catalytic and dehydration reaction;
(2) dehydration reaction gas is successively by gas heat exchanger, methanol evaporator and thick dme preheater, then condensation in thick dme condenser;
(3) thick dme rectifying in efficient tray column or packing tower, operating reflux ratio is 1: 0.3-3.0, from rectifying tower cat head or tower top side line extraction mouth extraction gas of dimethyl ether;
(4) gas of dimethyl ether gets the dme product through the rectifying tower condenser condenses.
2. method according to claim 1 is characterized in that: dme adopts two sections coolings, second wash towers to reclaim in the non-condensable gas in the rectifying tower condenser.
3. method according to claim 1 and 2 is characterized in that: the pipe external pressure≤1.6MPa of separating heat tube type dimethyl ether reactor, and pipe internal pressure≤1.0MPa, beds is the HZSM-5 type, its service temperature: 180-240 ℃.
4. method according to claim 1 and 2 is characterized in that: the pipe external pressure≤1.6MPa of separating heat tube type dimethyl ether reactor, and pipe internal pressure≤1.0MPa, beds is γ-AI 2O 3Type, its service temperature: 220-280 ℃.
5. method according to claim 1 and 2 is characterized in that: produce the fuel dimethyl ether product, its operating reflux ratio is 1: 0.3-0.8.
6. method according to claim 1 and 2 is characterized in that: producing its operating reflux ratio of chemical dme product is 1: 0.8-3.0.
CNA2007100536305A 2007-10-26 2007-10-26 Method for producing dimethyl ether by separating heat tube type reactor Pending CN101143807A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101880218A (en) * 2009-05-08 2010-11-10 上海吴泾化工有限公司 Dimethyl ether preparation technology by utilizing methanol dehydration and special equipment thereof
CN102728090A (en) * 2012-07-10 2012-10-17 东北制药集团股份有限公司 Fractional distillation equipment for separating propargyl alcohol and method of equipment
CN102766021A (en) * 2012-07-24 2012-11-07 唐山市冀东溶剂有限公司 Production system and production method for continuously producing ethanol by ethyl acetate through using hydrogenation

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101880218A (en) * 2009-05-08 2010-11-10 上海吴泾化工有限公司 Dimethyl ether preparation technology by utilizing methanol dehydration and special equipment thereof
CN101880218B (en) * 2009-05-08 2013-09-18 上海吴泾化工有限公司 Dimethyl ether preparation technology by utilizing methanol dehydration and special equipment thereof
CN102728090A (en) * 2012-07-10 2012-10-17 东北制药集团股份有限公司 Fractional distillation equipment for separating propargyl alcohol and method of equipment
CN102728090B (en) * 2012-07-10 2015-02-25 东北制药集团股份有限公司 Fractional distillation equipment for separating propargyl alcohol and method of equipment
CN102766021A (en) * 2012-07-24 2012-11-07 唐山市冀东溶剂有限公司 Production system and production method for continuously producing ethanol by ethyl acetate through using hydrogenation

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