CN106316800A - Method for low energy consumption preparation of dimethyl ether from methanol - Google Patents
Method for low energy consumption preparation of dimethyl ether from methanol Download PDFInfo
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- CN106316800A CN106316800A CN201510344638.1A CN201510344638A CN106316800A CN 106316800 A CN106316800 A CN 106316800A CN 201510344638 A CN201510344638 A CN 201510344638A CN 106316800 A CN106316800 A CN 106316800A
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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
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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 relates to a method for low energy consumption preparation of dimethyl ether from methanol, and belongs to the field of chemical engineering. The method comprises the following steps: 1, methanol from a tank area undergoes two-stage preheating by a wastewater cooler and a methanol preheater; 2, the preheated methanol is vaporized by a vaporizing tower, the vaporized methanol enters a reactor, reaction gas obtained after a reaction is divided into two flows, one of the two flows enters the methanol preheater, and the other flow enters one reboiler in the vaporizing tower; 3, the two reaction gas flows with the heat being partially used meet before entering a secondary methanol preheater, and exchange heat, and the obtained gas enters a rectifying tower from the bottom in a gas form; and 4, rectifying tower top dimethyl ether is cooled by an evaporative condenser, the cooled dimethyl ether enters a dimethyl ether refluxing tank, one part of the dimethyl ether is refluxed, and one part of the dimethyl ether is extracted as a product. Compared with the prior art, the method has the advantages of reasonable and full utilization of heat generated in the whole production system, saving of a large amount of process cooling water, optimized process route, reduction of the device investment, and suitableness for large-scale industrialization.
Description
Technical field
The present invention relates to a kind of low power consuming and made full use of system response heat by the method for preparing dimethyl ether from methanol, especially one, reduce external heat source supply, reduce a kind of low power consuming method of production cost, belong to chemical production technical field.
Background technology
At present, the main production process of dimethyl ether has one-step method from syngas, methanol method two kinds.And methanol method is divided into methanol vapor phase catalytic dehydration and liquid-phase catalysis evaporation.One-step method from syngas is in the industrialization exploratory stage, there is no industrialized report.Methanol vapor phase catalytic dehydration and methanol liquid phase catalytic dehydration the most all have industrial production device；And methanol vapor phase catalytic dehydration has, and investment is low, product adjustment is flexible, the simple feature of technique, but there is residual heat of reaction simultaneously and utilize insufficient, the shortcoming that energy consumption is higher.
Chinese patent literature (CN 102225889 A) discloses " a kind of by the method for dimethyl ether preparation by dehydrating methyl alcohol ", it is characterized in that: reactor uses three sections of thermal insulation intersegmental cold shock formula reactors, can control to leave reactor after product temperature reaches optimum temperature；Entering alcohol after the part light component condensed device cooling of dimethyl ether tower condenser overhead extraction and wash tower, by part Methanol Recovery dimethyl ether therein, gas is discharged at top.
Chinese patent literature (CN 200810045127X) discloses " a kind of low energy-consumption method for preparing dimethyl ether from methanol " and it is characterized in that: methanol is divided into two strands by the method, one methanol replaces process cooling water as cooling medium, the heat utilizing dimethyl ether distillation process cooling water to be taken away, makes first strand of methanol be preheated；Second strand of methanol enters in tower from the top of methanol compression rectification tower as cold reflux, under the effect of methanol reboiler, carries out heat exchange and changes into methanol steam；In the present invention, material benzenemethanol heats up through repeatedly heat exchange, make use of the heat arranging bottom water outside the heat of transformation and methanol compression rectification tower that gas phase dimethyl ether liquefies, but reaction gas waste heat not yet reaches the most sufficiently to utilize, the space that also can further improve in UTILIZATION OF VESIDUAL HEAT IN.
Summary of the invention
The purpose of the present invention is aiming at the deficiency of existing Technology, one is provided can whole dimethyl ether production system heat of reaction to be made full use of, reduce outer heating load, a kind of low power consuming method for preparing dimethyl ether from methanol that the cooling water circulation amount of whole system is greatly lowered can be made again.
Methanol gas phase dewatering preparing is that raw material heats, reacts, cools down and be then peeled off obtaining product dimethyl ether for the step that dimethyl ether is experienced, the technology of the most whole production system most critical exactly in heating and cooling procedure energy how to obtain optimal utilization.The present invention prepares dimethyl ether reaction mechanism, and heat characteristic distributions according to methanol vapor phase catalysis.Utilizing reaction heat to provide heat to vaporization tower, rectifying column uses gas-phase feed at the bottom of tower, and rectifying column tower top uses Novel evaporative condenser cooling product.Taking the above measure can be all of residual heat of reaction, dimethyl ether rectifying column and methyl alcohol vaporizing tower be no longer necessary to outer supplying heat source, and cooling water system uses evaporative condenser simultaneously, and cooling water amount is greatly lowered, and can be greatly saved the energy and resource.
For achieving the above object, the technical solution used in the present invention is:
1. a low power consuming is by the method for preparing dimethyl ether from methanol, it is characterised in that described in following technological process:
(1) by gaseous effluent cooler (02), the methanol from tank field being carried out methanol one-level preheating after pump pressurizes, make full use of waste heat in waste water, then recycling reaction gas waste heat is after two grades of preheaters (03) of methanol carry out two-stage preheating, enters evaporation stage；
(2) after preheating, methanol enters reactor, reacted reaction edema caused by disorder of QI two strands after vaporization tower vaporizes, and one goes two grades of preheaters (03) of methanol, and one goes one of them reboiler of vaporization tower (05)；Another reboiler of vaporization tower (06) can be closed down after system stability after driving；
(3) methanol steam after gasification is to temperature 250-260 DEG C after gas heat exchanger (07), enters reactor from reactor head；Reactor outlet reaction gas temperature about 350-360 DEG C；Dividing two strands is that system provides heat, one is temperature about 250-255 DEG C after vaporization tower reboiler (05) heat exchange, one goes temperature about 180-185 DEG C after gas heat exchanger (07) heat exchange, two grades of preheaters (03) of methanol are gone with another stock after converging afterwards, being about 120-135 DEG C with temperature after heat exchange of methanol, the pure gas phase of dimethyl ether feeds from rectifier bottoms 2-8 block column plate；
(4) rectifying column tower top dimethyl ether steam enters dimethyl ether return tank after Novel evaporative condenser cools down, and part backflow, as product extraction after a part is the most qualified.
The technological process of the present invention includes following system: 1. methanol preheats and gasification system, 2. reaction gas heat utilization system, 3. dimethyl ether rectifying column feed system and product condenser system.
Wherein, described in step (2) from reactor reaction gas out, one goes vaporization tower reboiler to provide heat for vaporization tower, in startup procedure, tend to normal along with reaction, be gradually reduced another reboiler conduction oil consumption of vaporization tower, and be gradually increased reaction tolerance, until suitable heat conductive oil mass.
Wherein, reaction gas described in step (3) after a series of heat exchange, dimethyl ether in rectifier bottoms gas-phase feed, gradually stepping up along with feeding temperature in startup procedure, it is gradually reduced rectifying column reboiler conduction oil consumption, until heat is provided by feeding gas completely at the bottom of tower.
Wherein, described rectifying column tower top dimethyl ether steam directly enters dimethyl ether return tank after Novel evaporative condenser cools down, and the most qualified extraction of a part, a part refluxes.
Wherein, material benzenemethanol to 125-135 DEG C, enters gasification system through one-level preheating and wastewater heat exchange, two grades of preheatings and reaction gas heat exchange.
Wherein, can reduce fuel delivery for conduction oil reboiler outside vaporization tower after driving to stablize, partial heat is by reaction gas heat supply.
Wherein, dimethyl ether rectifying column is float-valve type, and theoretical cam curve is 40-80 block, operates pressure 0.8-1.8MPa, operates temperature 40-155 DEG C.
Wherein, dimethyl ether product feeds between 2-8 block plate from rectifier bottoms number, and the heat that when utilizing charging, material carries carries out rectification to product, can stop rectifying column reboiler conduction oil supply after driving to stablize.
Wherein, rectifying column product uses the evaporative condenser of heat exhaust 4000-8000Kw/h to cool down, and water consumption and power consumption are little, saves the energy.
Compared with prior art, the method have the advantages that
(1) present invention uses the mode of the pure gas-phase feed of tower bottom of rectifying tower dimethyl ether, it is to avoid in the charging of prior art gas-liquid dimethyl ether is cooled to the energy that liquid phase is consumed, saves a large amount of recirculated water；Use pure gas phase tower reactor feeding manner, the available charging self-contained heat of dimethyl ether, decrease the outer heating load of tower reactor, save great amount of cost.
(2) rectifying column uses dimethyl ether pure gas phase tower reactor feeding manner, and rectifying column operates pressure and stably all decreases, and temperature reduces about 3-8 DEG C, and pressure reduces about 0.1-0.2 MPa, and system operation is more stable, obvious technical effects.
(3) present invention uses device waste water and reaction gas to preheat material benzenemethanol, can be directly entered gasification system, and system warm-up is fully used.
(4) present invention uses partial reaction gas for providing thermal source at the bottom of vaporization tower tower, reduces outer heating load, adds the stability of vaporization tower operation, considerably reduce energy loss.
(5) rectifying column overhead product of the present invention uses evaporative condenser to carry out the cooling of product, water consumption power consumption can be greatly lowered, and saved the energy and resource.
Accompanying drawing explanation
Fig. 1 is that a kind of low power consuming of the present invention is by the method process flow diagram of preparing dimethyl ether from methanol.
In Fig. 1, the implication represented by labelling is respectively as follows: 01-material benzenemethanol storage tank, 02-methanol one-level preheater, two grades of preheaters of 03-methanol, 04-vaporization tower, 05-vaporization tower reboiler 1,06-vaporization tower reboiler 2,07-gas heat exchanger, 08-reactor, 09-rectifying column, 10-rectifying column reboiler, 11-evaporative condenser, 12-dimethyl ether return tank, 13-scrubbing tower.
In Fig. 1, material benzenemethanol utilizes waste water residual heat to carry out one-level heat exchange through 02, then 03 is gone to utilize reaction gas heat to carry out secondary heat exchange, methanol after heat exchange enters 04 and is vaporized, carrying out heat exchange with partial reaction gas (tolerance is adjustably controlled) after vaporization, the methanol superheated steam after heat exchange enters 08 and carries out gas-phase dehydration reaction.Reaction gas converges entering before 03 after 07,05, with 03 heat exchange after 2-7 block column plate charging bottom 09, tower top dimethyl ether product enters 12 after 11 coolings, and a part is as backflow, the most qualified rear extraction of a part.Wherein fixed gas can carry out washing and recycling wherein dimethyl ether by 13, and waste water processing station is gone in waste water extraction after 02 heat exchange.
Below by embodiment, the present invention is illustrated in more detail.
Detailed description of the invention
A kind of low power consuming of the present invention is provided by the detailed description of the invention of the method for preparing dimethyl ether from methanol, at this it should be noted that the enforcement of the present invention is not limited to following embodiment in conjunction with accompanying drawing.
Embodiment 1
As shown in Figure 1, choosing purity is 99%(wt) as charging methanol, through two-stage heat exchange gasification and the entrance reactor that heats up, at 300-350 DEG C, under pressure 0.78 MPa, carry out dehydration.Product is from rectifier bottoms gas-phase feed, utilize self-contained heat to realize dimethyl ether to separate with first alcohol and water, obtain mainly containing the mixture of methanol, water in tower reactor, liquid phase dimethyl ether is obtained and containing a small amount of dimethyl ether and the fixed gas of other light components, as product extraction after a liquid phase dimethyl ether part backflow part is the most qualified after the cooling of overhead product condensed device.Wherein fixed gas goes scrubbing tower to carry out the recovery of dimethyl ether, and scrubbing tower tower top contains the light component materials such as carbon dioxide and is vented through blow-down pipe.Wherein dimethyl ether rectifying column feed entrance point choose particularly critical, in the present invention, rectifying column is 65 pieces of theoretical cam curves, and dimethyl ether pure gas-phase feed position is from rectifier bottoms number between 2-8 block plate, and tower top pressure is at 0.7-0.75
MPa, temperature is 35-40 DEG C.Vaporization tower has 78 blocks of theoretical trays, and pressure is 0.80 MPa, and temperature is 135 DEG C.Scrubbing tower uses packed tower, has 17 blocks of column plates, and tower top pressure is 0.6 MPa.
Embodiment 2
By condition and the step of embodiment 1, keep vaporization tower, response system and scrubbing tower operating condition constant, change rectifying column dimethyl ether feed entrance point, the 2nd piece of plate charging from rectifier bottoms number, can be fully closed for conduction oil valve outside rectifying column reboiler, tower top pressure 0.7MPa, temperature is 35 DEG C, and dimethyl ether product purity is 99.8%.
Embodiment 3
By condition and the step of embodiment 1, keep vaporization tower, response system and scrubbing tower operating condition constant, change rectifying column dimethyl ether feed entrance point, the 4th piece of plate charging from rectifier bottoms number, / 5th apertures need to be opened for conduction oil valve outside rectifying column reboiler, tower top pressure 0.73 MPa, temperature is 38 DEG C, and dimethyl ether product purity is 99.9%.
Embodiment 4
By condition and the step of embodiment 1, keep vaporization tower, response system and scrubbing tower operating condition constant, change rectifying column dimethyl ether feed entrance point, the 8th piece of plate charging from rectifier bottoms number, 2/5ths apertures need to be opened for conduction oil valve outside rectifying column reboiler, tower top pressure 0.75 MPa, temperature is 40 DEG C, and dimethyl ether product purity is 99.9%.
Unit product production consumption to present preparing dimethyl ether from methanol technique with present invention process contrasts, and details see table:
Claims (4)
1. a low power consuming is by the method for preparing dimethyl ether from methanol, it is characterised in that described in following technological process:
(1) methanol from tank field is carried out methanol one-level preheating by gaseous effluent cooler (02) after pump pressurizes, makes full use of waste heat in waste water,
Then recycling reaction gas waste heat is after two grades of preheaters (03) of methanol carry out two-stage preheating, enters evaporation stage；
(2) after preheating, methanol enters reactor, reacted reaction edema caused by disorder of QI two strands after vaporization tower vaporizes, and one goes two grades of preheaters (03) of methanol,
One goes one of them reboiler of vaporization tower (05)；Another reboiler of vaporization tower (06) can be closed down after system stability after driving；
(3) methanol steam after gasification is to temperature 250-260 DEG C after gas heat exchanger (07), enters reactor from reactor head；Reactor
Outlet reaction gas temperature about 350-360 DEG C；Points two strands is that system provides heat, and after vaporization tower reboiler (05) heat exchange, temperature is about for one
250-255 DEG C, one goes temperature about 180-185 DEG C after gas heat exchanger (07) heat exchange, and rear and another stock goes two grades of preheaters (03) of methanol after converging,
Being about 120-135 DEG C with temperature after heat exchange of methanol, the pure gas phase of thick dimethyl ether feeds from rectifier bottoms 2-8 block column plate；
(4) rectifying column tower top dimethyl ether steam enters dimethyl ether return tank after Novel evaporative condenser cools down, and part backflow, a part is through inspection
Survey qualified after as product extraction.
A kind of low power consuming the most according to claim 1 is by the method for preparing dimethyl ether from methanol, it is characterised in that described in step (2) from reaction
Device reaction gas out one go vaporization tower reboiler to provide heat for vaporization tower, in startup procedure, tend to normal along with reaction, be gradually reduced vaporization
Another reboiler conduction oil consumption of tower, and it is gradually increased reaction tolerance, until suitable heat conductive oil mass.
A kind of low power consuming the most according to claim 1 is by the method for preparing dimethyl ether from methanol, it is characterised in that the reaction gas described in step (3)
After a series of heat exchange, dimethyl ether is in rectifier bottoms gas-phase feed, and in startup procedure, gradually stepping up along with feeding temperature, is gradually reduced rectification
Tower reboiler conduction oil consumption, until heat is provided by feeding gas completely at the bottom of tower.
A kind of low power consuming the most according to claim 1 is by the method for preparing dimethyl ether from methanol, it is characterised in that described rectifying column tower top dimethyl ether steams
Vapour directly cools down through Novel evaporative condenser, reaches the purpose of water-saving and electricity-saving, and effect is notable.
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| CN201510344638.1A CN106316800B (en) | 2015-06-19 | 2015-06-19 | A kind of low power consuming by preparing dimethyl ether from methanol method |
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| CN201510344638.1A CN106316800B (en) | 2015-06-19 | 2015-06-19 | A kind of low power consuming by preparing dimethyl ether from methanol method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232352A (en) * | 2018-09-19 | 2019-01-18 | 江阴市大洋固废处置利用有限公司 | N-methyl pyrrolidone decompression purification system and purification method |
| CN109821266A (en) * | 2019-03-19 | 2019-05-31 | 天津凯赛特科技有限公司 | A kind of furfural multiple-effect reaction and rectification device and technique |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891597A (en) * | 2010-07-05 | 2010-11-24 | 杨奇申 | Dimethyl ether production method with multi-stage reactions |
| CN101941892A (en) * | 2010-09-20 | 2011-01-12 | 四川天一科技股份有限公司 | Method for preparing dimethyl ether from methyl alcohol |
| CN104058941A (en) * | 2013-03-22 | 2014-09-24 | 泉州恒河化工有限公司 | Method for preparing dimethyl ether by dehydration of methanol |
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- 2015-06-19 CN CN201510344638.1A patent/CN106316800B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891597A (en) * | 2010-07-05 | 2010-11-24 | 杨奇申 | Dimethyl ether production method with multi-stage reactions |
| CN101941892A (en) * | 2010-09-20 | 2011-01-12 | 四川天一科技股份有限公司 | Method for preparing dimethyl ether from methyl alcohol |
| CN104058941A (en) * | 2013-03-22 | 2014-09-24 | 泉州恒河化工有限公司 | Method for preparing dimethyl ether by dehydration of methanol |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232352A (en) * | 2018-09-19 | 2019-01-18 | 江阴市大洋固废处置利用有限公司 | N-methyl pyrrolidone decompression purification system and purification method |
| CN109232352B (en) * | 2018-09-19 | 2024-03-19 | 江阴市大洋固废处置利用有限公司 | N-methyl pyrrolidone decompression purification system and purification method |
| CN109821266A (en) * | 2019-03-19 | 2019-05-31 | 天津凯赛特科技有限公司 | A kind of furfural multiple-effect reaction and rectification device and technique |
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