CN105503523A - Methanol rectification method - Google Patents

Methanol rectification method Download PDF

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Publication number
CN105503523A
CN105503523A CN201510968500.9A CN201510968500A CN105503523A CN 105503523 A CN105503523 A CN 105503523A CN 201510968500 A CN201510968500 A CN 201510968500A CN 105503523 A CN105503523 A CN 105503523A
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China
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tower
methanol
atmospheric
rectification method
pressurizing
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CN201510968500.9A
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Inventor
边兴海
陈建国
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Coal Chemical Industry Co Ltd By Shares Of Precious Ace Semi Of Qitaihe
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Coal Chemical Industry Co Ltd By Shares Of Precious Ace Semi Of Qitaihe
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Priority to CN201510968500.9A priority Critical patent/CN105503523A/en
Publication of CN105503523A publication Critical patent/CN105503523A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention provides a methanol rectification method, and relates to methanol rectification. The methanol rectification method aims at solving the technical problems that for an existing methanol rectification method, energy consumption is large, and the purity of a finished product is low. The method comprises the steps that 1, crude methanol is preheated; 2, cooling is conducted, and a pretreated methanol solution is obtained; 3, the pretreated methanol solution is sent to the tower top of a pre-rectifying tower for refluxing; 4, the reflux methanol solution is fed into a pressurization tower; 5, condensation and refluxing are conducted in an atmospheric tower reboiler; 6, refluxing is conducted in an atmospheric tower. According to the methanol rectification method, the energy consumption is low, and the purity of the finished product is high. The methanol rectification method is used for methanol rectification.

Description

A kind of methanol rectification method
Technical field
The present invention relates to methanol rectification.
Background technology
The reaction conditions of the generation that methanol-fueled CLC reacts and synthesis is closely related, even if the element participating in reaction only has in hydrocarbon oxygen three, but often due to the effect of synthetic reaction condition, building-up reactions all can be made to depart from main reaction, generate various by product, the impurity component namely in methyl alcohol, therefore in order to obtain high purity methanol, rectification process must be adopted to purify, remove all impurity.
Summary of the invention
The present invention will solve existing methanol rectification method and there is energy consumption greatly, the technical problem that finished product purity is low, and provides a kind of methanol rectification method.
A kind of methanol rectification method, specifically carry out according to following steps:
One, crude carbinol is passed into crude carbinol preheater preheats, then enter the middle part of pre-rectifying tower, the alkali lye of mass concentration 5% and crude carbinol are converged before entering pre-rectifying tower, alkali lye and crude carbinol are converged, and make alkali lye and crude carbinol volume ratio be 0.3% ~ 3%;
Two, the gas that pre-rectifying tower tower top generates is passed into pre-tower air cooler, then flow through pre-tower condenser I and pre-tower condenser II successively, obtain pre-methanol solution;
Three, pre-methanol solution is passed in pre-tower backflash, then deliver to pre-rectifying tower tower top through the pressurization of pre-tower reflux pump and reflux;
Four, the prognosis methyl alcohol that pre-rectifying tower tower bottom flow goes out is passed into methanol pump pressurization, then pass into pressurizing tower preheater, then pass in pressurizing tower;
Five, the methanol steam that pressurizing tower tower top generates is passed into the condensation of atmospheric tower reboiler, obtain methanol solution; A part of methanol solution is back to the backflow of pressurizing tower jacking row by the pressurization of pressurizing tower reflux pump, and another part methanol solution, through the cooling of pressurizing tower methyl alcohol water cooler, obtains finished product methyl alcohol, delivers to tank field;
Six, the methanol water mix-ture generated at the bottom of pressurizing tower tower is passed in atmospheric tower, the gas that atmospheric tower tower top generates passes into atmospheric tower air cooler and Atmospheric Tower cooler successively, enter atmospheric tower backflash again, pressurize through atmospheric tower reflux pump, a part passes into atmospheric tower tower top as phegma and refluxes, and another part passes into the cooling of atmospheric tower refined methanol water cooler, obtains finished product methyl alcohol, deliver to tank field, complete a kind of methanol rectification method.
The invention has the beneficial effects as follows: methyl alcohol specification prepared by the present invention to be mass concentration be 99.9% methyl alcohol, be premium grads according to standard GB/T 338-2011; In the present invention, pre-rectifying tower and atmospheric tower overhead condensation adopt air cooling string water-cooled, greatly reduce the consumption of water coolant; Pressurization tower top methanol steam heat recycled by atmospheric tower, decreases the consumption of steam, additionally reduces the consumption of water coolant simultaneously; Not only high-temperature fine methyl alcohol preheated feed crude carbinol, fully reclaims heat but also reduces cooling water amount.In present method three wastes discharge amount, non-condensable gas flows out from washing letdown tank, wherein by volume calculates CO 2account for 70.7%, H 2account for 1.3%, N 2account for 3.2%, CH 3oH accounts for 1.8%, CH 4account for 3.2%, H 2o accounts for 19.7%; Methyl alcohol residual night from residual night, water cooler flowed out, wherein CH by mass 3oH accounts for 0.1%, high-boiling point alcohol accounts for 0.2%, H 2o accounts for 99.7%.In present method operation, solid caustic soda consumption is 7.5 ~ 9kg, and cooling water consumption is 650 ~ 800 tons, power consumption 1080kW/h.The present invention can reduce the consumption of sodium hydroxide, and treatment capacity increases by more than 5 percent.
The present invention is used for methanol rectification.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of methanol rectification method of present embodiment, specifically carry out according to following steps:
One, crude carbinol is passed into crude carbinol preheater preheats, then enter the middle part of pre-rectifying tower, the alkali lye of mass concentration 5% and crude carbinol are converged before entering pre-rectifying tower, alkali lye and crude carbinol are converged, and make alkali lye and crude carbinol volume ratio be 0.3% ~ 3%;
Two, the gas that pre-rectifying tower tower top generates is passed into pre-tower air cooler, then flow through pre-tower condenser I and pre-tower condenser II successively, obtain pre-methanol solution;
Three, pre-methanol solution is passed in pre-tower backflash, then deliver to pre-rectifying tower tower top through the pressurization of pre-tower reflux pump and reflux;
Four, the prognosis methyl alcohol that pre-rectifying tower tower bottom flow goes out is passed into methanol pump pressurization, then pass into pressurizing tower preheater, then pass in pressurizing tower;
Five, the methanol steam that pressurizing tower tower top generates is passed into the condensation of atmospheric tower reboiler, obtain methanol solution; A part of methanol solution is back to the backflow of pressurizing tower jacking row by the pressurization of pressurizing tower reflux pump, and another part methanol solution, through the cooling of pressurizing tower methyl alcohol water cooler, obtains finished product methyl alcohol, delivers to tank field;
Six, the methanol water mix-ture generated at the bottom of pressurizing tower tower is passed in atmospheric tower, the gas that atmospheric tower tower top generates passes into atmospheric tower air cooler and Atmospheric Tower cooler successively, enter atmospheric tower backflash again, pressurize through atmospheric tower reflux pump, a part passes into atmospheric tower tower top as phegma and refluxes, and another part passes into the cooling of atmospheric tower refined methanol water cooler, obtains finished product methyl alcohol, deliver to tank field, complete a kind of methanol rectification method.
Embodiment two: present embodiment and embodiment one unlike: in step one, methyl alcohol is preheated to 65 ~ 70 DEG C by crude carbinol preheater.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one unlike: add to pre-rectifying tower the sodium hydroxide solution that mass concentration is 5% by lye pump in step one, control flow is 100 ~ 150kg/h.Other is identical with embodiment one.
Lye pump outlet conduit is drawn branch directly to be introduced into tower crude carbinol pipeline, position
Embodiment four: present embodiment and embodiment one unlike: the gas temperature that in step 2, pre-rectifying tower tower top generates is 78 ~ 82 DEG C, and pressure is 0.05MPa.Other is identical with embodiment one.
Embodiment five: present embodiment and embodiment one unlike: controlling pre-methanol solution temperature in step 2 is 40 ~ 42 DEG C.Other is identical with embodiment one.
Embodiment six: present embodiment and embodiment one unlike: in step 4, the temperature of prognosis methyl alcohol is 83 ~ 88 DEG C.Other is identical with embodiment one.
Embodiment seven: present embodiment and embodiment one unlike: in step 4, pressurizing tower preheater preheats temperature is 125 DEG C.Other is identical with embodiment one.
Embodiment eight: present embodiment and embodiment one unlike: in step 4, pressurizing tower working pressure is 0.6MPa.Other is identical with embodiment one.
Embodiment nine: present embodiment and embodiment one unlike: the methanol water mix-ture temperature generated at the bottom of pressurizing tower tower in step 6 is 133 ~ 137 DEG C, and the gas temperature that atmospheric tower tower top generates is 70 ~ 72 DEG C.Other is identical with embodiment one.
Embodiment ten: present embodiment and embodiment one unlike: in step 6, Atmospheric Tower cooler is cooled to temperature is 60 DEG C, and it is 40 DEG C that atmospheric tower refined methanol water cooler is cooled to temperature.Other is identical with embodiment one.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
A kind of methanol rectification method of the present embodiment, specifically carry out according to following steps:
One, crude carbinol is passed into crude carbinol preheater preheats, then enter the middle part of pre-rectifying tower, the alkali lye of mass concentration 5% and crude carbinol are converged before entering pre-rectifying tower, alkali lye and crude carbinol are converged, and make alkali lye and crude carbinol volume ratio be 1%;
Two, the gas that pre-rectifying tower tower top generates is passed into pre-tower air cooler, then flow through pre-tower condenser I and pre-tower condenser II successively, obtain pre-methanol solution;
Three, pre-methanol solution is passed in pre-tower backflash, then deliver to pre-rectifying tower tower top through the pressurization of pre-tower reflux pump and reflux;
Four, the prognosis methyl alcohol that pre-rectifying tower tower bottom flow goes out is passed into methanol pump pressurization, then pass into pressurizing tower preheater, then pass in pressurizing tower;
Five, the methanol steam that pressurizing tower tower top generates is passed into the condensation of atmospheric tower reboiler, obtain methanol solution; A part of methanol solution is back to the backflow of pressurizing tower jacking row by the pressurization of pressurizing tower reflux pump, and another part methanol solution, through the cooling of pressurizing tower methyl alcohol water cooler, obtains finished product methyl alcohol, delivers to tank field;
Six, the methanol water mix-ture generated at the bottom of pressurizing tower tower is passed in atmospheric tower, the gas that atmospheric tower tower top generates passes into atmospheric tower air cooler and Atmospheric Tower cooler successively, enter atmospheric tower backflash again, pressurize through atmospheric tower reflux pump, a part passes into atmospheric tower tower top as phegma and refluxes, and another part passes into the cooling of atmospheric tower refined methanol water cooler, obtains finished product methyl alcohol, deliver to tank field, complete a kind of methanol rectification method.
Methyl alcohol specification prepared by present method to be mass concentration be 99.9% methyl alcohol, be premium grads according to standard GB/T 338-2011; In present method, pre-rectifying tower and atmospheric tower overhead condensation adopt air cooling string water-cooled, greatly reduce the consumption of water coolant; Pressurization tower top methanol steam heat recycled by atmospheric tower, decreases the consumption of steam, additionally reduces the consumption of water coolant simultaneously; Not only high-temperature fine methyl alcohol preheated feed crude carbinol, fully reclaims heat but also reduces cooling water amount.In present method three wastes discharge amount, non-condensable gas flows out from washing letdown tank, wherein by volume calculates CO 2account for 70.7%, H 2account for 1.3%, N 2account for 3.2%, CH 3oH accounts for 1.8%, CH 4account for 3.2%, H 2o accounts for 19.7%; Methyl alcohol residual night from residual night, water cooler flowed out, wherein CH by mass 3oH accounts for 0.1%, high-boiling point alcohol accounts for 0.2%, H 2o accounts for 99.7%.In present method operation, solid caustic soda consumption is 7.5 ~ 9kg, and cooling water consumption is 650 ~ 800 tons, power consumption 1080kW/h.

Claims (10)

1. a methanol rectification method, is characterized in that what the method was specifically carried out according to following steps:
One, crude carbinol is passed into crude carbinol preheater preheats, then enter the middle part of pre-rectifying tower, the alkali lye of mass concentration 5% and crude carbinol are converged before entering pre-rectifying tower, alkali lye and crude carbinol are converged, and make alkali lye and crude carbinol volume ratio be 0.3% ~ 3%;
Two, the gas that pre-rectifying tower tower top generates is passed into pre-tower air cooler, then flow through pre-tower condenser I and pre-tower condenser II successively, obtain pre-methanol solution;
Three, pre-methanol solution is passed in pre-tower backflash, then deliver to pre-rectifying tower tower top through the pressurization of pre-tower reflux pump and reflux;
Four, the prognosis methyl alcohol that pre-rectifying tower tower bottom flow goes out is passed into methanol pump pressurization, then pass into pressurizing tower preheater, then pass in pressurizing tower;
Five, the methanol steam that pressurizing tower tower top generates is passed into the condensation of atmospheric tower reboiler, obtain methanol solution; A part of methanol solution is back to the backflow of pressurizing tower jacking row by the pressurization of pressurizing tower reflux pump, and another part methanol solution, through the cooling of pressurizing tower methyl alcohol water cooler, obtains finished product methyl alcohol, delivers to tank field;
Six, the methanol water mix-ture generated at the bottom of pressurizing tower tower is passed in atmospheric tower, the gas that atmospheric tower tower top generates passes into atmospheric tower air cooler and Atmospheric Tower cooler successively, enter atmospheric tower backflash again, pressurize through atmospheric tower reflux pump, a part passes into atmospheric tower tower top as phegma and refluxes, and another part passes into the cooling of atmospheric tower refined methanol water cooler, obtains finished product methyl alcohol, deliver to tank field, complete a kind of methanol rectification method.
2. a kind of methanol rectification method according to claim 1, is characterized in that in step one, 2 methyl alcohol are preheated to 65 ~ 70 DEG C by crude carbinol preheater.
3. a kind of methanol rectification method according to claim 1, it is characterized in that adding to pre-rectifying tower the sodium hydroxide solution that mass concentration is 5% by lye pump in step one, control flow is 100 ~ 150kg/h.
4. a kind of methanol rectification method according to claim 1, it is characterized in that the gas temperature that in step 2, pre-rectifying tower tower top generates is 78 ~ 82 DEG C, pressure is 0.05MPa.
5. a kind of methanol rectification method according to claim 1, is characterized in that controlling pre-methanol solution temperature in step 2 is 40 ~ 42 DEG C.
6. a kind of methanol rectification method according to claim 1, is characterized in that the temperature of prognosis methyl alcohol in step 4 is 83 ~ 88 DEG C.
7. a kind of methanol rectification method according to claim 1, is characterized in that in step 4, pressurizing tower preheater preheats temperature is 125 DEG C.
8. a kind of methanol rectification method according to claim 1, is characterized in that in step 4, pressurizing tower working pressure is 0.6MPa.
9. a kind of methanol rectification method according to claim 1, it is characterized in that the methanol water mix-ture temperature generated at the bottom of pressurizing tower tower in step 6 is 133 ~ 137 DEG C, the gas temperature that atmospheric tower tower top generates is 70 ~ 72 DEG C.
10. a kind of methanol rectification method according to claim 1, it is characterized in that in step 6 that Atmospheric Tower cooler is cooled to temperature is 60 DEG C, and it is 40 DEG C that atmospheric tower refined methanol water cooler is cooled to temperature.
CN201510968500.9A 2015-12-21 2015-12-21 Methanol rectification method Pending CN105503523A (en)

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Application Number Priority Date Filing Date Title
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1760164A (en) * 2005-10-27 2006-04-19 天津大学 Energy saving equipment of double effect rectification for methanol, and method
CN101607869A (en) * 2009-07-21 2009-12-23 天津大学 Methanol double-effect rectification high-elasticity combined technique and system thereof
CN102757315A (en) * 2012-07-09 2012-10-31 四川天一科技股份有限公司 Device and method of co-production of dimethyl ether by methanol plant
CN104370697A (en) * 2014-11-07 2015-02-25 上海国际化建工程咨询公司 Flexible methanol rectification method and device capable of producing both MTO-grade and AA-grade methanol

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1760164A (en) * 2005-10-27 2006-04-19 天津大学 Energy saving equipment of double effect rectification for methanol, and method
CN101607869A (en) * 2009-07-21 2009-12-23 天津大学 Methanol double-effect rectification high-elasticity combined technique and system thereof
CN102757315A (en) * 2012-07-09 2012-10-31 四川天一科技股份有限公司 Device and method of co-production of dimethyl ether by methanol plant
CN104370697A (en) * 2014-11-07 2015-02-25 上海国际化建工程咨询公司 Flexible methanol rectification method and device capable of producing both MTO-grade and AA-grade methanol

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