CN102992951A - Method for preparing high-purity refined methanol by three-tower rectification - Google Patents
Method for preparing high-purity refined methanol by three-tower rectification Download PDFInfo
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Abstract
The invention discloses a method for preparing high-purity refined methanol by three-tower rectification, which is used for preparing high-purity refined methanol by treating a methanol crude product by using a three-tower rectification method. The method comprises the steps of: based on diluted alcohol water or soft water as an extraction agent, distilling in a pre-separating tower to remove low-boiling substances in the methanol crude product and water-insoluble gas so as to obtain pre-separated methanol; sending pre-separated methanol into a pressurizing tower for pressurized rectification treatment, cooling light components at the tower top of the pressurizing tower, returning a part of the light components to the tower top of the pressurizing tower for refluxing, and collecting the rest of the light components as the refined methanol product; sending heavy components at the tower bottom of the pressurizing tower into a main rectifying tower for rectification, cooling light components at the tower top of the main rectifying tower, returning a part of the light components to the tower top of the main rectifying tower for refluxing, and collecting the rest of the light components as the refined methanol product; and discharging the main rectifying tower bottom liquid as waste liquid. By using the 'three-tower rectification' method, the problem that methanol azeotropes cannot be separated in the methanol products is effectively solved, the purity of the obtained refined methanol product reaches more than 99.9%, the mass percent concentration of methanol in the discharged waste liquid is smaller than 1.0%, and the pollution of effluents to the environment is reduced because the methanol content is low.
Description
Technical field
The present invention relates to the methanol production technical field, be specifically related to the method that a kind of three-tower rectification prepares high purity extractive methyl alcohol.
Background technology
Methyl alcohol plays a very important role in world economy as one of important basic organic chemical industry raw material.Increasingly in short supply along with world energy sources, methyl alcohol progressively develops into again important energy substitution product, has also obtained developing rapidly take methyl alcohol as Chemicals industries such as raw material dimethyl ether synthesis, alkene.At present, China's methyl alcohol production capacity has accounted for 1/4 of world's aggregated capacity, and total capacity exceedes 2,900 ten thousand t/a.Along with the application with methanol fuel of developing rapidly of carbinol derivatives and derived product thereof, the methyl alcohol demand also can be increasing, therefore improves the methanol product quality, reduces to produce and consume the concern that just more and more causes enterprise.It is last procedure of methanol production that methanol rectification is purified, and its energy consumption accounts for about 20% of methanol production total energy consumption.Because the methanol rectification technology is directly connected to the methanol product quality that finally makes, therefore also be one important procedure in the methanol production.Selecting appropriate rectification process, is the Important Action that reduces the methanol production cost, saves energy and reduce the cost, improves Business Economic Benefit and the market competitiveness.
The refining methanol technology at home and abroad after deliberation for a long time, disclosed technical publications is also more, and a lot of producers and research unit is also arranged also in continuous this technology of research both at home and abroad, also makes some progress.Refining methanol technology foreign study present situation: mainly by make extraction agent with water thick methyl alcohol is extracted, remove the lower-boiling impurities such as the ether that is lower than the methyl alcohol boiling point, aldehyde, ketone, rectifying separation water and Methanol get methanol product again; Also have adopting to use water as the extraction agent extracting rectifying and remove on the basis of lower-boiling impurity, offer the impurity such as ethanol that side line is further removed enrichment at rectifying tower subsequently again, thereby obtain the methyl alcohol of higher degree.Domestic research at present: use 732 type Zeo-karbs to eliminate readily oxidizable substance, organic substance (such as aldehyde, ketone) and hydrogen, amine etc. in the methyl alcohol, improve the purity of methyl alcohol, effect is remarkable; Or the process for purification of the thick alcohol of the pure method production of employing connection, adopt lateral line discharging, discharge wherein C
6～C
10The accumulation of the alcohol dissolubility impurities such as higher alkane, increase the light constituent of the pre-tower of methanol rectification and the volatility of methyl alcohol, and increase condensation dynamics and the light constituent impurity such as pre-tower quantity of reflux removal dme, formaldehyde, methylamine, acetaldehyde, methyl-formiate, realize the purpose of refining methanol; Or remove the impurity such as minor amount of water, acetone, first vinegar, formaldehyde, formic acid and acetic acid that contain in the industrial methanol by the integrated isolation technique of batch reactive distillation; Or by increasing the shared composition of extraction agent water in the pre-tower of methyl alcohol and the water-and-oil separator, effectively improve the water-soluble of the standby methanol product of the pure legal system of connection.
At present the common issue with that faces of methanol rectification is methanol azeotrope impurity in the thick methyl alcohol such as dimethyl carbonate etc., these impurity meetings mixture identical with the formation of methanol boiling point, extremely difficult separation, present rectification and purification method can't be isolated these methanol azeotrope impurity, so that the purity of methanol product can't improve, the methanol product best level that makes also can only reach purity 99.5%, and quality is difficult to stable.And it is high to contain alcohol amount in the methanol rectified raffinate, in the raffinate methanol quality percentage concentration generally more than 3%, serious environment pollution in the process of discharging.Steam consumption can't make a breakthrough all the time in addition, and the ton methanol rectification consumes steam generally at 1.5～1.8 tons at present.
Summary of the invention
The purpose of this invention is to provide the method that a kind of three-tower rectification prepares high purity extractive methyl alcohol.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind of three-tower rectification prepares the method for high purity extractive methyl alcohol, may further comprise the steps:
(1) pre-separation tower extractive distillation
Take rare pure water or soft water as extraction agent, the methyl alcohol crude product is preheated to 70～90 ℃, send into pre-separation tower middle part, add extraction agent on pre-separation tower top, the flow of extraction agent is 20～40% of methyl alcohol crude product flow, and pre-separation Tata bottom pressure is controlled to be 30～60Kpa, column bottom temperature is 78～84 ℃, tower top temperature is 65～72 ℃, by low-boiling point material such as ethers, amine etc., the simultaneously gas that is insoluble in water such as CO, the CO in the methanol removal crude product in the distillation methanol removal crude product
2, CH
4Deng, make pre-separation methyl alcohol, pre-separation column overhead recycling of condensed steam, noncondensable gas emptying;
(2) the pressurizing tower compression rectification is processed
Pre-separation methyl alcohol is heated to 100～120 ℃, send into pressurizing tower from the pressurizing tower middle part and carry out compression rectification, the pressurizing tower internal pressure is controlled to be 500～700Kpa, the pressurizing tower column bottom temperature is 120～135 ℃, tower top temperature is 115～125 ℃, compression rectification has improved the envrionment temperature that methanol azeotrope separates, the methanol azeotrope detachment dynamic obviously improves, the light constituent that the pressurizing tower cat head obtains turns back to the pressurizing tower trim the top of column through the cooling rear portion, remainder is collected the methyl alcohol pan tank, obtain the high purity extractive methanol product, non-condensable gas emptying, the restructuring that obtains at the bottom of the pressurization Tata is divided into rarer methanol solution;
(3) main distillation column rectification process
Send into main distillation column by the main distillation column middle part after the restructuring lease making decompression that obtains at the bottom of the pressurization Tata and carry out rectifying, the main distillation column column bottom temperature is 102～108 ℃, tower top temperature is 64～66 ℃, the tower internal pressure is controlled to be 15～50Kpa, the light constituent that the main distillation column cat head obtains turns back to the main distillation column trim the top of column through the cooling rear portion, and remainder is collected the methyl alcohol pan tank, obtains the high purity extractive methanol product, non-condensable gas emptying, the main distillation column kettle base solution is as discharging of waste liquid.
Described rare pure water is that the methanol quality percentage ratio that contains that synthetic ammonia joins that copper washing-refining post water wash column in the pure technique produces is 2～5% soft water.
In the step (1), the proportion of the pre-separation methyl alcohol that obtains is 0.82～0.87g/cm
3
The pH value of pre-separation methyl alcohol is 6.5～8.5.In order to impel the decomposition of amine in the methyl alcohol crude product, carbonyl class, carbonyl compound, prevent that the organic acid in the methyl alcohol crude product from producing corrosion to rectifying device, the pH value of pre-separation methyl alcohol is controlled to be 6.5～8.5.
The purity of the high purity extractive methanol product that obtains 〉=99.9%.
The mass percent concentration of methyl alcohol≤1.0% in the main distillation column kettle base solution.
In the step (1), the consumption control of extraction agent is very crucial, control suitable consumption and can guarantee that effect of extracting is good, can effectively remove low-boiling point material and the gas that is insoluble in water in the methyl alcohol crude product, the flow control of extraction agent is 20～40% of methyl alcohol crude product flow among the present invention.
Three-tower rectification provided by the invention prepares the method for high purity extractive methyl alcohol, with rare pure water or soft water as extraction agent, at first remove low-boiling point material and the gas that is insoluble in water in the methyl alcohol crude product, then enter pressurizing tower and carry out the compression rectification processing, pressurizing tower adopts the bubble point temperature charging, be about to pre-separation methyl alcohol and be heated to 100～120 ℃, then send into pressurizing tower and carry out rectification process, feeding temperature is the important control index, guarantee the bubble point temperature charging, could the most reasonably utilize the heat energy of reboiler, reduce steam consumption, control pressurizing tower internal pressure is 500～700Kpa, the pressure that namely improves in the rectifying tower by compression rectification improves the envrionment temperature that methanol azeotrope separates, and the column bottom temperature of compression rectification tower can reach 120～135 ℃, and the detachment dynamic of methanol azeotrope obviously improves, effectively solved the separation problem of methanol azeotrope, the purity of product is reached more than 99.9%; Namely the pressurize restructuring that obtains at the bottom of the Tata of liquid divides and carries out rectification process at the bottom of adopting afterwards main distillation column to the compression rectification Tata, to remove the high-boiling-point impurity in the liquid at the bottom of the compression rectification Tata, such as different heptanone, the isobutyl-wet goods, control main distillation column column bottom temperature is 102～108 ℃, tower top temperature is 64～66 ℃, the tower internal pressure is controlled to be 15～50Kpa, further reclaimed the methyl alcohol in the restructuring at the bottom of the pressurization Tata minute, and the mass percent concentration of methyl alcohol≤1.0% in the main distillation column kettle base solution that can guarantee to obtain, reduce the content of methyl alcohol in the relief liquor, reduced the pollution of discharge to environment.
Adopt three-tower rectification provided by the invention to prepare the method for high purity extractive methyl alcohol, the purity of the refined methanol product that processing methyl alcohol crude product makes reaches more than 99.9%, be that the mass percent concentration of methyl alcohol reaches more than 99.9% in the refined methanol, methanol product purity significantly improves.And the discharging waste liquid is that the mass percent concentration of methyl alcohol in the main distillation column kettle base solution is down to below 1.0%, and methanol content is low, has reduced the pollution of discharge to environment.
Three-tower rectification provided by the invention prepares the method for high purity extractive methyl alcohol, promoted the output of high purity methanol more than 50%, obtained more highly purified refined methanol, product purity is brought up to more than 99.9% from present 99.0%, constant product quality, and reduced steam consumption, ton methyl alcohol consumption steam also drops to 0.87～1.0t from 1.5～1.8t, to reduce simultaneously the discharging of methanol residue, the mass percent concentration of methyl alcohol is from being reduced to below 1.0% more than 3.0% in the raffinate, thereby greatly reduces environmental pollution.
Three-tower rectification provided by the invention prepares the method for high purity extractive methyl alcohol, for China's methanol purification has been explored a new operational path, can be national small nitrogen fertilizer business and play good exemplary role, China's synthetic ammonia connection alcohol is produced and the development of methyl alcohol industry thereby drive.The preparation method of high purity methanol provided by the invention can be generalized to the separating methanol workshop section of other companies, and even on other organic separating technologies, have considerable economic benefit and long-range social benefit.
Embodiment
Below by specific embodiment technical scheme of the present invention is elaborated.
Embodiment 1
The three-tower rectification that present embodiment provides prepares the method for high purity extractive methyl alcohol, may further comprise the steps:
(1) pre-separation tower extractive distillation
Take rare pure water as extraction agent, this rare pure water is that the methanol quality percentage ratio that contains that synthetic ammonia joins that copper washing-refining post water wash column in the pure technique produces is 2% soft water, the methyl alcohol crude product is preheated to 70 ℃, send into pre-separation tower middle part, add the rare pure water of extraction agent on pre-separation tower top, the flow of rare pure water is 20% of methyl alcohol crude product flow, pre-separation Tata bottom pressure is controlled to be 40～60Kpa, column bottom temperature is 78～84 ℃, and tower top temperature is 65～72 ℃, by low-boiling point material and the gas that is insoluble in water in the distillation methanol removal crude product, obtain pre-separation methyl alcohol, pre-separation column overhead recycling of condensed steam, noncondensable gas emptying, the proportion of pre-separation methyl alcohol is 0.84g/cm
3, the pH value of pre-separation methyl alcohol is 8.0;
(2) the pressurizing tower compression rectification is processed
Pre-separation methyl alcohol is heated to 110 ℃, send into pressurizing tower from the pressurizing tower middle part and carry out compression rectification, the pressurizing tower internal pressure is controlled to be 500～700Kpa, the pressurizing tower column bottom temperature is 120～135 ℃, and tower top temperature is 115～125 ℃, and the light constituent that the pressurizing tower cat head obtains turns back to the pressurizing tower trim the top of column through the cooling rear portion, remainder is collected the methyl alcohol pan tank, obtain the high purity extractive methanol product, non-condensable gas emptying obtains restructuring at the bottom of the pressurization Tata and divides;
(3) main distillation column rectification process
Send into main distillation column by the main distillation column middle part after the restructuring lease making decompression that obtains at the bottom of the pressurization Tata and carry out rectifying, the main distillation column column bottom temperature is 102～108 ℃, tower top temperature is 64～66 ℃, the tower internal pressure is controlled to be 35～50Kpa, the light constituent that the main distillation column cat head obtains turns back to the main distillation column trim the top of column through the cooling rear portion, remainder is collected the methyl alcohol pan tank, obtain the high purity extractive methanol product, non-condensable gas emptying, the main distillation column kettle base solution is as discharging of waste liquid, the mass percent concentration of methyl alcohol is 0.9% in the main distillation column kettle base solution, and the purity of refined methanol product is 99.91%.
The method that the three-tower rectification that adopts present embodiment to provide prepares high purity extractive methyl alcohol prepares methanol product, and methanol product consumption steam per ton is 0.95 ton.
Embodiment 2
The three-tower rectification that present embodiment provides prepares the method for high purity extractive methyl alcohol, may further comprise the steps:
(1) pre-separation tower extractive distillation
Take rare pure water as extraction agent, this rare pure water is that the methanol quality percentage ratio that contains that synthetic ammonia joins that copper washing-refining post water wash column in the pure technique produces is 5% soft water, the methyl alcohol crude product is preheated to 80 ℃, send into pre-separation tower middle part, add the rare pure water of extraction agent on pre-separation tower top, the flow of rare pure water is 40% of methyl alcohol crude product flow, pre-separation Tata bottom pressure is controlled to be 30～50Kpa, column bottom temperature is 78～84 ℃, and tower top temperature is 65～72 ℃, by low-boiling point material and the gas that is insoluble in water in the distillation methanol removal crude product, obtain pre-separation methyl alcohol, pre-separation column overhead recycling of condensed steam, noncondensable gas emptying, the proportion of pre-separation methyl alcohol is 0.82g/cm
3, the pH value of pre-separation methyl alcohol is 8.5;
(2) the pressurizing tower compression rectification is processed
Pre-separation methyl alcohol is heated to 100 ℃, send into pressurizing tower from the pressurizing tower middle part and carry out compression rectification, the pressurizing tower internal pressure is controlled to be 500～600Kpa, the pressurizing tower column bottom temperature is 120～135 ℃, and tower top temperature is 115～125 ℃, and the light constituent that the pressurizing tower cat head obtains turns back to the pressurizing tower trim the top of column through the cooling rear portion, remainder is collected the methyl alcohol pan tank, obtain the high purity extractive methanol product, non-condensable gas emptying obtains restructuring at the bottom of the pressurization Tata and divides;
(3) main distillation column rectification process
Send into main distillation column by the main distillation column middle part after the restructuring lease making decompression that obtains at the bottom of the pressurization Tata and carry out rectifying, the main distillation column column bottom temperature is 102～108 ℃, tower top temperature is 64～66 ℃, the tower internal pressure is controlled to be 15～30Kpa, the light constituent that the main distillation column cat head obtains turns back to the main distillation column trim the top of column through the cooling rear portion, remainder is collected the methyl alcohol pan tank, obtain the high purity extractive methanol product, non-condensable gas emptying, the main distillation column kettle base solution is as discharging of waste liquid, the mass percent concentration of methyl alcohol is 0.86% in the main distillation column kettle base solution, and the purity of refined methanol product is 99.94%.
The method that the three-tower rectification that adopts present embodiment to provide prepares high purity extractive methyl alcohol prepares methanol product, and methanol product consumption steam per ton is 1.0 tons.
Embodiment 3
The three-tower rectification that present embodiment provides prepares the method for high purity extractive methyl alcohol, may further comprise the steps:
(1) pre-separation tower extractive distillation
Take soft water as extraction agent, the methyl alcohol crude product is preheated to 90 ℃, send into pre-separation tower middle part, add extraction agent soft water on pre-separation tower top, the flow of soft water is 30% of methyl alcohol crude product flow, pre-separation Tata bottom pressure is controlled to be 30～45Kpa, column bottom temperature is 78～84 ℃, tower top temperature is 65～72 ℃, by low-boiling point material and the gas that is insoluble in water in the distillation methanol removal crude product, obtain pre-separation methyl alcohol, pre-separation column overhead recycling of condensed steam, noncondensable gas emptying, the proportion of pre-separation methyl alcohol are 0.87g/cm
3, the pH value of pre-separation methyl alcohol is 6.5;
(2) the pressurizing tower compression rectification is processed
Pre-separation methyl alcohol is heated to 120 ℃, send into pressurizing tower from the pressurizing tower middle part and carry out compression rectification, the pressurizing tower internal pressure is controlled to be 550～650Kpa, the pressurizing tower column bottom temperature is 120～135 ℃, and tower top temperature is 115～125 ℃, and the light constituent that the pressurizing tower cat head obtains turns back to the pressurizing tower trim the top of column through the cooling rear portion, remainder is collected the methyl alcohol pan tank, obtain the high purity extractive methanol product, non-condensable gas emptying obtains restructuring at the bottom of the pressurization Tata and divides;
(3) main distillation column rectification process
Send into main distillation column by the main distillation column middle part after the restructuring lease making decompression that obtains at the bottom of the pressurization Tata and carry out rectifying, the main distillation column column bottom temperature is 102～108 ℃, tower top temperature is 64～66 ℃, the tower internal pressure is controlled to be 20～40Kpa, the light constituent that the main distillation column cat head obtains turns back to the main distillation column trim the top of column through the cooling rear portion, remainder is collected the methyl alcohol pan tank, obtain the high purity extractive methanol product, non-condensable gas emptying, the main distillation column kettle base solution is as discharging of waste liquid, the mass percent concentration of methyl alcohol is 0.91% in the main distillation column kettle base solution, and the purity of refined methanol product is 99.97%.
The method that the three-tower rectification that adopts present embodiment to provide prepares high purity extractive methyl alcohol prepares methanol product, and methanol product consumption steam per ton is 0.87 ton.
The three-tower rectification that adopts the embodiment of the invention 1 to provide prepares the method for high purity extractive methyl alcohol and carries out the Economic and Efficiency Analysis of methanol production: should turn to example with the Hunan, methanol was 63651 tons in 2010, the high purity methanol product production has promoted 50%, and the benefit of creating is by improving the quality of products:
63651 * 50% * (2000-1100)=2864.3 ten thousand yuan,
The mass percentage content of residual methanol drops to 0.9% from 3% in the waste liquid, and benefit is:
Ten thousand yuan of 63651 * (3%-0.9%) * 2000=267.3,
Reduce the ton methanol steam and consume 800kg, steam cost is by 100 yuan/tons of calculating, and benefit is:
63651 * 0.8 * 100 yuan/tons=509.2 ten thousand yuan,
Create altogether 3640.8 ten thousand yuan of economic benefits, economic benefit is considerable.
Claims (6)
1. a three-tower rectification prepares the method for high purity extractive methyl alcohol, it is characterized in that, may further comprise the steps:
(1) pre-separation tower extractive distillation
The methyl alcohol crude product is preheated to 70～90 ℃, send into pre-separation tower middle part, take rare pure water or soft water as extraction agent, add described extraction agent on pre-separation tower top, the flow of extraction agent is 20～40% of methyl alcohol crude product flow, pre-separation Tata bottom pressure is controlled to be 30～60Kpa, column bottom temperature is 78～84 ℃, tower top temperature is 65～72 ℃, by low-boiling point material and the gas that is insoluble in water in the distillation methanol removal crude product, obtain pre-separation methyl alcohol, pre-separation column overhead recycling of condensed steam, noncondensable gas emptying;
(2) the pressurizing tower compression rectification is processed
Pre-separation methyl alcohol is heated to 100～120 ℃, send into pressurizing tower from the pressurizing tower middle part and carry out compression rectification, the pressurizing tower internal pressure is controlled to be 500～700Kpa, the pressurizing tower column bottom temperature is 120～135 ℃, and tower top temperature is 115～125 ℃, and the light constituent that the pressurizing tower cat head obtains turns back to the pressurizing tower trim the top of column through the cooling rear portion, remainder is collected the methyl alcohol pan tank, obtain the high purity extractive methanol product, non-condensable gas emptying obtains restructuring at the bottom of the pressurization Tata and divides;
(3) main distillation column rectification process
Send into main distillation column by the main distillation column middle part after the restructuring lease making decompression that obtains at the bottom of the pressurization Tata and carry out rectifying, the main distillation column column bottom temperature is 102～108 ℃, tower top temperature is 64～66 ℃, the tower internal pressure is controlled to be 15～50Kpa, the light constituent that the main distillation column cat head obtains turns back to the main distillation column trim the top of column through the cooling rear portion, and remainder is collected the methyl alcohol pan tank, obtains the high purity extractive methanol product, non-condensable gas emptying, the main distillation column kettle base solution is as discharging of waste liquid.
2. three-tower rectification according to claim 1 prepares the method for high purity extractive methyl alcohol, it is characterized in that, described rare pure water is that the methanol quality percentage ratio that contains that synthetic ammonia joins that copper washing-refining post water wash column in the pure technique produces is 2～5% soft water.
3. three-tower rectification according to claim 1 prepares the method for high purity extractive methyl alcohol, it is characterized in that, the proportion of described pre-separation methyl alcohol is 0.82～0.87g/cm
3
4. three-tower rectification according to claim 1 prepares the method for high purity extractive methyl alcohol, it is characterized in that, the pH value of pre-separation methyl alcohol is 6.5～8.5.
5. arbitrary described three-tower rectification prepares the method for high purity extractive methyl alcohol according to claim 1-4, it is characterized in that the purity of high purity extractive methanol product 〉=99.9%.
6. three-tower rectification according to claim 5 prepares the method for high purity extractive methyl alcohol, it is characterized in that the mass percent concentration of methyl alcohol≤1.0% in the main distillation column kettle base solution.
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| CN109678667A (en) * | 2019-01-22 | 2019-04-26 | 安徽昊源化工集团有限公司 | A kind of crude carbinol isolation and purification method |
| CN110218146A (en) * | 2018-03-02 | 2019-09-10 | 赵志峰 | High purity reagent produces film-falling crystallization isolation technics |
| CN114426462A (en) * | 2020-10-15 | 2022-05-03 | 中国石油化工股份有限公司 | Device and method for removing trimethylamine and/or heavy alcohol in methanol |
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| CN102992951B (en) | 2015-06-24 |
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