CN103193590A - Method for continuously extracting, rectifying and separating mixed alcohols from water - Google Patents
Method for continuously extracting, rectifying and separating mixed alcohols from water Download PDFInfo
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- CN103193590A CN103193590A CN2013100981807A CN201310098180A CN103193590A CN 103193590 A CN103193590 A CN 103193590A CN 2013100981807 A CN2013100981807 A CN 2013100981807A CN 201310098180 A CN201310098180 A CN 201310098180A CN 103193590 A CN103193590 A CN 103193590A
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Abstract
The invention discloses a method for continuously extracting, rectifying and separating mixed alcohols from water, relates to a chemical separating method, and in particular to a method for continuously extracting, rectifying and separating mixed alcohols such as aqueous mixtures of ethanol, n-propyl alcohol, isobutyl alcohol and the like. According to the method, extractive distillation and common rectifying are combined together, and a multi-column combined step-by-step separating method is adopted to separate mixed alcohols from water step by step and recycle components with high purity. The method comprises steps of: with ethylene glycol as an extraction agent, separating the mixed alcohols from water in an extractive rectifying column B1, wherein the column B1 adopts normal pressure rectification, the reflux ratio is 1:1-10:1, the mixed alcohols can be get from the column top, and a mixture of a solvent and water can be get from the column bottom; recovering most of the solvent from a solvent recovering column B4 and recycling the solvent; and effectively separating the mixed alcohols through columns B2 and B3. According to the method, extractive distillation and common rectifying are combined together, the extraction agent is used to avoid the azeotrope of alcohols and water, and continuous separation of multiple columns are adopted to recover the components with high purity step by step, so that the method has high economic and environmental benefits.
Description
Technical field
The present invention relates to a kind of chemical separating method, particularly relate to a kind of method of continuous extraction rectifying separation alcohol mixture-water, can be used for reclaiming in the alcohol-water mixture valuable alcohols.
Background technology
Exhaustion day by day along with petroleum resources, the future source of energy structure will turn to based on coal and Sweet natural gas, produce preparing low-carbon mixed alcohol by synthetic gas fuel as an alternative by Sweet natural gas or gasification, more and more be subject to people's attention, yet in the technology of synthesis gas preparation low-carbon alcohol, what inevitably produce a large amount of contains pure waste liquid, if with the various waste liquids that produce in the industrial production directly discharging can cause the serious wasting of resources and environmental pollution, reclaim and obtain mixture of lower alcohols or the higher alcohols of purity has huge Significance for Environment and economic implications containing pure waste liquid.The low-carbon alcohol mixture has broad application prospects, summarize and to get up to mainly contain the following aspects: (1), is realized the alkylation of coal and can be dissolved and effectively transportation as one of means of gelatin liquefaction as alternative fuel (2) clean gasoline additive (3) chemical and industrial chemicals (4).As liquefied petroleum gas (LPG) (LPG) surrogate; Directly reach as general chemical solvents and be used for efficient power generation etc.
The traditional method of the pure water system of present domestic separation mainly contains: (1) sequence of constant boiling and rectification method, its major advantage is the mechanization degree height, output is big, quality is good, deficiency is that the sequence of constant boiling and rectification facility investment is big, because the gasification of new adding nonvariant boiling reagent certainly will increase energy consumption, the use of nonvariant boiling reagent benzene commonly used is harmful to operator's health, so will be replaced by the novel process of environmental protection gradually.(2) membrane distillation method, but because the mould material production cost is high relatively, membrane separation technique also not fully matured therefore be not used widely.
Summary of the invention
The object of the present invention is to provide a kind of method of continuous extraction rectifying separation alcohol mixture-water, this method adopts extracting rectifying to separate pure water mixed system with the method that conventional distillation combines, select the more excellent extraction agent ethylene glycol of separating effect, and a kind of more rational technical process is proposed, improve plant efficiency, saved production cost.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of continuous extraction rectifying separation alcohol mixture-water said method comprising the steps of:
(1) the alcohol-water mixture material enters pure water separation column B1 at the bubble point state, and extraction agent is from adding continuously near the cat head position, and the overhead product of B1 tower is ethanol, n-propyl alcohol and isopropylcarbinol, the mixture of extraction solvent and water at the bottom of the tower;
(2) the B1 overhead product enters ethanol recovery tower B2 through interchanger H1 and pump P2, and cat head obtains high purity ethanol; Obtain the mixture of n-propyl alcohol and isopropylcarbinol at the bottom of the tower, enter n-propyl alcohol isopropylcarbinol recovery tower B3 through interchanger H3 and pump P3 again, cat head obtains the high purity n-propyl alcohol, obtains the high purity isopropylcarbinol at the bottom of the tower;
(3) introduce solvent recovery tower B4 by the overhead product that obtains at the bottom of the B1 Tata through interchanger H1 and pump P1, realize the recovery of solvent ethylene glycol, and recycle.
The method of said a kind of continuous extraction rectifying separation alcohol mixture-water, the extraction agent of its described extracting rectifying is ethylene glycol, glycol circulation is used in the rectifying.
The method of said a kind of continuous extraction rectifying separation alcohol mixture-water, described processing condition are as follows: the B1 tower: total stage number 82, feed tray 60, reflux ratio 1.35; The total stage number 62 of B2 tower, feed tray 32, reflux ratio 2.63; The total stage number 84 of B3 tower, feed tray 40, reflux ratio 4.67; The total stage number 9 of B4 tower, feed tray 5, reflux ratio 0.47.
Advantage of the present invention and effect are:
The method of a kind of continuous extraction rectifying separation of the present invention alcohol mixture-water, in view of the deficiency on the prior art, the maturation and extraction rectifying method possesses skills, the extraction agent range of choice is bigger, it is convenient to use, be easy to advantages such as industrialization, the method that the present invention adopts extracting rectifying and conventional distillation to combine is separated pure water mixed system.1, select the more excellent extraction agent ethylene glycol of separating effect, improved separation efficiency, reduced reflux ratio, saved energy consumption.2 propose a kind of more rational technical process, have improved plant efficiency, save production cost, and have bigger energy economy ﹠ environment benefit.
Description of drawings
Fig. 1 is the designed continuous extraction rectification process schema of the present invention.
Embodiment
As shown in the figure: among the figure: B1: extractive distillation column; B2: ethanol recovery tower; B3: n-propyl alcohol isopropylcarbinol Separation and Recovery tower; B4: solvent recovery tower;
Fig. 2 is the extracting rectifying Experimental equipment.Among the figure 1: the ethylene glycol storage tank; 2: contain pure waste tank; 3: spinner-type flowmeter; 4: thermometer; 5: tower reactor; 6: tower reactor discharging condenser; 7: thief hole at the bottom of the tower; 8: tower reactor overhead product storage tank; 9: the overhead product storage tank; 10: the electromagnetism reflux ratio controller; 11: the cat head thief hole; 12: the body of the tower thief hole; 13 is overhead condenser.
Example 1: continuous extraction rectifying separation alcohol-water mixture flow process is with reference to Fig. 1, and extractive distillation column is with reference to Fig. 2, and the tower body internal diameter is 25mm, and the body of the tower filler is Φ 3
3mm stainless steel θ ring filler, the about 1.6m of filler part total height, number of theoretical plate is about 80, has 3 and 2 body of the tower thief holes at rectifying section and the stripping section of extractive distillation column, is convenient to detect liquid phase and forms content.When beginning experiment, open the water coolant of condenser at the bottom of cat head and the tower earlier, close the valve at the bottom of cat head and the tower, the ethylene glycol that in tower reactor, adds solvent ratio and be 4:1 with contain pure waste liquid mixed solution 300ml; Connect the tower reactor heating power supply, be heated to boiling, until wetting body of the tower filler.Suitably regulate heater voltage, keep total reflux 15 minutes; Open the charging valve port, solvent ethylene glycol is through spinner-type flowmeter, in the filler position charging near the cat head place; Contain pure waste liquid and flow out from storage tank 2, the position charging enters extractive distillation column near tower; Regulate feeding rate by valve port and spinner-type flowmeter, the ethylene glycol feed flow rates is 0.644ml/min, and containing pure waste liquid feed flow rates is 0.279ml/min; Open reflux ratio controller, setting reflux ratio is 1.35, begins to reflux; Open the cat head valve port and collect overhead distillate; Open tower bottom valve mouth and collect the tower bottom flow fluid; Every thief hole sampling at the bottom of cat head and the tower in 5 minutes, detect and form content, wait to form stablize 1 hour after, detect from 5 body of the tower thief holes samplings, each got sample in 15 minutes one time then, averaged.
Example 2: basic identical with example 1, setting the ethylene glycol feed flow rates is 0.644ml/min, and containing pure waste liquid feed flow rates is 0.279ml/min, and setting reflux ratio is 1 ~ 3.
Example 3: basic identical with example 1, setting reflux ratio is 1.35, and setting the ethylene glycol feed flow rates is 0.4 ~ 0.8ml/min, and containing pure waste liquid feed flow rates is 0.2ml/min.
Claims (3)
1. the method for a continuous extraction rectifying separation alcohol mixture-water is characterized in that, said method comprising the steps of:
(1) the alcohol-water mixture material enters pure water separation column B1 at the bubble point state, and extraction agent is from adding continuously near the cat head position, and the overhead product of B1 tower is ethanol, n-propyl alcohol and isopropylcarbinol, the mixture of extraction solvent and water at the bottom of the tower;
(2) the B1 overhead product enters ethanol recovery tower B2 through interchanger H1 and pump P2, and cat head obtains high purity ethanol; Obtain the mixture of n-propyl alcohol and isopropylcarbinol at the bottom of the tower, enter n-propyl alcohol isopropylcarbinol recovery tower B3 through interchanger H3 and pump P3 again, cat head obtains the high purity n-propyl alcohol, obtains the high purity isopropylcarbinol at the bottom of the tower;
(3) introduce solvent recovery tower B4 by the overhead product that obtains at the bottom of the B1 Tata through interchanger H1 and pump P1, realize the recovery of solvent ethylene glycol, and recycle.
2.. the method for the said a kind of continuous extraction rectifying separation alcohol mixture-water of claim 1 is characterized in that the extraction agent of described extracting rectifying is ethylene glycol, glycol circulation is used in the rectifying.
3. the method for the said a kind of continuous extraction rectifying separation alcohol mixture-water of claim 1 is characterized in that described processing condition are as follows: the B1 tower: total stage number 82, feed tray 60, reflux ratio 1.35; The total stage number 62 of B2 tower, feed tray 32, reflux ratio 2.63; The total stage number 84 of B3 tower, feed tray 40, reflux ratio 4.67; The total stage number 9 of B4 tower, feed tray 5, reflux ratio 0.47.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013100981807A CN103193590A (en) | 2013-03-26 | 2013-03-26 | Method for continuously extracting, rectifying and separating mixed alcohols from water |
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| CN2013100981807A CN103193590A (en) | 2013-03-26 | 2013-03-26 | Method for continuously extracting, rectifying and separating mixed alcohols from water |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104529704A (en) * | 2015-01-22 | 2015-04-22 | 神华集团有限责任公司 | Joint production system and joint production process for synthesizing and separating low-carbon mixed alcohol |
| CN108129266A (en) * | 2017-12-15 | 2018-06-08 | 天津凯赛特科技有限公司 | A kind of process for detaching high-moisture low carbon mixed alcohol |
| CN112250544A (en) * | 2020-10-20 | 2021-01-22 | 西南化工研究设计院有限公司 | Energy-saving process for separating ethanol and water in process of preparing ethylene glycol by diethyl oxalate through hydrogenation |
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|---|---|---|---|---|
| CN101801488A (en) * | 2007-07-13 | 2010-08-11 | Amt国际股份有限公司 | Low-energy extractive distillation process for dehydration of aqueous ethanol |
| CN102060660A (en) * | 2010-12-13 | 2011-05-18 | 上海兖矿能源科技研发有限公司 | Method for separating alcohol compound from Tropsch synthesis reaction water |
| CN102442882A (en) * | 2010-10-12 | 2012-05-09 | 中科合成油技术有限公司 | Separating and recovering method for organic oxygen-containing compounds in Fischer-Tropsch synthesis water phase |
| CN102633597A (en) * | 2012-03-22 | 2012-08-15 | 河北工业大学 | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture |
-
2013
- 2013-03-26 CN CN2013100981807A patent/CN103193590A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101801488A (en) * | 2007-07-13 | 2010-08-11 | Amt国际股份有限公司 | Low-energy extractive distillation process for dehydration of aqueous ethanol |
| CN102442882A (en) * | 2010-10-12 | 2012-05-09 | 中科合成油技术有限公司 | Separating and recovering method for organic oxygen-containing compounds in Fischer-Tropsch synthesis water phase |
| CN102060660A (en) * | 2010-12-13 | 2011-05-18 | 上海兖矿能源科技研发有限公司 | Method for separating alcohol compound from Tropsch synthesis reaction water |
| CN102633597A (en) * | 2012-03-22 | 2012-08-15 | 河北工业大学 | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104529704A (en) * | 2015-01-22 | 2015-04-22 | 神华集团有限责任公司 | Joint production system and joint production process for synthesizing and separating low-carbon mixed alcohol |
| CN108129266A (en) * | 2017-12-15 | 2018-06-08 | 天津凯赛特科技有限公司 | A kind of process for detaching high-moisture low carbon mixed alcohol |
| CN112250544A (en) * | 2020-10-20 | 2021-01-22 | 西南化工研究设计院有限公司 | Energy-saving process for separating ethanol and water in process of preparing ethylene glycol by diethyl oxalate through hydrogenation |
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Application publication date: 20130710 |