CN103044194A - Method for separating alcohol and water mixture through extraction and rectification - Google Patents
Method for separating alcohol and water mixture through extraction and rectification Download PDFInfo
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- CN103044194A CN103044194A CN2012105497702A CN201210549770A CN103044194A CN 103044194 A CN103044194 A CN 103044194A CN 2012105497702 A CN2012105497702 A CN 2012105497702A CN 201210549770 A CN201210549770 A CN 201210549770A CN 103044194 A CN103044194 A CN 103044194A
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Abstract
The invention discloses a method for separating alcohol and water mixture through extraction and rectification, and relates to an alcohol and water separation method. The method comprises the following processes: alcohol and water mixed materials enter an alcohol and water separation tower B1, while an extraction agent is continuously added from a position close to the tower top, distillate of the tower top of the tower B1 is controlled to be alcohol, normal propyl alcohol and isobutanol, and then the distillate enters an alcohol recovery tower B2; water and the extraction agent are led into a solvent recovery tower B4 from the tower bottom of the tower B1; mixture of the normal propyl alcohol and the isobutanol obtained from the tower bottom enters a normal propyl alcohol and isobutanol recovery tower B3 via a heat exchanger H3 and a pump P3; and distillate obtained from the tower bottom of the tower B1 is led into a solvent recovery tower B4 via a heat exchanger H1 and a pump P1. According to the invention, the extraction agent is adopted to break the azeotropy of alcohol and water, the mixture of multiple alcohols and water is well separated, and a high-purity product is obtained, while the separation effect is good, the production cost is lowered, materials can be utilized again, and the operation and control are easy, so that the method is suitable for large-scale separation processes.
Description
Technical field
The present invention relates to a kind of pure water separating method, particularly relate to a kind of method of utilizing the separation of extractive distillation alcohol-water mixture.
Background technology
Day by day exhaustion along with petroleum resources, the future source of energy structure will turn to take coal and Sweet natural gas as main, produce as an alternative fuel of preparing low-carbon mixed alcohol by synthetic gas by Sweet natural gas or gasification, more and more be subject to people's attention, for lacking the country of petroleum resources, shown that people can pass through non-oil resource, generated synthetic gas such as the gasification of coal and Sweet natural gas etc. and come suitability for industrialized production low-carbon alcohol fuel.Yet prepare in the technique of low-carbon alcohol at synthetic gas, what inevitably produce a large amount of contains pure waste liquid, from wherein reclaiming alcohols Sustainable development and environment protection is had great significance.
Catalyzing carbon monoxide is hydrogenated into the important channel into the production mixture of lower alcohols in recent years, but its side reaction meeting produces a large amount of alcohol-water mixtures.Mixture of lower alcohols generally refers to (C1-C5) alcohols mixture, can directly mix gasoline and make motor spirit.Also can obtain mixture of lower alcohols in the alcohol production process, mainly be the mixing system of methyl alcohol, second alcohol and water.
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, and sums up to mainly contain the following aspects:
(1) as alternative fuel: although the mixture of lower alcohols calorific value a little less than vapour, diesel oil, owing to the existence of oxygen in the alcohol, its ratio of combustion vapour, diesel oil are abundant; CO, NOx and hydro carbons quantity discharged are few in the tail gas, are environmental friendliness fuel; Directly as automotive fuel, its realistic meaning can not be underestimated if overcome problem mechanically.
(2) clean gasoline additive: research is found, the MTBE(methyl tertiary butyl ether) there is serious problem as gasoline dope, as being easy to leakage and polluted drinking water etc. in storage, transportation and the use procedure, threaten human health; Although the use of MTBE still can continue for some time.But final forbidding is a matter of time just.This Application and Development for mixture of lower alcohols provides huge development opportunity; Mixture of lower alcohols has very high octane value, and it is explosion-proof, anti-seismic performance is superior.Certainly higher alcohols content is higher better with mutual solubility gasoline.
(3) chemical and industrial chemicals: from more profound, the mixture of lower alcohols application prospect is that it is as the immense value of chemical products and large Chemical Manufacture raw material.The Application in Chemical Engineering prospect of mixture of lower alcohols is progressively good in recent years, and mixture of lower alcohols can obtain the higher alcohols of price such as second, third, fourth, amylalcohol through separating, and alleviates the problem of short industrial chemicals on the domestic market.
(4) other application of mixture of lower alcohols comprise: as one of means of gelatin liquefaction, realize alkylation and solubilization and the effectively transportation of coal.As liquefied petroleum gas (LPG) (LPG) surrogate; Directly reach as general chemical solvents and be used for efficient power generation etc.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing the separation of extractive distillation alcohol-water mixture, the present invention adopts extraction agent to break the azeotropic of alcohol-water, has separated the mixture of polyvalent alcohol and water, obtains the product of higher degree, material is utilized again, operate easily and control.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of utilizing the separation of extractive distillation alcohol-water mixture, described method comprises following process: the alcohol-water mixture material enters pure water separation column B1 at the bubble point state, extraction agent is from adding continuously near the cat head position simultaneously, the overhead product of control B1 tower is ethanol, n-propyl alcohol and isopropylcarbinol, enters afterwards ethanol recovery tower B2; Water and extraction agent ethylene glycol are introduced solvent recovery tower B4 at the bottom of the B1 Tata, realize the recycling of solvent ethylene glycol; Overhead product by tower B1 enters ethanol recovery tower B2 through interchanger H1 and pump P2, and cat head obtains high purity ethanol; The mixture that obtains n-propyl alcohol and isopropylcarbinol at the bottom of the tower enters n-propyl alcohol isopropylcarbinol recovery tower B3 through interchanger H3 and pump P3 again, and cat head obtains the high purity n-propyl alcohol, obtains the high purity isopropylcarbinol at the bottom of the tower; 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 solvent recuperation; Finish distillation operation in the tower for guaranteeing that the stream thigh can enter, the operation pressure of stream thigh is higher than the pressure that enters column plate, and keeps hot state, therefore control at technical process adding pump P and valve V, and be set unified charging standard, and pressure is 1.2atm, drop temperature is 80 ℃.
Described a kind of method of utilizing the separation of extractive distillation alcohol-water mixture, described Recycled ethanol, n-propyl alcohol, isopropylcarbinol contain high purity product.
Described a kind of method of utilizing the separation of extractive distillation alcohol-water mixture, described stage number is set to 82, and feed entrance point is chosen in tower middle part charging, and the extractant feed position is near the column plate of cat head, and the reflux ratio variation range is 1～5.
Described a kind of method of utilizing the separation of extractive distillation alcohol-water mixture, described B1 is extractive distillation column, B2, B3, B4 are common rectifying tower.
Advantage of the present invention and effect are:
The present invention adopts extraction agent to break the azeotropic of alcohol-water, and has better separated the mixture of polyvalent alcohol and water, obtains the product of higher degree, good separating effect reduces production costs, and material is utilized again, operation and control are fit to extensive sepn process easily.
Description of drawings
Fig. 1 is the process flow sheet that utilizes the separation of extractive distillation alcohol-water mixture.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
Raw material of the present invention enters extractive distillation column with B1 tower middle part in proportion, and extraction agent ethylene glycol is by entering near the top of tower position.B1 bottom product flow rate is controlled by valve, enters into the B4 common rectifying tower through pump, and the B4 bottom product is that extraction agent joins in the B1 tower again, realizes the recycle of solvent.B1 cat head partial reflux, reflux ratio 1～5, product flowrate is controlled by valve, enters into the B2 common rectifying tower through pump.The B2 bottom product enters into the B3 common rectifying tower by valve and pump control.
Embodiment one, and 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 simultaneously, and the overhead product of control B1 tower is ethanol, n-propyl alcohol and isopropylcarbinol, enters afterwards ethanol recovery tower B2; Water and extraction agent (ethylene glycol) are introduced solvent recovery tower B4 at the bottom of the B1 Tata, realize the recycling of solvent ethylene glycol.Overhead product by tower B1 enters ethanol recovery tower B2 through interchanger H1 and pump P2, and cat head obtains high purity ethanol.The mixture that obtains n-propyl alcohol and isopropylcarbinol at the bottom of the tower enters n-propyl alcohol isopropylcarbinol recovery tower B3 through interchanger H3 and pump P3 again, and cat head obtains the high purity n-propyl alcohol, obtains the high purity isopropylcarbinol at the bottom of the tower.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 solvent recuperation.More than each processing parameter see Table 1～3.
The composition of table 1 incoming flow thigh F
| Component | Flow (kg/sec) | Quality percentage composition % |
| Ethanol | 3.979 | 39．79 |
| N-propyl alcohol | 1.887 | 18．87 |
| Isopropylcarbinol | 1.623 | 16．23 |
| Water | 2.511 | 25．11 |
Each tower process parameter of table 2
| Tower | Total stage number | Feed tray | Reflux ratio | The solvent feed position |
| B1 | 82 | 60 | 1.35 | 3 |
| B2 | 62 | 32 | 2 | \ |
| B3 | 84 | 40 | 4 | \ |
| B4 | 9 | 5 | 1 | \ |
Product purity and the rate of recovery of each component after table 3 is optimized
| Component | Purity | The rate of recovery |
| Ethanol | 99.56% | 100% |
| N-propyl alcohol | 99.45% | 99.43% |
| Isopropylcarbinol | 99.43% | 99.36% |
| Water | 99.77% | 99.50% |
| Ethylene glycol | 99.99% | 99.96% |
Embodiment two, and is basic identical with embodiment one, but the reflux ratio of described B2 rectifying tower is 2.49, and it is higher to obtain in the product purity of alcohol, and the ethanol rate of recovery is higher.
Embodiment three, and is basic identical with embodiment one, but the reflux ratio of described B3 rectifying tower is 5.04, and it is higher to obtain in the product n-propyl alcohol and isopropylcarbinol purity, and the ethanol rate of recovery is higher.
Embodiment four, and is basic identical with embodiment one, but the reflux ratio of described B4 rectifying tower is 1.26, and it is higher to obtain in the product ethylene glycol purity, and the ethanol rate of recovery is higher.
Claims (4)
1. method of utilizing the separation of extractive distillation alcohol-water mixture, it is characterized in that, described method comprises following process: the alcohol-water mixture material enters pure water separation column B1 at the bubble point state, extraction agent is from adding continuously near the cat head position simultaneously, the overhead product of control B1 tower is ethanol, n-propyl alcohol and isopropylcarbinol, enters afterwards ethanol recovery tower B2; Water and extraction agent ethylene glycol are introduced solvent recovery tower B4 at the bottom of the B1 Tata, realize the recycling of solvent ethylene glycol; Overhead product by tower B1 enters ethanol recovery tower B2 through interchanger H1 and pump P2, and cat head obtains high purity ethanol; The mixture that obtains n-propyl alcohol and isopropylcarbinol at the bottom of the tower enters n-propyl alcohol isopropylcarbinol recovery tower B3 through interchanger H3 and pump P3 again, and cat head obtains the high purity n-propyl alcohol, obtains the high purity isopropylcarbinol at the bottom of the tower; 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 solvent recuperation; Finish distillation operation in the tower for guaranteeing that the stream thigh can enter, the operation pressure of stream thigh is higher than the pressure that enters column plate, and keeps hot state, therefore control at technical process adding pump P and valve V, and be set unified charging standard, and pressure is 1.2atm, drop temperature is 80 ℃.
2. a kind of method of utilizing the separation of extractive distillation alcohol-water mixture according to claim 1 is characterized in that, described Recycled ethanol, n-propyl alcohol, isopropylcarbinol contain high purity product.
3. a kind of method of utilizing the separation of extractive distillation alcohol-water mixture according to claim 1, it is characterized in that described stage number is set to 82, feed entrance point is chosen in tower middle part charging, the extractant feed position is near the column plate of cat head, and the reflux ratio variation range is 1～5.
4. a kind of method of utilizing the separation of extractive distillation alcohol-water mixture according to claim 1 is characterized in that, described B1 is extractive distillation column, and B2, B3, B4 are common rectifying tower.
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| CN2012105497702A CN103044194A (en) | 2012-12-18 | 2012-12-18 | Method for separating alcohol and water mixture through extraction and rectification |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981695A (en) * | 2019-12-13 | 2020-04-10 | 中能达(西安)再生资源股份有限公司 | Alcohol mixing and extracting method |
| CN115073270A (en) * | 2022-05-12 | 2022-09-20 | 山东昆达生物科技有限公司 | Continuous azeotropic extraction and rectification method for separating low-carbon polyol-water mixture |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4559109A (en) * | 1983-03-31 | 1985-12-17 | Phillips Petroleum Company | Dehydration of alcohol with extractive distillation |
| 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 |
| 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 |
-
2012
- 2012-12-18 CN CN2012105497702A patent/CN103044194A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4559109A (en) * | 1983-03-31 | 1985-12-17 | Phillips Petroleum Company | Dehydration of alcohol with extractive distillation |
| 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 |
| 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 |
|---|---|---|---|---|
| CN110981695A (en) * | 2019-12-13 | 2020-04-10 | 中能达(西安)再生资源股份有限公司 | Alcohol mixing and extracting method |
| CN115073270A (en) * | 2022-05-12 | 2022-09-20 | 山东昆达生物科技有限公司 | Continuous azeotropic extraction and rectification method for separating low-carbon polyol-water mixture |
| CN115073270B (en) * | 2022-05-12 | 2024-04-02 | 山东昆达生物科技有限公司 | Continuous azeotropic extractive distillation method for separating low-carbon polyol-water mixture |
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Application publication date: 20130417 |