CN113816834B - Energy-saving rectification-adsorption combined method for preparing high-purity absolute ethyl alcohol - Google Patents
Energy-saving rectification-adsorption combined method for preparing high-purity absolute ethyl alcohol Download PDFInfo
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- CN113816834B CN113816834B CN202111197855.4A CN202111197855A CN113816834B CN 113816834 B CN113816834 B CN 113816834B CN 202111197855 A CN202111197855 A CN 202111197855A CN 113816834 B CN113816834 B CN 113816834B
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- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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Abstract
The invention discloses a method for preparing high-purity absolute ethyl alcohol by combining energy-saving rectification and adsorption, which takes fermented liquor as a raw material, adopts high-efficiency tower plates or fillers with high separation efficiency as mass transfer separation core internals of rectification equipment, and adopts potassium permanganate solution to carry out surface wetting treatment on the surfaces of the fillers; the tower equipment is washed by high-purity absolute ethyl alcohol after pickling and passivation by adopting a mixed solution of nitric acid and hydrofluoric acid; adding nitrate into the molecular sieve, and soaking in absolute ethyl alcohol; feeding the raw material into a degassing tank, feeding the gas into an absorption tower, feeding the absorption liquid and the liquid phase of the degassing tank into a first rectification tower, feeding the side line extract liquid and the tower top material flow of the first rectification tower into a second rectification tower and a third rectification tower respectively, and taking the top gas phase of the second rectification tower and the third rectification tower as heat sources of reboilers of the first rectification tower and the second rectification tower; and (3) feeding the materials at the tops of the second rectifying tower and the third rectifying tower into an adsorption working section, wherein the product ethanol of the adsorption tower is used for preheating the feeding of the adsorption tower. The method has the advantages of high recovery rate and low energy consumption, and ensures the safe and stable operation of the subsequent working section by removing non-condensed steam.
Description
Technical Field
The invention relates to the technical field of chemical material production, in particular to a method for preparing high-purity absolute ethyl alcohol by combining energy-saving rectification and adsorption.
Background
In the present stage, the development of high-purity chemicals is slow, and the urgent demand of the rapid development of the society is difficult to meet. Ethanol is used as an important basic chemical raw material and has important significance in the development history of chemical industry. Except for chemical industry, high-purity absolute ethyl alcohol with high purity is widely applied to cleaning of electronic chips, integrated circuits and precise instruments, but the requirement on the content of metal impurity ions is extremely low, and the requirement on moisture is generally less than 100 ppm. Due to the reasons, the production process of the high-purity absolute ethyl alcohol in China is very complicated, and meanwhile, the energy consumption is extremely high, so that the development of the high-purity absolute ethyl alcohol in China is always restricted.
At present, the domestic production of high-purity absolute ethyl alcohol is mainly carried out by a three-tower three-effect distillation process device. Although the energy consumption of the three-tower triple-effect ethanol process device is low, the three-tower triple-effect ethanol process device is limited by a process route, and has two major defects, namely, the temperature of the bottom of the combined tower is too high to reach about 120 ℃, so that vinasse protein denaturation and feed color blackening are caused, nutrient content is reduced, and the material is easily coked due to too high temperature, so that equipment is blocked, the production device is required to be cleaned frequently, and the shutdown cleaning of the production device also causes great loss; secondly, the top pressure of the combined tower is lower, so that the dehydration effect of alcohol vapor in the tower top to the molecular sieve is poorer. In the period of increasing energy cost at present, with the development of new technology in the ethanol industry, the three-tower three-effect distillation process cannot meet the requirement of high-purity absolute ethanol. In addition, the mass transfer separation efficiency of the internal parts of the tower is low, and the problems of substandard purity, high energy consumption and the like of the high-purity absolute ethyl alcohol can be caused, so that the research and development of a more energy-saving high-purity absolute ethyl alcohol process technology are urgently needed.
Disclosure of Invention
In order to solve the defects in the production process of the high-purity absolute ethyl alcohol, the invention provides an energy-saving separation process for preparing the high-purity absolute ethyl alcohol by combining rectification and adsorption, and an energy-saving process method for producing the high-purity absolute ethyl alcohol from fermented liquor by combining rectification and adsorption.
In order to achieve the purpose, the invention adopts the following technical scheme:
an energy-saving rectification-adsorption combined method for preparing high-purity absolute ethyl alcohol, which adopts a device comprising a degassing tank, an absorption tower, a first rectification tower, a second rectification tower, a third rectification tower, an adsorption tower A and an absorption tower B;
the method comprises the following steps that gas after passing through a degassing tank is sent into an absorption tower, absorption liquid and a liquid phase in the degassing tank are processed by a feeding preheater and then sent into a first rectifying tower, a side line produced liquid of the first rectifying tower is sent into a second rectifying tower, a tower top object is processed by the feeding preheater and a third rectifying tower preheater and then sent into a third rectifying tower, gas phases at the tops of the second rectifying tower and the third rectifying tower are respectively used as heat sources of a first rectifying tower reboiler connected with the first rectifying tower and a second rectifying tower reboiler connected with the second rectifying tower, the side line produced liquid of the second rectifying tower and the third rectifying tower enter an absorption tower A and an absorption tower B through an evaporation heat exchanger for processing, and tower top steam is discharged through the evaporation heat exchanger after the absorption tower A and the absorption tower B resolve alcohol steam to obtain a finished product;
mass transfer separation internals in the first rectification tower, the second rectification tower and the third rectification tower adopt high-efficiency packing or tower plates;
the absorption tower, the first rectification tower, the second rectification tower, the third rectification tower, the adsorption tower A and the absorption tower B are washed by absolute ethyl alcohol after pickling and passivation by nitric acid and hydrofluoric acid;
the molecular sieves in the first rectifying tower, the second rectifying tower and the third rectifying tower are soaked or washed by the absolute ethyl alcohol solution of nitrate.
Preferably, the bottom of the rectifying tower is connected with a rectifying tower auxiliary reboiler.
Preferably, the bottoms of the absorption tower A and the absorption tower B are communicated with a superheater.
Preferably, the operation temperature of the degassing tank is 50-70 ℃, and the pressure is 0.02-0.1 MPa.
Preferably, the concentration of the nitric acid and the hydrofluoric acid is 40-60 wt%, the pickling time is 30-60 min, the washing rate is 0.1-1 m/s, the washing time of the absolute ethyl alcohol is 20-40 min, and the washing rate is 0.5-3 m/s.
Preferably, the surface of the packing is subjected to surface wettability treatment by adopting 1-10 g/ml potassium permanganate solution on the efficient packing or tower plate of mass transfer separation internals in the first rectification tower, the second rectification tower and the third rectification tower.
Preferably, the concentration of the anhydrous ethanol solution of the nitrate is 1-5 g/L, the soaking time is 30-60 min, the washing time is 30-60 min, and the washing speed is 0.1 m/s.
Preferably, the ethanol content of the tops of the second rectifying tower and the third rectifying tower is more than 95% (v/v). The ethanol content after adsorption and dehydration by a molecular sieve is 99.999 wt%.
Preferably, the ratio of the flow rate of the first rectifying tower side line extracted out of the second rectifying tower to the flow rate of the feed is 0.3-0.6.
Preferably, the feeding temperature of the adsorption tower A and the feeding temperature of the adsorption tower B are 100-130 ℃, the pressure is 0.2-0.35 MPa, and the temperature of the evaporation heat exchanger is 120-150 ℃.
According to the technical scheme, compared with the prior art, the invention discloses and provides an energy-saving rectification-adsorption combined method for preparing high-purity absolute ethyl alcohol, which has the following beneficial effects:
overcomes the defects of the prior art, creatively adopts a mode of combining rectification and adsorption to produce the high-purity absolute ethyl alcohol on the basis of a three-tower ethyl alcohol rectification process, and obviously reduces the operation energy consumption. The process method provided by the invention has great practicability and obvious economic benefit.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a diagram of an apparatus used in the energy-saving rectification-adsorption combined method for preparing high-purity absolute ethanol according to the invention;
wherein, the system comprises a degassing tank-1, an absorption tower-2, a first rectification tower-3, a second rectification tower-4, a third rectification tower-5, an adsorption tower A-6, an absorption tower B-7, a feed preheater-8, a first rectification tower auxiliary reboiler-9, a first rectification tower reboiler-10, a second rectification tower reboiler-11, a third rectification tower reboiler-12, a third rectification tower preheater-13, an evaporation heat exchanger-14 and a superheater-15.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in the attached figure 1, the device adopted by the energy-saving rectification-adsorption combined method for preparing high-purity absolute ethyl alcohol comprises a degassing tank 1, an absorption tower 2, a first rectification tower 3, a second rectification tower 4, a third rectification tower 5, an adsorption tower A6 and an absorption tower B7;
after a raw material passes through a degassing tank 1, gas is sent into an absorption tower 2, absorption liquid and a liquid phase in the degassing tank 1 are processed by a feed preheater 8 and then sent into a first rectification tower 3, a side line extracted liquid in the first rectification tower 3 is sent into a second rectification tower 4, tower top materials are processed by the feed preheater 8 and a third rectification tower preheater 13 and then sent into a third rectification tower 5, gas phases at the tops of the second rectification tower 4 and the third rectification tower 5 are respectively used as heat sources of a first rectification tower reboiler 10 connected with the first rectification tower 3 and a second rectification tower reboiler 11 connected with the second rectification tower 4, the side line extracted liquids in the second rectification tower 4 and the third rectification tower 5 enter an absorption tower A6 and an absorption tower B7 through an evaporation heat exchanger 14 for processing, and after the absorption tower A6 and the absorption tower B7 analyze alcohol vapor, the tower top vapor is discharged through the evaporation heat exchanger 14 to obtain a finished product;
mass transfer separation internals in the first rectification tower, the second rectification tower and the third rectification tower adopt high-efficiency packing or tower plates;
the absorption tower 2, the first rectification tower 3, the second rectification tower 4, the third rectification tower 5, the adsorption tower A6 and the absorption tower B7 are washed by nitric acid and hydrofluoric acid through pickling and passivation and then washed by absolute ethyl alcohol;
the molecular sieves in the first rectification tower 3, the second rectification tower 4 and the third rectification tower 5 are soaked or washed by the absolute ethyl alcohol solution of nitrate.
In some specific schemes, a rectification-column auxiliary reboiler 9 is connected to the bottom of the rectification-column 3. The bottoms of the absorption tower A6 and the absorption tower B7 are communicated with a superheater 15.
Wherein the operating temperature of the degassing tank 1 is 50-70 ℃, the pressure is 0.02-0.1 MPa, the concentration of nitric acid and hydrofluoric acid is 40-60 wt%, the acid washing time is 30-60 min, the washing rate is 0.1-1 m/s, the washing time of absolute ethyl alcohol is 20-40 min, the washing rate is 0.5-3 m/s, the high-efficiency packing or column plate of mass transfer separation internals in the first rectifying tower 3, the second rectifying tower 4 and the third rectifying tower 5 adopts 1-10 g/ml potassium permanganate solution to carry out surface wetting treatment on the surface of the packing, the concentration of the absolute ethyl alcohol solution of nitrate is 1-5 g/L, the soaking time is 30-60 min, the washing rate is 0.1m/s, the ethanol content at the tops of the second rectifying tower 4 and the third rectifying tower 5 is more than 95% (v/v), the ethanol content after dehydration by a molecular adsorption sieve is 99.999 wt%, the ratio of the flow rate of a side-draw rectification first tower 3 to the flow rate of a side-draw rectification second tower 4 to the feed flow rate is 0.3-0.6, the feed temperature of the adsorption tower A6 and the feed temperature of the adsorption tower B7 are 100-130 ℃, the pressure is 0.2-0.35 MPa, and the temperature of the evaporative heat exchanger 14 is 120-150 ℃.
The technical scheme of the invention is further explained by taking the fermented mature mash with the feed flow of 80000kg/h as an example:
the volume percentage of ethanol is 12.5 percent, the volume percentage of water and other components is 87.5 percent, and the feeding temperature is 25 ℃.
The fermented mash from the fermentation working section enters a degassing tank to remove a large amount of non-condensed steam, the non-condensed steam is sent to an absorption tower to recover ethanol, and the absorption liquid and the liquid phase of the degassing tank are preheated by a feed preheater and then enter the top of a rectification tower. The heating medium of the mash feeding preheater is that the top gas of the rectifying tower is preheated to 59 ℃, and then the steam condensed water of the heating rectifying tower is firstly sent to the heating rectifying tower for feeding and then sent to the preheating rectifying tower for feeding. And (3) the preheated mash with the temperature of 72 ℃ enters a degassing section at the top of the rectification first tower, and the degassed mash overflows to the top of a stripping section of the rectification first tower after vapor-liquid mass transfer separation.
The mash entering the stripping section of the rectifying tower is subjected to vapor-liquid mass transfer separation, and the concentrated alcohol vapor is discharged from the top of the stripping section of the rectifying tower and respectively enters a mash feeding preheater. There is no backflow under normal operating conditions. And (3) preheating and feeding steam extracted from the tower top, pumping the crude wine in the reflux tank to a three-tower rectification feed preheater through a crude wine extraction pump, feeding the preheated crude wine into the three-tower rectification feed, and controlling the feed amount of the three-tower rectification by the liquid level of the reflux tank. The heating medium of the first preheater of the rectifying tower III is alcohol solution;
crude wine mash with the temperature of 71 ℃ is extracted from the middle side line liquid phase of the first rectifying tower and enters a feeding tank of the rectifying tower, and then is sent to a feeding preheater of a second rectifying tower through a side extracting pump (variable frequency pump) of the first rectifying tower, and is preheated to 100 ℃ to feed the second rectifying tower, a heating medium of the preheater is 160 ℃ alcohol gas generated by a molecular sieve adsorption tower, the heated alcohol is changed into a liquid phase, and the liquid phase is sent to a feeding first preheater of the third rectifying tower to preheat the feeding of the third rectifying tower.
And (4) conveying the tower bottom liquid to a reboiler of the rectification tower through the rectification tower bottom liquid to perform forced circulation, and returning the heated tower bottom liquid to the rectification tower bottom. The heating medium of the rectifying tower reboiler is the tower top alcohol vapor from the rectifying tower and the tower bottom produced liquid. And one part of the alcohol gas at the top of the second rectifying tower is extracted as a product after heat exchange, and the other part of the alcohol gas is taken as reflux of the second rectifying tower. And heating the produced liquid in the tower kettle of the rectification second tower to the boundary region behind the tower kettle of the rectification first tower.
The mass transfer separation core internal part of the rectifying equipment adopted in the industrial implementation is a high-efficiency guide sieve plate, the tower equipment is subjected to acid cleaning and passivation for 45min by adopting a 45% nitric acid and hydrofluoric acid mixed solution in advance, and the molecular sieve is soaked for 50min by adopting a 3g/L nitrate anhydrous ethanol solution.
The process flow is simple and easy to control, and compared with the conventional three-tower rectification process, the energy consumption is reduced by 28.5 percent, and the energy-saving effect is obvious.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. An energy-saving rectification-adsorption combined method for preparing high-purity absolute ethyl alcohol is characterized in that the adopted device comprises a degassing tank, an absorption tower, a first rectification tower, a second rectification tower, a third rectification tower, an adsorption tower A and an absorption tower B;
after the fermented liquor passes through a degassing tank, gas is sent into an absorption tower, the absorption liquid and a liquid phase in the degassing tank are treated by a feed preheater and then sent into a first rectification tower, a side line produced liquid of the first rectification tower is sent into a second rectification tower, a tower top object is treated by the feed preheater and a third rectification tower preheater and then sent into a third rectification tower, gas phases at the tops of the second rectification tower and the third rectification tower are respectively used as heat sources of a first rectification tower reboiler connected with the first rectification tower and a second rectification tower reboiler connected with the second rectification tower, the side line produced liquids of the second rectification tower and the third rectification tower enter an absorption tower A and an absorption tower B through an evaporation heat exchanger for treatment, and after the absorption tower A and the absorption tower B resolve alcohol vapor, the tower top vapor is discharged through the evaporation heat exchanger to obtain a finished product;
mass transfer separation internals in the first rectification tower, the second rectification tower and the third rectification tower adopt high-efficiency packing or tower plates; carrying out surface wettability treatment on the surface of a high-efficiency filler or a tower plate of a mass transfer separation internal member in the first rectification tower, the second rectification tower and the third rectification tower by adopting a potassium permanganate solution of 1-10 g/ml;
the absorption tower, the first rectification tower, the second rectification tower, the third rectification tower, the adsorption tower A and the absorption tower B are washed by absolute ethyl alcohol after pickling and passivation by nitric acid and hydrofluoric acid; the concentration of the nitric acid and the hydrofluoric acid is 40-60 wt%, the pickling time is 30-60 min, the washing rate is 0.1-1 m/s, the washing time of the absolute ethyl alcohol is 20-40 min, and the washing rate is 0.5-3 m/s;
the molecular sieves in the first rectifying tower, the second rectifying tower and the third rectifying tower are soaked or washed by the absolute ethyl alcohol solution of nitrate; the concentration of the anhydrous ethanol solution of the nitrate is 1-5 g/L, the soaking time is 30-60 min, the washing time is 30-60 min, and the washing speed is 0.1 m/s.
2. The energy-saving rectification-adsorption combined method for preparing high-purity absolute ethanol according to claim 1, wherein a rectification-tower auxiliary reboiler is connected to the bottom of the rectification tower.
3. The energy-saving rectification-adsorption combined high-purity absolute ethanol preparation method as claimed in claim 1, wherein the bottoms of the adsorption tower A and the absorption tower B are communicated with a superheater.
4. The energy-saving rectification-adsorption combined method for preparing high-purity absolute ethanol according to claim 1, wherein the degassing tank is operated at 50-70 ℃ and under 0.02-0.1 MPa.
5. The energy-saving rectification-adsorption combined high-purity absolute ethanol preparation method as claimed in claim 1, wherein the ethanol content at the top of the second rectification tower and the third rectification tower is more than 95% (v/v); the ethanol content after adsorption and dehydration by a molecular sieve is 99.999 wt%.
6. The energy-saving rectification-adsorption combined method for preparing high-purity absolute ethanol according to claim 1, wherein the ratio of the flow rate of a first rectification column to the flow rate of a second rectification column is 0.3-0.6.
7. The energy-saving rectification-adsorption combined method for preparing high-purity absolute ethanol according to claim 1, wherein the feeding temperature of the adsorption tower A and the feeding temperature of the absorption tower B are 100-130 ℃, the pressure is 0.2-0.35 MPa, and the temperature of the evaporation heat exchanger is 120-150 ℃.
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| CN114534287A (en) * | 2022-02-13 | 2022-05-27 | 河北首朗新能源科技有限公司 | Distillation degassing device and degassing method |
| CN114712884B (en) * | 2022-06-08 | 2023-01-13 | 北京化工大学 | Device and method for producing electronic grade ethanol by rectification-membrane separation |
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