CN102992955B - Method for preparing absolute ethanol - Google Patents
Method for preparing absolute ethanol Download PDFInfo
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- CN102992955B CN102992955B CN201310001787.9A CN201310001787A CN102992955B CN 102992955 B CN102992955 B CN 102992955B CN 201310001787 A CN201310001787 A CN 201310001787A CN 102992955 B CN102992955 B CN 102992955B
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Abstract
The invention discloses a method for preparing absolute ethanol. The method includes the following steps: A, ethanol water saturated steam is heated to form ethanol water superheated steam; B, the ethanol water superheated steam is sent into an ethanol dehydration tower to be adsorbed and dehydrated; C, pressure-sharing is performed on the ethanol dehydration tower and a reverse buffer tank; D, an evacuating device is used for evacuating the ethanol dehydration tower so as to complete regeneration of molecular sieve and store a low-concentration ethanol solution; E, the low-concentration ethanol solution is sent in the reverse buffer tank to obtain a middle-temperature ethanol solution; F, the middle-temperature ethanol solution is sent into a rectifying tower to perform rectification so as to obtain high-concentration ethanol water saturated steam; and G, the high-concentration ethanol water saturated steam obtained through rectification is heated to form the ethanol water superheated steam, and the ethanol water superheated steam is sent into the ethanol dehydration tower to be adsorbed and dehydrated. The method for preparing the absolute ethanol has the advantages of being high in efficiency, low in energy consumption, capable of avoiding resource waste and low in heat exchange cost.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of method preparing dehydrated alcohol.
Background technology
Dehydrated alcohol is important organic solvent, is widely used in all respects such as medicine, coating, sanitary product, makeup, grease.Simultaneously, dehydrated alcohol or important basic chemical raw materials, for the manufacture of chemical substances such as acetaldehyde, second diene, ethamine, ethyl acetate, acetic acid, monochloroethane, and deriving many intermediates of the products such as medicine, dyestuff, coating, spices, synthetic rubber, washing composition, agricultural chemicals, its goods reach more than 300 kinds.
Because dehydrated alcohol is widely used, demand is large, how to realize obtaining with higher yield the hot issue that dehydrated alcohol becomes this area research.
Traditional dehydrated alcohol manufacture method has azeotropic distillation, extraction fractional distillation and membrane separation process etc., but these methods all inevitably can bring partial impurities into, and investment is large, energy consumption is high.
Along with the development of Polymer Technology, molecular sieve has very strong avidity with it to high polar molecule gradually, especially to water, also can keep the characteristic of high adsorption rate when low dividing potential drop, lower concentration or high temperature etc. are very harsh, more and more be widely used in the manufacture of raw spirit.
Molecular sieve can lose adsorptive power after water content reaches capacity, and now, the ethanolic soln steam in ethanol dehydration tower cannot obtain adsorption dewatering.In traditional molecular sieve adsorbing and dewatering technique, usually directly discharge after low-concentration ethanol steam residual in ethanol dehydration tower cooling, this causes ethanolic soln to be fully used, and reduces the yield of dehydrated alcohol.Further, cooling low-concentration ethanol steam needs to use a large amount of heat-eliminating mediums, and heat exchange cost is very high.
In addition, traditional molecular sieve adsorbing and dewatering technique, comprise cryogenic absorption and high temperature regeneration two key steps, regeneration temperature is higher than adsorption temp 10 DEG C ~ 50 DEG C, and the main mode vacuumizing and rinse cooperation that adopts makes regenerating molecular sieve.Rinse namely be dehydrated alcohol product is steam heated to higher than the temperature of molecular sieve 10 DEG C ~ 50 DEG C, then the molecular sieve in ethanol dehydration tower is rinsed, water and molecular sieve is impelled to depart from, finally again regeneration is vacuumized to ethanol dehydration tower, vacuum tightness is generally-0.08Mpa ~-0.09Mpa, reaches the object of the residual amount reducing molecular sieve.The shortcoming of this mode is, need to use the dehydrated alcohol product obtained to rinse molecular sieve, after having rinsed, dehydrated alcohol product can be diluted into low-concentration ethanol solution, cause the yield of dehydrated alcohol greatly to reduce, the yield of existing molecular sieve adsorption is between 60% ~ 65%; Need to be steam heated to dehydrated alcohol product higher than the temperature of molecular sieve 10 DEG C ~ 50 DEG C, energy expenditure is large, improves the cost that dehydrated alcohol manufactures.
Summary of the invention
Namely object of the present invention is to overcome the deficiency that the existing molecular sieve adsorbing and dewatering process recovery ratio for dehydrated alcohol is low, energy consumption is high, wasting of resources amount large, heat exchange cost is high, provides a kind of method preparing dehydrated alcohol.
Object of the present invention is achieved through the following technical solutions:
Prepare a method for dehydrated alcohol, comprise the steps:
A. ethanol water saturation steam heating is formed ethanol water superheated vapour;
B. ethanol water superheated vapour is sent into ethanol dehydration tower adsorption dewatering, obtain dehydrated alcohol steam and be adsorbed on the low-concentration ethanol steam in molecular sieve, before water concentration in any one ethanol dehydration tower is saturated, stop sending into ethanol water superheated vapour in this ethanol dehydration tower;
C. ethanol dehydration tower and inverse put surge tank are all pressed, the low-concentration ethanol steam in ethanol dehydration tower flows in inverse put surge tank;
D. vacuum extractor is adopted to vacuumize ethanol dehydration tower, the vacuum tightness in ethanol dehydration tower is kept to be-0.091Mpa ~-0.094Mpa, complete the regeneration of molecular sieve, store after the low-concentration ethanol steam extracted out is cooled to low-concentration ethanol solution in vacuum;
E. the low-concentration ethanol solution that stores in step D is sent in inverse put surge tank with low-concentration ethanol steam heat-exchanging, obtain middle temperature ethanolic soln;
F. ethanolic soln warm in obtaining in step e is sent into rectifying tower rectifying, obtain ethanol water saturation steam;
G., after the ethanol water saturation steam heating obtained in step F being formed ethanol water superheated vapour, ethanol dehydration tower adsorption dewatering is sent into.
Preferably, in described step B, obtain dehydrated alcohol steam extremely liquid through heat exchange, obtain dehydrated alcohol product.
Preferably, the middle temperature ethanolic soln heat exchange obtained in described dehydrated alcohol steam and described step e.
Preferably, in described step B, ethanol dehydration tower internal pressure is 0.1 ~ 2.5Mpa.
Preferably, in described step C, before ethanol dehydration tower and inverse put surge tank are all pressed, be normal pressure in inverse put surge tank.
Preferably, in described step D, the vacuum tightness in ethanol dehydration tower is kept to be-0.091Mpa ~-0.094MPa.
Preferably, in described step e, low-concentration ethanol solution is sent in inverse put surge tank by the mode of spraying.
Preferably, in described steps A, the temperature of ethanol water superheated vapour is 115 DEG C ~ 135 DEG C, in described step G, and the temperature of ethanol water superheated vapour is 115 DEG C ~ 135 DEG C.
Preferably, in described steps A, the mass concentration of ethanol water saturation steam is 90 ~ 99%.
Ethanol dehydration tower and inverse put surge tank are all pressed and are represented that ethanol dehydration tower is communicated with inverse put surge tank, open the valve on ethanol dehydration tower and inverse put surge tank, because the pressure in ethanol dehydration tower is greater than the pressure in inverse put surge tank, ethanolic soln steam in ethanol dehydration tower can flow in inverse put surge tank automatically, realizes the pressure equalization of ethanol dehydration tower and inverse put surge tank inside.
The effect that ethanol dehydration tower and inverse put surge tank are all pressed mainly is to make the low-concentration ethanol steam in ethanol dehydration tower automatically enter inverse put surge tank.This mode can allow follow-up vacuum step extract less low-concentration ethanol steam, improves the efficiency of vacuum step.In addition, the low-concentration ethanol steam extracted due to vacuum step is less, and the heat transferring medium for the cooling of low-concentration ethanol steam is also less, has saved resource.
Applicant is found by research, regenerating molecular sieve is carried out under the condition that vacuum tightness is-0.091Mpa ~-0.094Mpa in ethanol dehydration tower, do not need heating, do not need to rinse, molecular sieve also can obtain good regeneration effect, under the identical recovery time, the residual amount of molecular sieve have dropped 40% ~ 70% than traditional technology.
Applicant is also found by research, and vacuum tightness in ethanol dehydration tower is set as-0.091Mpa ~-0.094Mpa, can balance in acquisition cost and income.Theoretically, the pressure of relative vacuum is-0.1Mpa, and being equivalent to absolute pressure is 0, and this can not reach in practice.To vacuum tightness be remained on higher than-0.094Mpa, need to adopt the component that size is more accurate, material property is more excellent, so production cost has just increased substantially, and the amplification of cost is far longer than the amplification of vacuum tightness index and the cost because of dehydrated alcohol yield raising reduction.Can under the condition at-0.091Mpa ~-0.094Mpa by vacuumizing the holomorphosis realizing molecular sieve when, without the need to further gas clean-up.
Advantage of the present invention and beneficial effect are:
1. reclaim low-concentration ethanol steam and recycle, make use of ethanolic soln to the full extent, improve the yield of dehydrated alcohol, saved resource, cost is low;
2. adopt the low-concentration ethanol solution of cooling to spray low-concentration ethanol steam cooling, the Appropriate application energy of low-concentration ethanol solution itself, energy consumption is low;
3. pair low-concentration ethanol solution vapor step-by-step processing, the low-concentration ethanol steam extracted at vacuum step is less, reduces heat exchange cost, improves and vacuumize efficiency, reduce energy consumption;
4. adopt the middle temperature ethanolic soln in inverse put surge tank to carry out heat exchange to dehydrated alcohol steam, not only dehydrated alcohol steam can be cooled to liquid finished product, also can improve the temperature of liquid ethanol solution self, make it when rectifying without the need to heating up again, achieving making full use of of heat energy;
5. do not need to rinse, only adopt and vacuumize mode molecular sieve is regenerated, the level that the residual amount of molecular sieve can be enable to reach than traditional technology is low by 40% ~ 70%, achieve better regeneration effect, compared to traditional technology, saving the dehydrated alcohol product for rinsing molecular sieve, substantially increasing the yield of dehydrated alcohol, enable the yield of dehydrated alcohol reach 75% ~ 80%;
6., without the need to heating molecular sieve when regenerating molecular sieve, save the energy;
7. eliminate conventional molecular sieve regeneration time for molecular sieve being cooled to the cold blowing step of adsorption temp, save the recovery time, improve production efficiency.
Accompanying drawing explanation
In order to be illustrated more clearly in embodiments of the invention, be briefly described to the accompanying drawing used required for describing in the embodiment of the present invention below.Apparent, the accompanying drawing in the following describes is only some embodiments recorded in the present invention, to those skilled in the art, when not paying creative work, according to accompanying drawing below, can also obtain other accompanying drawing.
Fig. 1 is the structural representation of the dehydrated alcohol manufacturing installation of the embodiment of the present invention 1, embodiment 2 and embodiment 3;
Fig. 2 is the structural representation of the dehydrated alcohol manufacturing installation of the embodiment of the present invention 4.
Wherein, the component title that Reference numeral is corresponding is as follows:
1-ethanol dehydration tower A, 2-ethanol dehydration tower B, 3-vacuum buffer tank, 4-light wine storage tank, 5-vacuum pump, 61-interchanger A, 62-interchanger B, 63-interchanger C, 71-valve A, 72-valve B, 73-valve C, 74-valve D, 75-valve E, 76-valve F, 77-valve G, 78-valve H, 8-inverse put surge tank, 9-squirt pump, 10-rectifying tower, 11-transferpump.
Embodiment
In order to make those skilled in the art understand the present invention better, below in conjunction with the accompanying drawing in the embodiment of the present invention, clear, complete description is carried out to the technical scheme in the embodiment of the present invention.Apparent, embodiment described below is only the part in the embodiment of the present invention, instead of all.Based on the embodiment that the present invention records, other all embodiment that those skilled in the art obtain when not paying creative work, all in the scope of protection of the invention.
Embodiment 1:
As shown in Figure 1, a kind of high yield prepares the technique of dehydrated alcohol, comprises the steps:
A. by mass concentration be 92% ethanol water saturation steam be heated to 115 DEG C by interchanger A61 and form ethanol water superheated vapours.
B. valve A71 and valve E75 is opened, valve-off B72, ethanol water superheated vapour is sent in ethanol dehydration tower A1 and carry out adsorption dewatering, the pressure of ethanol dehydration tower A1 is 0.1Mpa, ethanol water superheated vapour enters from the top of ethanol dehydration tower A1, after adsorption bed, moisture is absorbed by molecular sieve, obtains dehydrated alcohol steam.Open valve E75, released the bottom of dehydrated alcohol steam from ethanol dehydration tower A1, store to normal temperature liquid state through interchanger B62 heat exchange, namely obtain dehydrated alcohol product, the mass concentration of this dehydrated alcohol product is greater than 99.85%.Water concentration in ethanol dehydration tower A1, close to before saturated, stops sending into ethanol water superheated vapour in ethanol dehydration tower A1.
C. inverse put surge tank 8 internal pressure maintenance-0.02MPa, valve-off A71 and valve E75, open valve B72 and valve G77, the inside of ethanol dehydration tower A1 is communicated with the inside of inverse put surge tank 8, because the pressure in inverse put surge tank 8 is less than the pressure in ethanol dehydration tower A1, ethanolic soln steam in ethanol dehydration tower A1 flows in inverse put surge tank 8 automatically, until the internal pressure of ethanol dehydration tower A1 and inverse put surge tank 8 is equal.
D. valve-off A71 and valve E75, open valve B72 and valve H78, temperature in ethanol dehydration tower A1 is maintained 120 DEG C, vacuum pump 5 couples of ethanol dehydration tower A1 are adopted to vacuumize, pumpdown time is 50s, make the vacuum tightness in ethanol dehydration tower A1 remain-0.091Mpa, complete the regeneration of molecular sieve, the residual amount of molecular sieve reduces 43% than traditional technology.When vacuumizing, entering vacuum buffer tank 3 after the low-concentration ethanol steam of extraction is become low-concentration ethanol solution by interchanger C63 heat exchange, entering light wine storage tank 4 subsequently and store.
E. by squirt pump 9 the low-concentration ethanol solution in light wine storage tank 4 sprayed and cool into inverse put surge tank 8 pairs of low-concentration ethanol steam, obtain middle temperature ethanolic soln.
F. by transferpump 11, middle temperature ethanolic soln is sent into rectifying tower 10 rectifying, obtain the ethanol water saturation steam that concentration is higher.
G. the ethanol water saturation steam in step F is sent in ethanol dehydration tower after being heated to 120 DEG C of formation ethanol water superheated vapours by interchanger A61 and is carried out adsorption dewatering.
In the present embodiment, ethanol dehydration tower A1 and ethanol dehydration tower B2 carries out adsorbing and regenerating respectively, and when ethanol dehydration tower A1 is when adsorbing, ethanol dehydration tower B2 is regenerating; When ethanol dehydration tower B2 is when adsorbing, ethanol dehydration tower A1 is regenerating, the continuity of assurance device.
Ethanol dehydration tower B2 carries out adsorbing identical with ethanol dehydration tower A1 with the process regenerated, and ethanol dehydration tower B2 controls the break-make of ethanol dehydration tower B2 and miscellaneous equipment by valve C73, valve D74 and valve F76.
In the present embodiment, the yield of dehydrated alcohol is 98%.
Embodiment 2:
As shown in Figure 1, a kind of high yield prepares the technique of dehydrated alcohol, comprises the steps:
A. by mass concentration be 92% ethanol water saturation steam be heated to 128 DEG C by interchanger A61 and form ethanol water superheated vapours.
B. valve A71 and valve E75 is opened, valve-off B72, ethanol water superheated vapour is sent in ethanol dehydration tower A1 and carry out adsorption dewatering, the pressure of ethanol dehydration tower A1 is 1.7Mpa, ethanol water superheated vapour enters from the top of ethanol dehydration tower A1, after adsorption bed, moisture is absorbed by molecular sieve, obtains dehydrated alcohol steam.Open valve E75, released the bottom of dehydrated alcohol steam from ethanol dehydration tower A1, store to normal temperature liquid state through interchanger B62 heat exchange, namely obtain dehydrated alcohol product, the mass concentration of this dehydrated alcohol product is greater than 99.85%.Water concentration in ethanol dehydration tower A1, close to before saturated, stops sending into ethanol water superheated vapour in ethanol dehydration tower A1.
C. inverse put surge tank 8 internal pressure keeps 0.02MPa, valve-off A71 and valve E75, open valve B72 and valve G77, the inside of ethanol dehydration tower A1 is communicated with the inside of inverse put surge tank 8, because the pressure in inverse put surge tank 8 is less than the pressure in ethanol dehydration tower A1, ethanolic soln steam in ethanol dehydration tower A1 flows in inverse put surge tank 8 automatically, until the internal pressure of ethanol dehydration tower A1 and inverse put surge tank 8 is equal.
D. valve-off A71 and valve E75, open valve B72 and valve H78, temperature in ethanol dehydration tower A1 is maintained 128 DEG C, vacuum pump 5 couples of ethanol dehydration tower A1 are adopted to vacuumize, pumpdown time is 50s, make the vacuum tightness in ethanol dehydration tower A1 remain-0.093Mpa, complete the regeneration of molecular sieve, the residual amount of molecular sieve reduces 68% than traditional technology.When vacuumizing, entering vacuum buffer tank 3 after the low-concentration ethanol steam of extraction is become low-concentration ethanol solution by interchanger C63 heat exchange, entering light wine storage tank 4 subsequently and store.
E. by squirt pump 9 the low-concentration ethanol solution in light wine storage tank 4 sprayed and cool into inverse put surge tank 8 pairs of low-concentration ethanol steam, obtain middle temperature ethanolic soln.
F. by transferpump 11, middle temperature ethanolic soln is sent into rectifying tower 10 rectifying, obtain the ethanol water saturation steam that concentration is higher.
G. the ethanol water saturation steam in step F is sent into ethanol dehydration tower after being heated to 128 DEG C of formation ethanol water superheated vapours by interchanger A61 and is carried out adsorption dewatering.
In the present embodiment, ethanol dehydration tower A1 and ethanol dehydration tower B2 carries out adsorbing and regenerating respectively, and when ethanol dehydration tower A1 is when adsorbing, ethanol dehydration tower B2 is regenerating; When ethanol dehydration tower B2 is when adsorbing, ethanol dehydration tower A1 is regenerating, the continuity of assurance device.
Ethanol dehydration tower B2 carries out adsorbing identical with ethanol dehydration tower A1 with the process regenerated, and ethanol dehydration tower B2 controls the break-make of ethanol dehydration tower B2 and miscellaneous equipment by valve C73, valve D74 and valve F76.
In the present embodiment, the yield of dehydrated alcohol is 99.2%.
Embodiment 3:
As shown in Figure 1, a kind of high yield prepares the technique of dehydrated alcohol, comprises the steps:
A. by mass concentration be 92% ethanol water saturation steam be heated to 135 DEG C by interchanger A61 and form ethanol water superheated vapours.
B. valve A71 and valve E75 is opened, valve-off B72, ethanol water superheated vapour is sent in ethanol dehydration tower A1 and carry out adsorption dewatering, the pressure of ethanol dehydration tower A1 is 2.5Mpa, ethanol water superheated vapour enters from the top of ethanol dehydration tower A1, after adsorption bed, moisture is absorbed by molecular sieve, obtains dehydrated alcohol steam.Open valve E75, released the bottom of dehydrated alcohol steam from ethanol dehydration tower A1, store to normal temperature liquid state through interchanger B62 heat exchange, namely obtain dehydrated alcohol product, the mass concentration of this dehydrated alcohol product is greater than 99.85%.Water concentration in ethanol dehydration tower A1, close to before saturated, stops sending into ethanol water superheated vapour in ethanol dehydration tower A1.
C. inverse put surge tank 8 internal pressure keeps 0.05MPa, valve-off A71 and valve E75, open valve B72 and valve G77, the inside of ethanol dehydration tower A1 is communicated with the inside of inverse put surge tank 8, because the pressure in inverse put surge tank 8 is less than the pressure in ethanol dehydration tower A1, ethanolic soln steam in ethanol dehydration tower A1 flows in inverse put surge tank 8 automatically, until the internal pressure of ethanol dehydration tower A1 and inverse put surge tank 8 is equal.
D. valve-off A71 and valve E75, open valve B72 and valve H78, temperature in ethanol dehydration tower A1 is maintained 135 DEG C, vacuum pump 5 couples of ethanol dehydration tower A1 are adopted to vacuumize, pumpdown time is 50s, make the vacuum tightness in ethanol dehydration tower A1 remain-0.094Mpa, complete the regeneration of molecular sieve, the residual amount of molecular sieve reduces 68% than traditional technology.When vacuumizing, entering vacuum buffer tank 3 after the low-concentration ethanol steam of extraction is become low-concentration ethanol solution by interchanger C63 heat exchange, entering light wine storage tank 4 subsequently and store.
E. by squirt pump 9 the low-concentration ethanol solution in light wine storage tank 4 sprayed and cool into inverse put surge tank 8 pairs of low-concentration ethanol steam, obtain middle temperature ethanolic soln.
F. by transferpump 11, middle temperature ethanolic soln is sent into rectifying tower 10 rectifying, obtain the ethanol water saturation steam that concentration is higher.
G. the ethanol water saturation steam in step F sends into ethanol dehydration tower A1 after being heated to 135 DEG C of formation ethanol superheated vapours by interchanger A61 and ethanol dehydration tower B2 carries out adsorption dewatering.
In the present embodiment, ethanol dehydration tower A1 and ethanol dehydration tower B2 carries out adsorbing and regenerating respectively, and when ethanol dehydration tower A1 is when adsorbing, ethanol dehydration tower B2 is regenerating; When ethanol dehydration tower B2 is when adsorbing, ethanol dehydration tower A1 is regenerating, the continuity of assurance device.
Ethanol dehydration tower B2 carries out adsorbing identical with ethanol dehydration tower A1 with the process regenerated, and ethanol dehydration tower B2 controls the break-make of ethanol dehydration tower B2 and miscellaneous equipment by valve C73, valve D74 and valve F76.
In the present embodiment, the yield of dehydrated alcohol is 99.2%.
Embodiment 4:
As shown in Figure 2, a kind of high yield prepares the technique of dehydrated alcohol, comprises the steps:
A. by mass concentration be 92% ethanol water saturation steam be heated to 128 DEG C by interchanger A61 and form ethanol water superheated vapours.
B. valve A71 and valve E75 is opened, valve-off B72, ethanol water superheated vapour is sent in ethanol dehydration tower A1 and carry out adsorption dewatering, the pressure of ethanol dehydration tower A1 is 1.7Mpa, ethanol water superheated vapour enters from the top of ethanol dehydration tower A1, after adsorption bed, moisture is absorbed by molecular sieve, obtains dehydrated alcohol steam.Open valve E75, released the bottom of dehydrated alcohol steam from ethanol dehydration tower A1, store to normal temperature liquid state through interchanger B62 heat exchange, namely obtain dehydrated alcohol product, the mass concentration of this dehydrated alcohol product is greater than 99.85%.Water concentration in ethanol dehydration tower A1, close to before saturated, stops sending into ethanol water superheated vapour in ethanol dehydration tower A1.
C. inverse put surge tank 8 internal pressure keeps 0.05MPa, valve-off A71 and valve E75, open valve B72 and valve G77, the inside of ethanol dehydration tower A1 is communicated with the inside of inverse put surge tank 8, because the pressure in inverse put surge tank 8 is less than the pressure in ethanol dehydration tower A1, ethanolic soln steam in ethanol dehydration tower A1 flows in inverse put surge tank 8 automatically, until the internal pressure of ethanol dehydration tower A1 and inverse put surge tank 8 is equal.
D. valve-off A71 and valve E75, open valve B72 and valve H78, temperature in ethanol dehydration tower A1 is maintained 128 DEG C, vacuum pump 5 couples of ethanol dehydration tower A1 are adopted to vacuumize, pumpdown time is 50s, make the vacuum tightness in ethanol dehydration tower A1 remain-0.093Mpa, complete the regeneration of molecular sieve, the residual amount of molecular sieve reduces 68% than traditional technology.When vacuumizing, entering vacuum buffer tank 3 after the low-concentration ethanol steam of extraction is become low-concentration ethanol solution by interchanger C63 heat exchange, entering light wine storage tank 4 subsequently and store.
E. by squirt pump 9 the low-concentration ethanol solution in light wine storage tank 4 sprayed and cool into inverse put surge tank 8 pairs of low-concentration ethanol steam, obtain middle temperature ethanolic soln.
F. by transferpump 11, middle temperature ethanolic soln is sent into rectifying tower 10 rectifying by interchanger B62, obtain the aqueous ethanolic solution that concentration is higher.Middle temperature ethanolic soln in interchanger B62 with the dehydrated alcohol steam heat-exchanging in step B, make dehydrated alcohol steam be cooled to liquid state, obtain dehydrated alcohol product, and the temperature of warm ethanolic soln in promoting.
G. the ethanol water saturation steam in step F is sent into ethanol dehydration tower after being heated to 128 DEG C of formation ethanol water superheated vapours by interchanger A61 and is carried out adsorption dewatering.
In the present embodiment, ethanol dehydration tower A1 and ethanol dehydration tower B2 carries out adsorbing and regenerating respectively, and when ethanol dehydration tower A1 is when adsorbing, ethanol dehydration tower B2 is regenerating; When ethanol dehydration tower B2 is when adsorbing, ethanol dehydration tower A1 is regenerating, the continuity of assurance device.
Ethanol dehydration tower B2 carries out adsorbing identical with ethanol dehydration tower A1 with the process regenerated, and ethanol dehydration tower B2 controls the break-make of ethanol dehydration tower B2 and miscellaneous equipment by valve C73, valve D74 and valve F76.
In the present embodiment, the yield of dehydrated alcohol is 99.2%.
It should be noted that, the common practise being measured as those skilled in the art of the residual amount of molecular sieve, repeats no more herein.
Pumpdown time can set according to practical situation, and the pumpdown time is longer, and the residual amount of molecular sieve is lower.
As mentioned above, just the present invention can be realized preferably.
Claims (3)
1. high yield prepares a technique for dehydrated alcohol, it is characterized in that, comprises the steps:
A. be that the ethanol water saturation steam of 92% is by interchanger A(61 by mass concentration) be heated to 128 DEG C of formation ethanol water superheated vapours;
B. valve A(71 is opened) and valve E(75), valve-off B(72), ethanol water superheated vapour is sent into ethanol dehydration tower A(1) in carry out adsorption dewatering, ethanol dehydration tower A(1) pressure be 1.7Mpa, ethanol water superheated vapour is from ethanol dehydration tower A(1) top enter, after adsorption bed, moisture is absorbed by molecular sieve, obtains dehydrated alcohol steam;
Open valve E(75), by dehydrated alcohol steam from ethanol dehydration tower A(1) bottom release, through interchanger B(62) heat exchange stores to normal temperature liquid state, obtains dehydrated alcohol product;
At ethanol dehydration tower A(1) in water concentration close to before saturated, stop to ethanol dehydration tower A(1) in send into ethanol water superheated vapour;
C. inverse put surge tank (8) internal pressure keeps 0.02MPa, valve-off A(71) and valve E(75), open valve B(72) and valve G(77), ethanol dehydration tower A(1) inside be communicated with the inside of inverse put surge tank (8), ethanol dehydration tower A(1) in ethanolic soln steam automatically flow in inverse put surge tank (8), until ethanol dehydration tower A(1) equal with the internal pressure of inverse put surge tank (8);
D. valve-off A(71) and valve E(75), open valve B(72) and valve H(78), by ethanol dehydration tower A(1) in temperature maintain 128 DEG C, adopt vacuum pump (5) to ethanol dehydration tower A(1) vacuumize, pumpdown time is 50s, make ethanol dehydration tower A(1) in vacuum tightness remain-0.093Mpa, complete the regeneration of molecular sieve;
When vacuumizing, the low-concentration ethanol steam of extraction is by interchanger C(63) heat exchange enters vacuum buffer tank (3) after becoming low-concentration ethanol solution, and enter light wine storage tank (4) subsequently and store;
E. by squirt pump (9) the low-concentration ethanol solution in light wine storage tank (4) sprayed and into inverse put surge tank (8), low-concentration ethanol steam is cooled, obtain middle temperature ethanolic soln;
F. by transferpump (11), middle temperature ethanolic soln is sent into rectifying tower (10) rectifying, obtain the ethanol water saturation steam that concentration is higher;
G. the ethanol water saturation steam in step F is by interchanger A(61) be heated to 128 DEG C form ethanol water superheated vapours after send in ethanol dehydration tower and carry out adsorption dewatering;
In above-mentioned steps, as ethanol dehydration tower A(1) when adsorbing, ethanol dehydration tower B(2) regenerating, as ethanol dehydration tower B(2) when adsorbing, ethanol dehydration tower A(1) regenerating; Ethanol dehydration tower B(2) carry out adsorbing and the process regenerated and ethanol dehydration tower A(1) identical, ethanol dehydration tower B(2) by valve C(73), valve D(74) and valve F(76) control ethanol dehydration tower B(2) with the break-make of miscellaneous equipment.
2. high yield prepares a technique for dehydrated alcohol, it is characterized in that, comprises the steps:
A. be that the ethanol water saturation steam of 92% is by interchanger A(61 by mass concentration) be heated to 135 DEG C of formation ethanol water superheated vapours;
B. valve A(71 is opened) and valve E(75), valve-off B(72), ethanol water superheated vapour is sent into ethanol dehydration tower A(1) in carry out adsorption dewatering, ethanol dehydration tower A(1) pressure be 2.5Mpa, ethanol water superheated vapour is from ethanol dehydration tower A(1) top enter, after adsorption bed, moisture is absorbed by molecular sieve, obtains dehydrated alcohol steam;
Open valve E(75), by dehydrated alcohol steam from ethanol dehydration tower A(1) bottom release, through interchanger B(62) heat exchange stores to normal temperature liquid state, obtains dehydrated alcohol product;
At ethanol dehydration tower A(1) in water concentration close to before saturated, stop to ethanol dehydration tower A(1) in send into ethanol water superheated vapour;
C. inverse put surge tank (8) internal pressure keeps 0.05MPa, valve-off A(71) and valve E(75), open valve B(72) and valve G(77), ethanol dehydration tower A(1) inside be communicated with the inside of inverse put surge tank (8), ethanol dehydration tower A(1) in ethanolic soln steam automatically flow in inverse put surge tank (8), until ethanol dehydration tower A(1) equal with the internal pressure of inverse put surge tank (8);
D. valve-off A(71) and valve E(75), open valve B(72) and valve H(78), by ethanol dehydration tower A(1) in temperature maintain 135 DEG C, adopt vacuum pump (5) to ethanol dehydration tower A(1) vacuumize, pumpdown time is 50s, make ethanol dehydration tower A(1) in vacuum tightness remain-0.094Mpa, complete the regeneration of molecular sieve;
When vacuumizing, the low-concentration ethanol steam of extraction is by interchanger C(63) heat exchange enters vacuum buffer tank (3) after becoming low-concentration ethanol solution, and enter light wine storage tank (4) subsequently and store;
E. by squirt pump (9) the low-concentration ethanol solution in light wine storage tank (4) sprayed and into inverse put surge tank (8), low-concentration ethanol steam is cooled, obtain middle temperature ethanolic soln;
F. by transferpump (11), middle temperature ethanolic soln is sent into rectifying tower (10) rectifying, obtain the ethanol water saturation steam that concentration is higher;
G. the ethanol water saturation steam in step F is by interchanger A(61) be heated to 135 DEG C form ethanol water superheated vapours after send in ethanol dehydration tower and carry out adsorption dewatering;
In above-mentioned steps, as ethanol dehydration tower A(1) when adsorbing, ethanol dehydration tower B(2) regenerating, as ethanol dehydration tower B(2) when adsorbing, ethanol dehydration tower A(1) regenerating; Ethanol dehydration tower B(2) carry out adsorbing and the process regenerated and ethanol dehydration tower A(1) identical, ethanol dehydration tower B(2) by valve C(73), valve D(74) and valve F(76) control ethanol dehydration tower B(2) with the break-make of miscellaneous equipment.
3. high yield prepares a technique for dehydrated alcohol, it is characterized in that, comprises the steps:
A. be that the ethanol water saturation steam of 92% is by interchanger A(61 by mass concentration) be heated to 128 DEG C of formation ethanol water superheated vapours;
B. valve A(71 is opened) and valve E(75), valve-off B(72), ethanol water superheated vapour is sent into ethanol dehydration tower A(1) in carry out adsorption dewatering, ethanol dehydration tower A(1) pressure be 1.7Mpa, ethanol water superheated vapour is from ethanol dehydration tower A(1) top enter, after adsorption bed, moisture is absorbed by molecular sieve, obtains dehydrated alcohol steam;
Open valve E(75), by dehydrated alcohol steam from ethanol dehydration tower A(1) bottom release, through interchanger B(62) heat exchange stores to normal temperature liquid state, namely obtains dehydrated alcohol product;
At ethanol dehydration tower A(1) in water concentration close to before saturated, stop to ethanol dehydration tower A(1) in send into ethanol water superheated vapour;
C. inverse put surge tank (8) internal pressure keeps 0.05MPa, valve-off A(71) and valve E(75), open valve B(72) and valve G(77), ethanol dehydration tower A(1) inside be communicated with the inside of inverse put surge tank (8), ethanol dehydration tower A(1) in ethanolic soln steam automatically flow in inverse put surge tank (8), until ethanol dehydration tower A(1) equal with the internal pressure of inverse put surge tank (8);
D. valve-off A(71) and valve E(75), open valve B(72) and valve H(78), by ethanol dehydration tower A(1) in temperature maintain 128 DEG C, adopt vacuum pump (5) to ethanol dehydration tower A(1) vacuumize, pumpdown time is 50s, make ethanol dehydration tower A(1) in vacuum tightness remain-0.093Mpa, complete the regeneration of molecular sieve;
When vacuumizing, the low-concentration ethanol steam of extraction is by interchanger C(63) heat exchange enters vacuum buffer tank (3) after becoming low-concentration ethanol solution, and enter light wine storage tank (4) subsequently and store;
E. by squirt pump (9) the low-concentration ethanol solution in light wine storage tank (4) sprayed and into inverse put surge tank (8), low-concentration ethanol steam is cooled, obtain middle temperature ethanolic soln;
F. by transferpump (11), middle temperature ethanolic soln is passed through interchanger B(62) send into rectifying tower (10) rectifying, obtain the aqueous ethanolic solution that concentration is higher;
Middle temperature ethanolic soln is at interchanger B(62) in the dehydrated alcohol steam heat-exchanging in step B, make dehydrated alcohol steam be cooled to liquid state, obtain dehydrated alcohol product, and the temperature of warm ethanolic soln in promoting;
G. the ethanol water saturation steam in step F is by interchanger A(61) be heated to 128 DEG C form ethanol water superheated vapours after send into ethanol dehydration tower and carry out adsorption dewatering;
In above-mentioned steps, as ethanol dehydration tower A(1) when adsorbing, ethanol dehydration tower B(2) regenerating, as ethanol dehydration tower B(2) when adsorbing, ethanol dehydration tower A(1) regenerating; Ethanol dehydration tower B(2) carry out adsorbing and the process regenerated and ethanol dehydration tower A(1) identical, ethanol dehydration tower B(2) by valve C(73), valve D(74) and valve F(76) control ethanol dehydration tower B(2) with the break-make of miscellaneous equipment.
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| CN105602834A (en) * | 2016-01-26 | 2016-05-25 | 柳州易农科技有限公司 | Absolute ethyl alcohol production device |
| CN105622341A (en) * | 2016-01-26 | 2016-06-01 | 柳州易农科技有限公司 | Continuous production equipment for absolute alcohol |
| CN105602845A (en) * | 2016-01-26 | 2016-05-25 | 柳州易农科技有限公司 | Device for increasing recovery rate of ethanol |
| CN105543086A (en) * | 2016-01-26 | 2016-05-04 | 柳州易农科技有限公司 | Equipment for producing ethanol |
| CN107602349A (en) * | 2017-09-18 | 2018-01-19 | 唐山中溶科技有限公司 | A kind of alcohol production continuous dehydration method and its device |
| CN114163304A (en) * | 2021-12-10 | 2022-03-11 | 四川天采科技有限责任公司 | Adsorption distillation separation and purification method of tower-type ethanol steam moving bed |
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| CN1348942A (en) * | 2001-06-21 | 2002-05-15 | 北京迈胜普技术有限公司 | Molecular sieve adsorbing and dewatering process of producing absolute alcohol |
| CN1733666A (en) * | 2005-09-02 | 2006-02-15 | 钟娅玲 | Multiple adsorption tower alternate internal recycle method for producing anhydrous alcohol |
| CN102351644A (en) * | 2011-08-19 | 2012-02-15 | 天津大学 | Method and device for molecular sieve compound rectifying and refining ethanol product from biobutanol apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1348942A (en) * | 2001-06-21 | 2002-05-15 | 北京迈胜普技术有限公司 | Molecular sieve adsorbing and dewatering process of producing absolute alcohol |
| CN1733666A (en) * | 2005-09-02 | 2006-02-15 | 钟娅玲 | Multiple adsorption tower alternate internal recycle method for producing anhydrous alcohol |
| CN102351644A (en) * | 2011-08-19 | 2012-02-15 | 天津大学 | Method and device for molecular sieve compound rectifying and refining ethanol product from biobutanol apparatus |
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