CN109678668A - A kind of ethyl alcohol-tertiary butanol and water distillation and separation method - Google Patents
A kind of ethyl alcohol-tertiary butanol and water distillation and separation method Download PDFInfo
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- CN109678668A CN109678668A CN201811409585.7A CN201811409585A CN109678668A CN 109678668 A CN109678668 A CN 109678668A CN 201811409585 A CN201811409585 A CN 201811409585A CN 109678668 A CN109678668 A CN 109678668A
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- C—CHEMISTRY; METALLURGY
- 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
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
Abstract
The invention discloses contain ethyl alcohol-tert-butyl alcohol distillation and separation method in a kind of waste water, belong to multicomponent Azeotrope separation field, be intended to provide it is a kind of investment it is small, low energy consumption, three-waste free discharge, the ethyl alcohol of high income-tertiary butanol and water distillation and separation method, its drip irrigation device is as follows, and ethyl alcohol and the tert-butyl alcohol are separated by the waste water containing ethyl alcohol, the tert-butyl alcohol and water after pre-dehydration processing, azeotropic processing, stripping processing, extracting rectifying processing processing, obtain product ethyl alcohol and the tert-butyl alcohol；Entrainer is added in the azeotropic processing stage, for removing the water in surplus material.Reluctant waste water is eliminated environmental pollution by the present invention, while recycling has obtained high value-added product.
Description
Technical field
The present invention relates to multicomponent Azeotrope separation technical fields, in particular to ethyl alcohol-tertiary butanol and water rectifying separation side
Method.
Background technique
Ethanol molecule formula is C2H6O, fluid density are 0.789g/cm3, and alcohol gas density is 1.59kg/m3, are commonly called as wine
Essence, it is a kind of inflammable, volatile colourless transparent liquid under room temperature, normal pressure, and relative density 0.816, boiling point is 78.4 DEG C,
Fusing point is -114.3 DEG C, and energy and water are dissolved each other with any ratio；It is most organic molten to be miscible in ether, chloroform, methanol, acetone, glycerol etc.
Agent.Ethyl alcohol has many uses, and acetic acid, beverage, essence, dyestuff, fuel etc. can be manufactured with ethyl alcohol.Medically also commonly use volume fraction
Make disinfectant etc. for 70% ~ 75% ethyl alcohol, has in national defence chemical industry, health care, food industry, industrial and agricultural production extensive
Purposes.
The tert-butyl alcohol, also known as 2- methyl-2-propanol, trimethyl carbinol etc., molecular formula: C4H10O, it is colourless with camphor smell
Crystallization has in the presence of a small amount of water in liquid.25.5 DEG C of fusing point, 82.3 DEG C of boiling point, relative density 0.7887, refractive index 1.3878,
Viscosity (30 DEG C) 3.316mPa s.The tert-butyl alcohol can be used for synthesis of artificial Moschus and medicine intermediate, it is also possible to prepare tert-butyl
Chlorine and tert-butyl phenol, are alternatively arranged as solvent.
When ethyl alcohol-tertiary butanol and water ternary azeotrope exists simultaneously, due to water and ethyl alcohol azeotropic, tert-butyl alcohol azeotrope with water,
Ethyl alcohol and tert-butyl alcohol azeotropic cause the difficulty of separating alcohol and the tert-butyl alcohol to increase, and the energy consumption of separating technology is high, and ethyl alcohol and tertiary fourth
The purity of alcohol is difficult to reach requirement.
Summary of the invention
The purpose of the present invention is to overcome the shortcomings in the prior art and to provide ethyl alcohol-tertiary butanol and water separation sides
Method, have low energy consumption, the high advantage of product purity.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of ethyl alcohol-tertiary butanol and water distillation and separation method, the raw material containing ethyl alcohol, the tert-butyl alcohol and water is handled by pre-dehydration,
Ethyl alcohol and the tert-butyl alcohol are separated after azeotropic processing, stripping processing, rectification process, obtain product ethyl alcohol and the tert-butyl alcohol；The azeotropic
Entrainer is added in processing stage, for removing the water in surplus material.
Further, comprising the following steps:
S1. raw material carries out pre-dehydration processing, obtains liquid phase material and water, and the tower top liquid phase material is ethyl alcohol, the tert-butyl alcohol and lacks
Measure the mixture of water；
S2. entrainer will be added in the S1 in the liquid phase material of tower top and carry out azeotropic distillation, obtain tower top low boiling point gas gas-phase objects
Material is the mixture of ethyl alcohol, the tert-butyl alcohol, water and entrainer；Tower reactor obtains water-free ethyl alcohol and the tert-butyl alcohol；
S3. water-oil separating will be carried out after the condensation of low boiling point gaseous phase materials obtained in the S2, and will obtain oily phase and water phase, it will be described
It is oily mutually back to azeotropic again in S2；
S4. water phase obtained in the S3 is stripped, the water after stripping is directly excluded, the remaining tower top liquid phase after stripping
Material returns in S2 and carries out azeotropic distillation again；
S5. extractant is added in tower reactor obtains in the S2 ethyl alcohol and the tert-butyl alcohol and carries out extraction and separation, obtain alcohol product and
The mixture of the tert-butyl alcohol and extractant；Also rectification under vacuum can be directly used and be directly separated ethyl alcohol and tert-butyl alcohol product；
S6. the mixture of the tert-butyl alcohol obtained in the S5 and extractant is regenerated, obtains tert-butyl alcohol product.
Further, comprising the following steps:
A1. raw material carries out pre-dehydration processing, obtains liquid phase material and water, the liquid phase material is ethyl alcohol, the tert-butyl alcohol and a small amount of water
Mixture；
A2. will in the liquid phase material in the A1 be added entrainer carry out azeotropic distillation, tower top obtain low boiling point gaseous phase materials and
The mixture of ethyl alcohol, the tert-butyl alcohol and water, entrainer；Tower reactor obtains water-free ethyl alcohol and the tert-butyl alcohol；
A3. water-oil separating will be carried out after the condensation of low boiling point gaseous phase materials obtained in the A2, and will obtain oily phase and water phase, it will be described
It is oily mutually back to azeotropic again in A2；
A4. water phase obtained in the A3 is stripped, the water after stripping is directly excluded, the tower top residue liquid phase after stripping
Material returns in A2 and carries out azeotropic distillation again；
A5. ethyl alcohol obtained in the A2 and the tert-butyl alcohol are subjected to rectification under vacuum, obtain alcohol product and tert-butyl alcohol product.
Further, heat remaining after pre-dehydration is recycled using tower bottom preheater in pre-dehydration processing.
Further, entrainer is any one in hexamethylene or pentamethylene.
Further, extractant is any one in Ergol or methyl phenyl ethers anisole or both mixture.
Further, the extractant obtained after regenerating in S6 is returned in S5 and is recycled.
A kind of ethyl alcohol-tertiary butanol and water rectifying separator, the predehydration 1 including passing sequentially through piping connection, azeotrope column
2, stripper 3, extractive distillation column 4, regenerator 5；Wherein, 7 He of condenser is additionally provided between the azeotrope column 2 and stripper 3
Oil water separator 6；Condenser 7 is connected with 2 tower top of azeotrope column, for being condensed to 2 tower top material of azeotrope column, the other end and oil
Separator 6 is connected, and condensed material is sent into the oil water separator and carries out water-oil separating.
Further, one end of oil water separator 6 is connect with condenser 7, and the other end is connect with the tower top of stripper 3, is used
Stripper 3 is sent into the water phase for going out water-oil separating to strip.
Further, oil water separator 6 is additionally provided with the pipeline being connected with 2 tower reactor of azeotrope column, and being used for will be after water-oil separating
Oil mutually carry out azeotropic again back to azeotrope column 2.
In conclusion the invention has the following advantages:
1. using predehydration first to slough most of water, the presence for solving a large amount of water in waste water leads to azeotropic system energy consumption
Greatly, regeneration energy consumption is big, and entrainer dosage is big, the problem that equipment size is big, investment is big.
2. use azeotropic separation, solve ethyl alcohol and water and the tert-butyl alcohol and water be difficult to caused by ternary azeotropic simultaneously by
The technical problem of ethyl alcohol and tert-butyl alcohol separation；
3. the method for the present invention can efficiently separate ethyl alcohol, the tert-butyl alcohol and water, the purity of alcohol isolated is up to 99.8%, tertiary fourth
Alcohol purity can effectively reduce waste up to 99.9%, improve the rate of recovery；
4. the present invention pre-dehydration processing in using tower bottom preheater to pre-dehydration after remaining heat recycle, it is effectively save
The energy.
5. solvent selection Ergol or methyl phenyl ethers anisole one or both mixture in the present invention, utilize itself and tertiary fourth
The big characteristic of alcohol solubility, changes the relative volatility of ethyl alcohol and the tert-butyl alcohol, while boiling point is higher than ethyl alcohol, by extracting rectifying
Operation can not only increase product purity, while reducing energy consumption effectively by the tert-butyl alcohol and separation of ethanol.
6. should process investment it is small, low energy consumption, no three wastes, high income, purity is high, eliminate original technique to environment
Pollution can effectively use the waste ethanol of generation, the useless tert-butyl alcohol, turn waste into wealth, improve enterprise's added value.
7. process is using hexamethylene or pentamethylene as entrainer, entrainer has nontoxic, low boiling point, holds
It easily obtains, cheap advantage.Since hexamethylene or pentamethylene are not readily dissolved in water but can form lower azeotropic point with water
Mixture, can thus be come out prior to water azeotropic from tower top, so that ethyl alcohol-tertiary butanol and water of original ternary azeotropic
Water is entrained agent and takes away in azeotropic, and cannot form ternary azeotropic and become easy separation, and plant energy consumption is lower, and separation is easy, if
The advantages of standby small investment.
8. process uses one or two kinds of mixtures of Ergol or methyl phenyl ethers anisole as extractant, so that former
Carrying out ethyl alcohol-tert-butyl alcohol relative volatility under normal pressure becomes 1.17-1.3 from 1.01 difficult separation and is readily isolated, and in this way may be used
The advantages of tower height degree is effectively reduced, reduces equipment investment, reduces reflux ratio and energy consumption.
Detailed description of the invention
Fig. 1 is ethyl alcohol in embodiment 1-tertiary butanol and water rectifying separating technology flow chart.
1 predehydration, 2 azeotrope columns, 3 strippers, 4 extractive distillation columns, 5 regenerators, 6 oil water separators, 7 condensations
Device.
Specific embodiment
After raw material pre-dehydration, using hexamethylene azeotropic deep dehydration, later ethyl alcohol and the tert-butyl alcohol are dehydrated in benzoic acid
Under the action of benzyl ester is as extractant, carry out atmospheric extraction rectifying, tower top obtain alcohol product, tower reactor mixture to regenerator into
Row decompression regeneration, extractant Ergol are recycled.
Embodiment 1: as shown in Figure 1, comprising the following steps:
S1. raw material enters the progress pre-dehydration processing of predehydration 1, and 1 operating pressure of predehydration is 101kpa, tower top operation temperature
It is 85-100 DEG C, theoretical cam curve 36-85, preferably 44 pieces；Best feed entrance point 26-44 block, preferably 29 pieces；Pre-dehydration
The operating reflux ratio of tower is 1.8, obtains gaseous phase materials and water, gaseous phase materials are the mixtures of ethyl alcohol, the tert-butyl alcohol and a small amount of water, in advance
Dehydrating tower 1 recycles tower reactor heat by tower bottom preheater, effectively save energy consumption, and the water of tower reactor meets national integrated wastewater
Discharge standard (GB8978-2002) second level water quality discharge standard, is expelled directly out；
S2. gaseous phase materials S1 obtained enter azeotrope column 2 and hexamethylene progress azeotropic distillation are added, and obtain low boiling point gaseous phase materials
With the mixture of ethyl alcohol, the tert-butyl alcohol and water, hexamethylene；Azeotrope column 2 uses atmospheric distillation, and tower operating pressure is 101kpa, theoretical
The number of plates is 42-60, and Optimization Theory plate number is 45, and 7/18 piece of best feed entrance point, the operating reflux ratio of azeotrope column 2 is 0.55；
S3. will enter oil water separator 6 after the condensation of low boiling point gaseous phase materials obtained in S2 and carry out water-oil separating, obtain it is oily mutually and
Water phase, by oily mutually back to azeotropic dehydration again in S2；
S4. water phase obtained in S3 is entered stripper to strip, tower operating pressure be 101kpa, number of theoretical plate 10-35,
Preferably 22, best feed entrance point is 2, and the operating reflux ratio of stripper is 2, and the water after stripping meets national integrated wastewater discharge
Standard (GB8978-2002) second level water quality discharge standard, is expelled directly out, and the remaining liquid phase material after stripping returns in S2 again
Azeotropic distillation is carried out, while hexamethylene is recycled；
S5. ethyl alcohol obtained in S2 and the tert-butyl alcohol are entered into extractive distillation column 4, Ergol is added and carries out extraction and separation, tower
Operating pressure is 101kpa, and number of theoretical plate 55, best feed entrance point is 3/18, and the operating reflux ratio of extractive distillation column 4 is 4,
The mixture of alcohol product and the tert-butyl alcohol and Ergol is obtained, alcohol product purity is 99.8%；
S6. the mixture of the tert-butyl alcohol obtained in S5 and Ergol is entered regenerator 5 to regenerate, tower operating pressure is
20kpa, number of theoretical plate 16, best feed entrance point are 12, and the operating reflux ratio of extractive distillation column is 0.22, obtain Benzyl Benzoate
Ester and tert-butyl alcohol product, Ergol return to extractive distillation column 4 and are recycled, and tert-butyl alcohol product purity is 99.9%.
Embodiment 2
A1. raw material enters the progress pre-dehydration processing of predehydration 1, and 1 operating pressure of predehydration is 105kpa, tower top operation temperature
It is 85-100 DEG C, theoretical cam curve 55,38 pieces of best feed entrance point；The operating reflux ratio of predehydration is 1.4, obtains liquid phase
Material and water, gaseous phase materials are the mixtures of ethyl alcohol, the tert-butyl alcohol and a small amount of water, and predehydration 1 is by tower bottom preheater to tower reactor
Heat is recycled, effectively save energy consumption, and the water of tower reactor meets national sewage comprehensive emission standard (GB8978-2002) second level water
Matter discharge standard, is expelled directly out；
A2. liquid phase material A1 obtained enters azeotrope column 2 and pentamethylene progress azeotropic distillation is added, and obtains low boiling point gaseous phase materials
With the mixture of ethyl alcohol, the tert-butyl alcohol and water, pentamethylene；Azeotrope column 2 uses atmospheric distillation, and tower operating pressure is 102kpa, theoretical
Plate number is 38,4/12 piece of best feed entrance point, and the operating reflux ratio of azeotrope column 2 is 0.4；
A3. will enter oil water separator 6 after the condensation of low boiling point gaseous phase materials obtained in A2 and carry out water-oil separating, obtain it is oily mutually and
Water phase, by oily mutually back to azeotropic dehydration again in A2；
A4. the mixture that water phase obtained in A3 enters stripper and ethyl alcohol, the tert-butyl alcohol obtained in A2 and water, pentamethylene is total to
With being stripped, tower operating pressure is 105kpa, and number of theoretical plate 18, best feed entrance point is 2, the operating reflux ratio of stripper
It is 1.9, the water after stripping meets national sewage comprehensive emission standard (GB8978-2002) second level water quality discharge standard, directly arranges
Out, the remaining liquid phase material after stripping returns in A2 and carries out azeotropic distillation again, while recycling to pentamethylene；
A5., ethyl alcohol obtained in A2 and the tert-butyl alcohol are directly carried out to decompression 3kpa rectifying, 85 pieces of number of theoretical plate, feed Board position 36
Block, reflux ratio 3.5 obtain alcohol product and tert-butyl alcohol product, and overhead ethanol product purity is 99.88%, tower reactor tert-butyl alcohol product
Purity is 99.9%.
Embodiment 3
C1. raw material enters the progress pre-dehydration processing of predehydration 1, and 1 operating pressure of predehydration is 110kpa, tower top operation temperature
It is 88-108 DEG C, theoretical cam curve 44,26 pieces of best feed entrance point；The operating reflux ratio of predehydration is 1.6, obtains liquid phase
Material and water, gaseous phase materials are the mixtures of ethyl alcohol, the tert-butyl alcohol and a small amount of water, and predehydration 1 is by tower bottom preheater to tower reactor
Heat is recycled, effectively save energy consumption, and the water of tower reactor meets national sewage comprehensive emission standard (GB8978-2002) second level water
Matter discharge standard, is expelled directly out
C2. liquid phase material C1 obtained enters azeotrope column 2 and pentamethylene progress azeotropic distillation is added, and obtains low boiling point gaseous phase materials
With the mixture of ethyl alcohol, the tert-butyl alcohol and water, pentamethylene；Azeotrope column 2 uses atmospheric distillation, and tower operating pressure is 108kpa, theoretical
Plate number is 42,3/10 piece of best feed entrance point, and the operating reflux ratio of azeotrope column 2 is 0.48；
C3. will enter oil water separator 6 after the condensation of low boiling point gaseous phase materials obtained in C2 and carry out water-oil separating, obtain it is oily mutually and
Water phase, by oily mutually back to azeotropic dehydration again in C2；
C4. the mixture that water phase obtained in C3 enters stripper and ethyl alcohol, the tert-butyl alcohol obtained in C2 and water, pentamethylene is total to
With being stripped, tower operating pressure is 105kpa, and number of theoretical plate 18, best feed entrance point is 2, the operating reflux ratio of stripper
It is 1.9, the water after stripping meets national sewage comprehensive emission standard (GB8978-2002) second level water quality discharge standard, directly arranges
Out, the remaining liquid phase material after stripping returns in C2 and carries out azeotropic distillation again, while recycling to pentamethylene；
C5. ethyl alcohol obtained in C2 and the tert-butyl alcohol are entered into extractive distillation column 4, Ergol and methyl phenyl ethers anisole 1:1(wt% is added)
Extraction and separation are carried out, tower operating pressure is 101kpa, and number of theoretical plate 42, best feed entrance point is 2/11, extractive distillation column 4
Operating reflux ratio is 3.5, obtains the mixture of alcohol product and the tert-butyl alcohol and Ergol, and alcohol product purity is 99.7%；
C6. the mixture of the tert-butyl alcohol obtained in C5 and Ergol, methyl phenyl ethers anisole is entered regenerator 5 to regenerate, tower behaviour
Making pressure is 35kpa, and number of theoretical plate 22, best feed entrance point is 15, and the operating reflux ratio of extractive distillation column is 0.4, is obtained
Ergol, methyl phenyl ethers anisole and tert-butyl alcohol product, Ergol, methyl phenyl ethers anisole return to extractive distillation column 4 and are recycled, the tert-butyl alcohol
Product purity is 99.8%.
Embodiment 4
D1. raw material enters the progress pre-dehydration processing of predehydration 1, and 1 operating pressure of predehydration is 106kpa, tower top operation temperature
It is 88-107 DEG C, theoretical cam curve 38,22 pieces of best feed entrance point；The operating reflux ratio of predehydration is 1.85, obtains liquid
Phase materials and water, gaseous phase materials are the mixtures of ethyl alcohol, the tert-butyl alcohol and a small amount of water, and predehydration 1 is by tower bottom preheater to tower
Kettle heat is recycled, effectively save energy consumption, and the water of tower reactor meets national sewage comprehensive emission standard (GB8978-2002) second level
Water quality discharge standard, is expelled directly out
D2. liquid phase material D1 obtained enters azeotrope column 2 and pentamethylene progress azeotropic distillation is added, and obtains low boiling point gaseous phase materials
With the mixture of ethyl alcohol, the tert-butyl alcohol and water, pentamethylene；Azeotrope column 2 uses atmospheric distillation, and tower operating pressure is 102kpa, theoretical
Plate number is 55,6/18 piece of best feed entrance point, and the operating reflux ratio of azeotrope column 2 is 0.32；
D3. will enter oil water separator 6 after the condensation of low boiling point gaseous phase materials obtained in D2 and carry out water-oil separating, obtain it is oily mutually and
Water phase, by oily mutually back to azeotropic dehydration again in D2；
D4. the mixture that water phase obtained in D3 enters stripper and ethyl alcohol, the tert-butyl alcohol obtained in D2 and water, pentamethylene is total to
With being stripped, tower operating pressure is 105kpa, and number of theoretical plate 18, best feed entrance point is 2, the operating reflux ratio of stripper
It is 1.9, the water after stripping meets national sewage comprehensive emission standard (GB8978-2002) second level water quality discharge standard, directly arranges
Out, the remaining liquid phase material after stripping returns in D2 and carries out azeotropic distillation again, while recycling to pentamethylene；
D5. ethyl alcohol obtained in D2 and the tert-butyl alcohol are entered into extractive distillation column 4, methyl phenyl ethers anisole is added and carries out extraction and separation, tower operation
Pressure is 101kpa, and number of theoretical plate 65, best feed entrance point is 5/18, and the operating reflux ratio of extractive distillation column 4 is 4.2, is obtained
To the mixture of alcohol product and the tert-butyl alcohol and methyl phenyl ethers anisole, alcohol product purity is 99.65%；
D6. the mixture of the tert-butyl alcohol obtained in D5 and methyl phenyl ethers anisole is entered regenerator 5 to regenerate, tower operating pressure is
50kpa, number of theoretical plate 18, best feed entrance point are 12, and the operating reflux ratio of extractive distillation column is 0.2, obtain methyl phenyl ethers anisole and
Tert-butyl alcohol product, methyl phenyl ethers anisole return to extractive distillation column 4 and are recycled, and tert-butyl alcohol product purity is 99.9%.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art
Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this
All by the protection of Patent Law in the scope of the claims of invention.
Claims (10)
1. recycling ethyl alcohol-tertiary butanol and water separation method in a kind of waste water, which is characterized in that by containing ethyl alcohol, the tert-butyl alcohol it is useless
Water separates ethyl alcohol and the tert-butyl alcohol after pre-dehydration processing, azeotropic processing, stripping processing, rectification process, obtains product ethyl alcohol
And the tert-butyl alcohol；Entrainer is added in the azeotropic processing stage, for removing the water in surplus material.
2. a kind of ethyl alcohol-tertiary butanol and water distillation and separation method according to claim 1, which is characterized in that including following step
It is rapid:
S1. raw material carries out pre-dehydration processing, and tower top obtains liquid phase material and tower reactor obtains water, and the tower top liquid phase material is second
The mixture of alcohol, the tert-butyl alcohol and a small amount of water；
S2. entrainer will be added in the liquid phase material in the S1 and carries out azeotropic distillation, tower top, which obtains low boiling point gaseous phase materials, is
The mixture of ethyl alcohol, the tert-butyl alcohol and water, entrainer；Tower reactor obtains water-free ethyl alcohol and t-butanol mixture；
S3. water-oil separating is carried out after the low boiling point gaseous phase materials that tower top in the S2 obtains being condensed, obtains oily phase and water phase, it will
The oil is mutually back to azeotropic dehydration again in S2；
S4. water phase obtained in the S3 is stripped, the tower reactor water after stripping is directly excluded, the remaining tower top after stripping
Liquid phase material returns in S2 and carries out azeotropic distillation again；
S5. extractant is added in tower reactor obtains in the S2 ethyl alcohol and the tert-butyl alcohol and carries out extraction and separation, obtain alcohol product and
The mixture of the tert-butyl alcohol and extractant；
S6. the mixture of the tert-butyl alcohol obtained in the S5 and extractant is regenerated, obtains tert-butyl alcohol product.
3. a kind of ethyl alcohol-tertiary butanol and water distillation and separation method according to claim 1, which is characterized in that including following step
It is rapid:
A1. raw material carries out pre-dehydration processing, obtains liquid phase material and water, and the tower top liquid phase material is ethyl alcohol, the tert-butyl alcohol and lacks
Measure the mixture of water；
A2. entrainer will be added in the liquid phase material in the A1 and carry out azeotropic distillation, obtain low boiling point gaseous phase materials and ethyl alcohol,
The mixture of the tert-butyl alcohol and water, entrainer；
A3. water-oil separating will be carried out after the condensation of low boiling point gaseous phase materials obtained in the A2, and will obtain oily phase and water phase, it will be described
It is oily mutually back to azeotropic again in A2；
A4. water phase obtained in the A3 is stripped, the water after stripping is directly excluded, the remaining liquid phase material after stripping
Back to azeotropic distillation is carried out in A2 again；
A5. ethyl alcohol obtained in the A2 and the tert-butyl alcohol are subjected to rectification under vacuum, obtain alcohol product and tert-butyl alcohol product.
4. a kind of ethyl alcohol-tertiary butanol and water distillation and separation method according to claim 2 or 3, which is characterized in that described pre-
In dehydration, heat remaining after pre-dehydration is recycled using tower bottom preheater.
5. a kind of ethyl alcohol-tertiary butanol and water distillation and separation method according to claim 1, which is characterized in that the entrainer
It is any one in hexamethylene or pentamethylene.
6. a kind of ethyl alcohol-tertiary butanol and water distillation and separation method according to claim 2, which is characterized in that the extractant
Be Ergol, in methyl phenyl ethers anisole any one or both mixture.
7. a kind of ethyl alcohol-tertiary butanol and water distillation and separation method according to claim 2, which is characterized in that in the S6 again
The extractant obtained after life is returned in S5 and is recycled.
8. a kind of ethyl alcohol-tertiary butanol and water rectifying separator, which is characterized in that the pre-dehydration including passing sequentially through piping connection
Tower (1), azeotrope column (2), stripper (3), extractive distillation column (4), regenerator (5)；Wherein, the azeotrope column (2) and the vapour
Condenser (7) and oil water separator (6) are additionally provided between stripper (3)；The condenser (7) and the azeotrope column (2) tower top
It is connected, for condensing to the azeotrope column (2) tower top material, the other end is connected with the oil water separator (6), will condense
Material afterwards is sent into the oil water separator and carries out water-oil separating.
9. a kind of ethyl alcohol according to claim 8-tertiary butanol and water rectifying separator, which is characterized in that the grease point
One end from device (6) is connect with the condenser (7), and the other end is connect with the tower top of the stripper (3), for dividing grease
The water phase separated out is sent into the stripper (3) and is stripped.
10. a kind of ethyl alcohol according to claim 9-tertiary butanol and water rectifying separator, which is characterized in that the grease
Separator (6) is additionally provided with the pipeline being connected with the azeotrope column (2) tower reactor, for the oil after water-oil separating mutually to be returned to institute
It states azeotrope column (2) and carries out azeotropic again.
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Citations (5)
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| CN1417182A (en) * | 2002-12-10 | 2003-05-14 | 西安交通大学 | Heat pump azeotropic rectification process and equipment for fuel ethanol |
| CN101412671A (en) * | 2008-11-06 | 2009-04-22 | 烟台国邦化工机械科技有限公司 | Method for separating isobutyl acetate, ethanol and water by azeotropic distillation |
| CN103772145A (en) * | 2012-10-23 | 2014-05-07 | 中国石油化工股份有限公司 | Separation method used for preparing isopropanol via hydrogenation of acetone |
| CN105669377A (en) * | 2016-01-22 | 2016-06-15 | 北京凯文特科技有限公司 | Technique for separating mixed alcohol |
| CN105712839A (en) * | 2014-12-05 | 2016-06-29 | 中国石油天然气股份有限公司 | Separation method applicable to both propylene hydration and acetone hydrogenation for isopropyl alcohol preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1417182A (en) * | 2002-12-10 | 2003-05-14 | 西安交通大学 | Heat pump azeotropic rectification process and equipment for fuel ethanol |
| CN101412671A (en) * | 2008-11-06 | 2009-04-22 | 烟台国邦化工机械科技有限公司 | Method for separating isobutyl acetate, ethanol and water by azeotropic distillation |
| CN103772145A (en) * | 2012-10-23 | 2014-05-07 | 中国石油化工股份有限公司 | Separation method used for preparing isopropanol via hydrogenation of acetone |
| CN105712839A (en) * | 2014-12-05 | 2016-06-29 | 中国石油天然气股份有限公司 | Separation method applicable to both propylene hydration and acetone hydrogenation for isopropyl alcohol preparation |
| CN105669377A (en) * | 2016-01-22 | 2016-06-15 | 北京凯文特科技有限公司 | Technique for separating mixed alcohol |
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