CN108250040A - A kind of method that alcohol solution separates and recovers in high purity aluminium oxide production - Google Patents
A kind of method that alcohol solution separates and recovers in high purity aluminium oxide production Download PDFInfo
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- CN108250040A CN108250040A CN201810025578.0A CN201810025578A CN108250040A CN 108250040 A CN108250040 A CN 108250040A CN 201810025578 A CN201810025578 A CN 201810025578A CN 108250040 A CN108250040 A CN 108250040A
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- alcohol
- alcohol solution
- water
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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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Abstract
The present invention relates to material preparation process fields, particularly belong to high purity aluminium oxide preparation field, are related to a kind of method that alcohol solution separates and recovers in high purity aluminium oxide production, include the following steps：Step 1, the alcohol solution that will be obtained in the alcohol hydrolyzing process in high purity aluminium oxide production process adjust the pH value of alcohol solution to neutral or weak acid using phosphoric acid；Alcohol solution after the adjusting pH value obtained in step 2, step 1, which is sent in early steam tower, carries out air-distillation, obtains alcohol water vapour；Step 3, the alcohol water vapour that will be obtained in step 2 are sent to the part water absorbed in piece alkali water suction tower in alcohol water vapour, are thoroughly dehydrated into molecular screen membrane separator later；The beneficial effects of the present invention are：The cost of investment and operating cost of alkoxide hydrolysis can not only be reduced, and the common process that can also be separated and recovered to alcohol solution is improved.
Description
Technical field
The present invention relates to material preparation process fields, particularly belong to high purity aluminium oxide preparation field, are related to a kind of high pure oxygen
Change the method that alcohol solution separates and recovers in aluminium production.
Background technology
Separation and purification is needed from largely diluter alcohol solution in industrial processes to obtain the alcohol of high-purity, and is adopted
The alcohol that can not obtain forming higher than alcohol water azeotropic with common distillating method.The traditional handicraft for detaching alcohol-water system is pressed from both sides with benzene
Band agent azeotropic distillation, due to harm of the benzene to human body, which will gradually be substituted, it is industrial also have using alcohol, water,
Diisopropyl ether ternary azeotrope carries out azeotropic distillation dehydration, although diisopropyl ether toxicity is low, is easy to air and forms peroxidating
Object has the danger of explosion, and water amount effect is unsatisfactory.
In order to detach alcohol and water, technical staff proposes the technique of various separation and recovery alcohol, including azeotropic distillation, extraction
Rectifying etc..
The Chinese invention patent of Publication No. CN200810138752.9 proposes a kind of utilization bulkhead azeotropy rectification column point
Process from alcohol and water, by next door tower be applied to azeotropic distillation during, first in next door tower azeotropy rectification column, alcohol by
Dewatering period tower reactor is guessd out, and waste water is guessd out by side line rectifying section tower reactor, completes separation, the entrainer of alcohol and water simultaneously in a tower
The tasks such as recycling, eliminate a rectifying column and a condenser, and bulkhead azeotropy can avoid the back-mixing in old process from imitating
It should.Under identical separation requirement, energy ratio routine azeotropic distillation flow needed for bulkhead azeotropy rectification column flow saves 10~30%,
Equipment investment saves 20~45%.
The Chinese invention patent of Publication No. CN1249294A proposes a kind of side of adding salt extraction-azeotropic distillation recycling alcohol
Alcohol dilute aqueous solution in industrial production is just raised the alcohol just concentrated, then using C6 aliphatic hydrocarbon conducts by method through rectifying first
The aqueous solution of extractant, inorganic sodium or sylvite carries out saline extraction as salting-out separation agent to it, by the organic phase after extraction
It is sent into azeotropic distillation dehydrating tower to be refined, the concentrated device recycling Posterior circle of release agent uses, and tower reactor can obtain alcohol content and be
More than 99.5% product, but the technological operation is complex, and equipment investment is higher.
The Chinese invention patent of Publication No. CN201710323700.8 proposes a kind of utilization multifunctional alcohol dehydrating tower, fills out
Material the technologies such as utilizes with plate column compound rectifying column, pressure-variable adsorption and ability multistage multiple-effect, efficiently solves and is total to close to alcohol and water
The aqueous alcohol material liquid for boiling composition further refines the problem of removing azeotropic water.The defects of the method, is that multifunctional alcohol is dehydrated
Tower, compound rectifying column are detached and are regenerated with adsorption and desorption mechanism, once absorption close to after saturation, due to adsorbing power
Deficiency may be decreased adsorption rate, directly results in hydrone and enters in separated alcohol, improves alcohol water content.Thus, it is producing
It needs tightly to be controlled in the process, filler supersaturation is avoided to cause damages.In addition, the desorption of filler, replacement etc. need to expend largely
Energy and manpower and materials reduce production efficiency.
Invention content
The defects of in order to overcome the above-mentioned prior art, the technical problems to be solved by the invention are：There is provided one kind can not only
Enough reduce the cost of investment and operating cost of alkoxide hydrolysis, moreover it is possible to which the common process of alcohol solution separation and recovery is improved
High purity aluminium oxide production in alcohol solution separate and recover method.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：Alcohol water in a kind of high purity aluminium oxide production
The method of solution separation and recovery, includes the following steps：
Step 1, the alcohol solution that will be obtained in the alcohol hydrolyzing process in high purity aluminium oxide production process, are adjusted using phosphoric acid
The pH value of alcohol solution is to neutral or weak acid；
Alcohol solution after the adjusting pH value obtained in step 2, step 1, which is sent in early steam tower, carries out air-distillation, obtains
To alcohol water vapour；
Step 3, the alcohol water vapour that will be obtained in step 2 are sent to the part water absorbed in piece alkali water suction tower in alcohol water vapour,
It is thoroughly dehydrated into molecular screen membrane separator later；
Step 4 detaches the aqueous solution of the low alcohol content of the piece alkali water suction tower bottom of towe in step 3 and molecular screen membrane separator
The water gone out returns to be reused in alcohol hydrolyzing process.
Further, the alcohol solution in the step 1 is isopropanol water solution or isobutyl alcohol solution or n-butanol water
One kind in solution.
Further, the molecular screen membrane that the molecular screen membrane separator uses is organic zeolite membrane.
Further, the organic zeolite membrane is zeolite molecular sieve film or NaA molecular sieve membrane or type ZSM 5 molecular sieve film
In one kind.
Further, the molecular screen membrane that the molecular screen membrane separator uses is organic molecule sieve membrane.
Further, the alcohol content of the alcohol solution in the step 1 is 10~20%.
Further, the temperature of early steam tower is set as 80~100 DEG C in the step 2.
Further, described alkali water suction tower is made of piece alkali.
The beneficial effects of the present invention are：Traditional high purity alumina producing, alcohols separation and recovery is using azeotropic distillation, extraction
Technique, high energy consumption take up a large area, often need to add in a large amount of solvents and extracted or azeotropic；Molecular sieve adsorbing and dewatering is due to alcohol
Water content is high in water mixed liquid, and absorption is slower, and is difficult to put into practical application in industry；Pervaporation Technology is remarkably improved separation
Efficiency reduces process energy consumption, improves the purity of recycling alcohols.Alcohol water vapour is first passed through into piece alkali adsorption tower in the present invention and absorbs alcohol
Part water in water vapour enters back into molecular screen membrane progress alcohol water and is completely separated, can reduce setting for molecular screen membrane to greatest extent
Standby input keeps the Effec-tive Function of dehydration procedure；High-purity lye is formed after piece Alkali absorption moisture, can be used in high purity aluminium oxide life
The other processes of production will not generate environmental protection pressure.The water that the technique is detached greatly reduces, and can be set not increasing
The operational efficiency of molecular screen membrane separator is improved under the premise of standby, reduces enhance production capacities required equipment investment and operating cost,
Estimated, of the invention alcohol-water separation method, energy consumption are only about the 1/3 of energy consumption of rectification, about molecular sieve absorption energy consumption 2/5.
Description of the drawings
The method institute that Fig. 1 is separated and recovered for alcohol solution in a kind of high purity aluminium oxide production of the specific embodiment of the invention
The structure diagram of device；
Label declaration：
1st, alcohol solution；2nd, feed pump；3rd, alcohol recycling can；4th, heat exchanger；5th, reactor product cooler；6th, early steam tower；7th, piece
Alkali water suction tower；8th, molecular screen membrane separator；9th, condenser；10th, vacuum machine；11st, water pot.
Specific embodiment
For the technology contents that the present invention will be described in detail, the objects and the effects, below in conjunction with embodiment and coordinate attached
Figure is explained.
The design of most critical of the present invention is：The part water in piece alkali water suction tower absorption alcohol water vapour is first passed through, is entered back into
Molecular screen membrane separator, according to inorganic permeable membrane separation principle, using water, the kinetic diameter of alcohol molecule difference and for
The polarity difference of molecular sieve realizes the separation of alcohol and water.
A kind of method that alcohol solution separates and recovers in high purity aluminium oxide production, includes the following steps：
Step 1, the alcohol solution that will be obtained in the alcohol hydrolyzing process in high purity aluminium oxide production process, are adjusted using phosphoric acid
The pH value of alcohol solution is to neutral or weak acid；
Alcohol solution after the adjusting pH value obtained in step 2, step 1, which is sent in early steam tower, carries out air-distillation, obtains
To alcohol water vapour；
Step 3, the alcohol water vapour that will be obtained in step 2 are sent to the part water absorbed in piece alkali water suction tower in alcohol water vapour,
It is thoroughly dehydrated into molecular screen membrane separator later；
Step 4 detaches the aqueous solution of the low alcohol content of the piece alkali water suction tower bottom of towe in step 3 and molecular screen membrane separator
The water gone out returns to be reused in alcohol hydrolyzing process.
As shown in Figure 1, the technological process of method that alcohol solution separates and recovers in a kind of above-mentioned high purity aluminium oxide production
For：Alcohol solution 1 enters heat exchanger 4 via feed pump 2, and alcohol solution is sent into early steam tower 6 and carries out air-distillation, is obtained
Obtained alcohol water vapour is sent to the part water absorbed in piece alkali water suction tower 7 in alcohol water vapour, enters back into molecular sieve by alcohol water vapour
Membrane separator 8 carries out thoroughly being dehydrated the alcohol separated, and obtained alcohol is cooled down successively via heat exchanger 4 and product
Device 5 enters alcohol recycling can 3 and carries out recycling preservation, with the aqueous solution and molecular screen membrane of the low alcohol content of time slice alkali water suction 7 bottom of towe of tower
The water that separator 8 is isolated returns to be reused in alcohol hydrolyzing process, and the water that molecular screen membrane separator 8 is separated is via condensation
Device 9 cools down, and acts on into water pot 11 and preserving via vacuum machine 10.
The advantageous effect of method that alcohol solution separates and recovers in a kind of above-mentioned high purity aluminium oxide production is：It is traditional high
Pure alumina produces, and alcohols separation and recovery is taken up a large area using azeotropic distillation, extraction process, high energy consumption, often needed to add in greatly
Amount solvent is extracted or azeotropic；For molecular sieve adsorbing and dewatering due to water content height in alcohol-water mixture, absorption is slower, and is difficult to throw
Enter practical application in industry；Pervaporation Technology is remarkably improved separative efficiency, reduces process energy consumption, improves the pure of recycling alcohols
Degree.In the present invention by alcohol water vapour first pass through piece alkali adsorption tower absorb alcohol water vapour in part water, enter back into molecular screen membrane into
Row alcohol water is completely separated, and can reduce the equipment investment of molecular screen membrane to greatest extent, keeps the Effec-tive Function of dehydration procedure；Piece alkali
High-purity lye is formed after absorbing moisture, can be used in the other processes of high purity aluminium oxide production, environmental protection pressure will not be generated.The work
The water that skill is detached greatly reduces, and the operation of molecular screen membrane separator can be improved under the premise of equipment is not increased
Efficiency reduces enhance production capacities required equipment investment and operating cost, and estimated, of the invention alcohol-water separation method, energy consumption is only
Energy consumption 2/5 is adsorbed in about the 1/3 of energy consumption of rectification, about molecular sieve.
Further, the alcohol solution in the step 1 is isopropanol water solution or isobutyl alcohol solution or n-butanol water
One kind in solution.
Further, the molecular screen membrane that the molecular screen membrane separator uses is organic zeolite membrane.
Further, the organic zeolite membrane is zeolite molecular sieve film or NaA molecular sieve membrane or type ZSM 5 molecular sieve film
In one kind.
Seen from the above description, by using in zeolite molecular sieve film or NaA molecular sieve membrane or type ZSM 5 molecular sieve film
It is a kind of to be used as organic zeolite membrane, since zeolite molecular sieve film or NaA molecular sieve membrane or type ZSM 5 molecular sieve film are all hydrophilies
Inoranic membrane is conducive to improve the flux of hydrone.
Further, the molecular screen membrane that the molecular screen membrane separator uses is organic molecule sieve membrane.
Further, the alcohol content of the alcohol solution in the step 1 is 10~20%.
Further, the temperature of early steam tower is set as 80~100 DEG C in the step 2.
Further, described alkali water suction tower is made of piece alkali.
Embodiment 1
The isopropanol water solution of aluminium isopropoxide hydrolysis recycling, wherein isopropanol content in terms of mass fraction about 15~
20%, water content 80~85%；The alcohol solution is sent into early steam tower, temperature is set as 85 DEG C, and the IPA vapor of tower top (contains
Water is about 13%) to remove part water by piece alkali water suction tower；Steam is sent into NaA type molecular screen membrane separators later, is passed through
Molecular screen membrane respectively obtains pure isopropyl alcohol and water for the pore size of water, isopropanol molecule and the difference of dissolving polarity.
Embodiment 2
The isopropanol water solution of aluminium isopropoxide hydrolysis recycling, wherein isopropanol content are calculated as 15% with mass fraction, and water contains
Amount 85%；The alcohol solution is sent into early steam tower, temperature is set as 85 DEG C, the IPA vapor of tower top (water content is about 13%)
Part water is removed by piece alkali water suction tower；Later by steam be sent into NaA type molecular screen membrane separators, by molecular screen membrane for
The difference of water, the pore size of isopropanol molecule and dissolving polarity, respectively obtains pure isopropyl alcohol and water.
Embodiment 3
The isobutyl alcohol solution of isobutanol aluminum hydrolysis recycling, wherein isobutyl alcohol content are about 12% in terms of mass fraction, water
Content 88%；The alcohol solution is sent into early steam tower, temperature is set as 95 DEG C, and (water content is about for the isobutanol steam of tower top
30%) part water is removed by piece alkali water suction tower；Steam is sent into type ZSM 5 molecular sieve membrane separator later, passes through molecular sieve
Film respectively obtains pure isobutyl alcohol and water for the pore size of water, isobutanol molecule and the difference of dissolving polarity.
Embodiment 4
The n-butanol aqueous solution of Tributyl aluminate hydrolysis recycling, wherein levels of n-butanol are about 20% in terms of mass fraction, water
Content 80%；The n-butanol aqueous solution is sent into early steam tower, temperature is set as 97 DEG C, and (water content is about for the n-butanol steam of tower top
37%) to remove part water by the tower that absorbs water；Steam is sent into NaA type molecular screen membrane separators later, passes through molecular screen membrane pair
The difference of Yu Shui, the pore size of alcohol molecule and dissolving polarity, respectively obtain pure alcohol and water.
In conclusion the method that alcohol solution separates and recovers in a kind of high purity aluminium oxide production provided by the invention, tradition
High purity aluminium oxide produces, and using azeotropic distillation, extraction process, high energy consumption takes up a large area, often needs to add in alcohols separation and recovery
A large amount of solvents are extracted or azeotropic；For molecular sieve adsorbing and dewatering due to water content height in alcohol-water mixture, absorption is slower, and is difficult to
Put into practical application in industry；Pervaporation Technology is remarkably improved separative efficiency, reduces process energy consumption, improves the pure of recycling alcohols
Degree.In the present invention by alcohol water vapour first pass through piece alkali adsorption tower absorb alcohol water vapour in part water, enter back into molecular screen membrane into
Row alcohol water is completely separated, and can reduce the equipment investment of molecular screen membrane to greatest extent, keeps the Effec-tive Function of dehydration procedure；Piece alkali
High-purity lye is formed after absorbing moisture, can be used in the other processes of high purity aluminium oxide production, environmental protection pressure will not be generated.The work
The water that skill is detached greatly reduces, and the operation of molecular screen membrane separator can be improved under the premise of equipment is not increased
Efficiency reduces enhance production capacities required equipment investment and operating cost, and estimated, of the invention alcohol-water separation method, energy consumption is only
Energy consumption 2/5 is adsorbed in about the 1/3 of energy consumption of rectification, about molecular sieve.
By using a kind of as inorganic point in zeolite molecular sieve film or NaA molecular sieve membrane or type ZSM 5 molecular sieve film
Sub- sieve membrane since zeolite molecular sieve film or NaA molecular sieve membrane or type ZSM 5 molecular sieve film are all hydrophilic inorganic films, is conducive to
Improve the flux of hydrone.
The foregoing is merely the embodiment of the present invention, are not intended to limit the scope of the invention, every to utilize this hair
The equivalents that bright specification and accompanying drawing content are made directly or indirectly are used in relevant technical field, similarly include
In the scope of patent protection of the present invention.
Claims (8)
1. a kind of method that alcohol solution separates and recovers in high purity aluminium oxide production, which is characterized in that include the following steps：
Step 1, the alcohol solution that will be obtained in the alcohol hydrolyzing process in high purity aluminium oxide production process adjust alcohol water using phosphoric acid
The pH value of solution is to neutral or weak acid；
Alcohol solution after the adjusting pH value obtained in step 2, step 1, which is sent in early steam tower, carries out air-distillation, obtains alcohol
Water vapour；
Step 3, the alcohol water vapour that will be obtained in step 2 are sent to the part water absorbed in piece alkali water suction tower in alcohol water vapour, later
It is thoroughly dehydrated into molecular screen membrane separator；
What step 4, the aqueous solution of the low alcohol content of tower bottom of towe that the piece alkali in step 3 is absorbed water and molecular screen membrane separator were isolated
Water returns to be reused in alcohol hydrolyzing process.
2. the method that alcohol solution separates and recovers in high purity aluminium oxide production according to claim 1, which is characterized in that institute
It is one kind in isopropanol water solution or isobutyl alcohol solution or n-butanol aqueous solution to state the alcohol solution in step 1.
3. the method that alcohol solution separates and recovers in high purity aluminium oxide production according to claim 1, which is characterized in that institute
Molecular screen membrane that molecular screen membrane separator uses is stated as organic zeolite membrane.
4. the method that alcohol solution separates and recovers in high purity aluminium oxide production according to claim 3, which is characterized in that institute
Organic zeolite membrane is stated as one kind in zeolite molecular sieve film or NaA molecular sieve membrane or type ZSM 5 molecular sieve film.
5. the method that alcohol solution separates and recovers in high purity aluminium oxide production according to claim 1, which is characterized in that institute
Molecular screen membrane that molecular screen membrane separator uses is stated as organic molecule sieve membrane.
6. the method that alcohol solution separates and recovers in high purity aluminium oxide production according to claim 1, which is characterized in that institute
The alcohol content for stating the alcohol solution in step 1 is 10~20%.
7. the method that alcohol solution separates and recovers in high purity aluminium oxide production according to claim 1, which is characterized in that institute
The temperature for stating early steam tower in step 2 is set as 80~100 DEG C.
8. the method that alcohol solution separates and recovers in high purity aluminium oxide production according to claim 1, which is characterized in that institute
Piece alkali water suction tower is stated to be made of piece alkali.
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Application publication date: 20180706 |