CN105732378B - A kind of method that organic-aqueous mixture carries out dehydration purification - Google Patents
A kind of method that organic-aqueous mixture carries out dehydration purification Download PDFInfo
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Abstract
The invention discloses a kind of methods that organic-aqueous mixture carries out dehydration purification, belong to organic material preparation technique range, using circulated inert gas as carrier, it is humidified by inert gas, desorption and regeneration, Gas Phase Adsorption detaches and the closed circuit circulatory system of cryogenic condensation, it can obtain micro- water organic matter of high-purity, wherein desorption and regeneration is detached with Gas Phase Adsorption is realized using two or more adsorption tanks cyclic switchings in parallel, the method is particularly suitable for the organic matters such as methyl acetate or isopropanol and the azeotropic mixture of water is dehydrated, it overcomes because azeotropic can not be by distilling the disadvantage for completing dehydration purification with the pure liquid phase adsorption dehydration energy of tradition is big and sorbent life is short, provide no gas phase emission, it is environmentally friendly simple, the treatment process of high efficiency low cost.
Description
Technical field
The invention belongs to organic material preparation technique range, especially a kind of organic-aqueous mixture carries out dehydration purification
Method.
Background technology
Have in industrial production and all contain water in many raw materials, intermediate product and product, and aqueous is to cause further to locate
The difficult reason of reason process high energy consumption, poor efficiency, processing.For the organic-aqueous mixture of liquid phase, traditional processing method has essence
It evaporates, extract, adsorb, but for some special object systems, organic matter can form azeotropic mixture with water, cause processing difficult, or can
Capable separating technology is complicated, high energy consumption, it is difficult to obtain the organic matter of high-purity.
Point of the organic-aqueous mixture of liquid phase may be implemented one is using liquid phase adsorption process in existing patent and document
From technique includes mainly two adsorbing separation, alternating temperature purging desorption and regeneration parts, and process is：Mixture enters adsorption tower,
By the bed with selective absorption, moisture therein is selectively adsorbed, and obtains the higher organic products of purity；Saturation
Adsorbent bed first empty use water or steam to replace again, then adsorbent is regenerated with hot dry air, after cooling again
It can be adsorbed.Aqueous organic mixture is handled using this method, is generated during having the drawback that a large amount of organic mixed
It closes liquid and needs recycling, hot steam consumption is big, and the temperature of desorption and regeneration is higher.
Another kind is to utilize superheated steam phase adsorption method, and the separation of the organic-aqueous mixture of steam phase may be implemented,
Technique mainly condenses to obtain two parts of product and desorption and regeneration including adsorbing separation, relative to the technological process of liquid phase adsorption,
Solve the problems, such as that a large amount of organic liquid mixture is generated in liquid phase adsorption regeneration needs recycling, it is single to consider system pressure drop and vaporization
The factors such as overheat, therefore can only be adsorbed at a temperature of higher than organic mixture boiling point.It is limited to adsorbent at high temperature
The low limitation of adsorption capacity, also therefore available organic liquid mixture is also restrained.
By taking methyl acetate as an example：Methyl acetate is a kind of important solvent and Organic Chemicals, in the industry often with
The form of byproduct largely occurs, such as in the industrial processes of p-phthalic acid (PTA), can all generate and largely contain
Industrial wastes/exhaust gas of methyl acetate.Under normal circumstances, polyvinyl alcohol per ton production all can 1.7 tons of by-product methyl acetate,
Every 1 ton of PTA process units can all generate 6 kilograms of methyl acetate and form presence with the azeotropic of about 95% purity.Factory is more
It is recycled by the way of flowing back into technique, the excessive exhaust gas that then enters is removed to CC Catalytic Converter, and it is to use also to have part factory
Acetic acid and methanol of the hydrolysis manufacture output value compared with methyl acetate cheap market price.The purity of the methyl acetate required currently on the market
99.5% or more, the market price of this 99.5% high-purity methyl acetate is high compared to the methyl acetate of about 95% purity
30~40%, so methyl acetate is separated and recovered from industry byproduct, existing important environment protection significance, and have good application
Value and economic benefit.But also contain the impurity such as first alcohol and water in these methyl acetate waste liquid/exhaust gas, due to methyl acetate with
Water, methanol easily form azeotropic mixture, and the methyl acetate of isolated high-purity is difficult to common rectificating method.Currently, for poly-
The recoverying and utilizing method of vinyl alcohol and p-phthalic acid's production process by-product methyl acetate, mainly have catalytic rectification method,
Extraction rectifying method, salt separation method etc..Methyl acetate hydrolysis is acetic acid and methanol by catalytic rectification process, it is contemplated that tumer
The raw material of the commercial synthesis of ester is exactly that the market demand of acetic acid and methanol and high-purity methyl acetate increasingly increases, and this method is not
There are what economic benefit and social benefit；Extraction fractional distillation high energy consumption, Solvent quantity is big, and purity is not high；Salt separation side
Method separating effect is preferable and energy consumption is relatively low, but complex process；It is also difficult to obtain high-purity methyl acetate using membrane separation technique,
Using traditional temp.-changing adsorption method, need to regenerate adsorbent using a large amount of vapor pair and hot-air, so energy
It is also relatively high in terms of consumption.Therefore, there is an urgent need for a kind of azeotropic mixture is formed for organic-aqueous mixture, especially organic matter and water
Environmentally friendly simple, high efficiency low cost the dehydration purification processes technique of mixture, to solve industrial preparation high-purity organic matter at present
Technical barrier.
Invention content
It is an object of the invention in place of overcome the deficiencies in the prior art, provide a kind of organic-aqueous mixture to be taken off
The method of water purification, the method overcome organic matters to form azeotropic mixture to be difficult to the bottleneck detached with water, and has low energy
Consumption, small investment, it is simple for process the advantages that.
The technical solution adopted by the present invention to solve the technical problems is：
A kind of method that organic-aqueous mixture carries out dehydration purification, including：
1) inert gas is humidified：Inert gas is sent into after being pressurized with gas compressor from humidification tower bottom, organic-aqueous mixed
It closes object at the top of conditioning Tower to enter, organic-aqueous mixture is in conditioning Tower by being changed into gas phase simultaneously after fluid distribution means
Be evenly distributed in inert gas, using the organic-aqueous mixture to inert gas be humidified with obtain organic-aqueous mixture and
The humidification mixed gas of inert gas, and sent out from humidification column overhead；Tower reactor waste liquid sends out otherwise processed；
2) desorption and regeneration and the cooling of the regenerative adsorption tank of heat：The mixed gas that is humidified is after humidification column overhead submitting by heater
Heating, to make the humidification mixed gas have the stronger desorption and regeneration ability for adsorbent, at this time be humidified mixed gas into
Enter regenerative adsorption tank, by fixed bed of sorbent layer, to carry out desorption and regeneration to the adsorbent for being saturated absorption, from adsorbent
The mixture being desorbed enters condenser with gaseous state together with humidification mixed gas, is mixed rich in water through cooling obtained liquid phase
Solution is closed, is discharged after being collected in intermediate knockout drum, mixed gas after cooling continues to be sent to separation adsorption tanks and adsorbed；It is de-
The humidification mixed gas that the regenerative adsorption tank of heat is sent out with conditioning Tower after the completion of attached regeneration cools down, and the humidification for taking heat out of is mixed
It closes to continue after gas condensed device cooling to be sent to separation adsorption tanks and be adsorbed；
As needed, regenerative adsorption tank can be standby, that is, the mixed gas that is humidified can directly be sent after being sent out from humidification column overhead
It is adsorbed toward separation adsorption tanks；
3) Gas Phase Adsorption detaches：The mixed gas after cooling come from regenerative adsorption tank enters separation adsorption tanks, passes through and inhales
Attached dose of fixed bed, mixed gas are inhaled by organic matter when the fixed bed of sorbent layer relative to water and impurity organic matter are less
It is attached, and the organic matter that is adsorbed of part can also by subsequent gases water and impurity organic matter cement out, i.e. gaseous mixture
During body passes through fixed bed of sorbent layer, water and impurity organic matter are selectively adsorbed and are trapped in fixed bed of sorbent layer
On, remaining inert gas and the organic gas containing high concentration target product organic matter then pass through fixed bed of sorbent layer to step
It is rapid 4)；After absorption, the adsorbent of adsorption saturation will carry out desorption and regeneration；
4) cryogenic condensation：In step 3) mixed gas after adsorbent adsorbs enter condenser, remaining inert gas and
Organic gas containing high concentration target product organic matter is through sub-cooled and enters knockout drum progress gas-liquid separation, obtains
Liquid phase be dewatered high-purity target product organic matter, obtained gas phase be the inert gas containing micro-content organism；
5) inert gas recycles：Inert gas of the step 4) containing micro-content organism returns to step 1) through gas compressor supercharging
Carry out cycling and reutilization.
In one embodiment：Step 2) the desorption and regeneration is identical using at least two as step 3) Gas Phase Adsorption separation process
Adsorption tanks compose in parallel absorbing unit to carry out, which is inhaled in regenerative adsorption tank with detaching by switching
Conversion is recycled between attached tank, rest part adsorption tanks are made while partial adsorbates tank carries out Gas Phase Adsorption separation as separation adsorption tanks
Desorption and regeneration is carried out for regenerative adsorption tank；Adsorption time can according to the combined situations of different adsorbents, the amount of fill of adsorbent with
And the situation of gas determines, which is industry routine techniques.
In one embodiment：The organic-aqueous mixture at least contains target product organic matter and water, the mass fraction of water
≤ 20%, and the organic-aqueous mixture is liquid phase or gas phase.
In one embodiment：In the organic-aqueous mixture, target product organic matter is that can generate the organic of azeotropic with water
Object, such as methyl acetate, isopropanol.
In one embodiment：In the organic-aqueous mixture, target product organic matter is methyl acetate, the mass fraction of water
It is 1.5~10%, further includes impurity organic matter, such as benzene class and alcohols etc. in the organic-aqueous mixture.
In one embodiment：Dew-point temperature≤150 DEG C of step 1) the humidification mixed gas, gas dew point pass through temperature tune
Device is controlled to regulate and control.
In one embodiment：The temperature of the step 2) desorption and regeneration is 100~300 DEG C and higher than the dew of humidification mixed gas
Point temperature.
In one embodiment：The adsorbent is to have the porous material that preferentially selective sorption acts on, the porosity to water
Material is at least one of activated alumina, molecular sieve, silica gel, zeolite；The fixed bed of sorbent layer is single adsorption agent
Fixed bed or the compound fixed bed of a variety of adsorbents.
In one embodiment：Operation temperature≤150 DEG C of step 3) the Gas Phase Adsorption separation, operating pressure is not less than normal
Pressure.
In one embodiment：Humidification mixed gas is directly entered separation adsorption tanks after conditioning Tower submitting and carries out Gas Phase Adsorption point
From；In the step 2) desorption and regeneration, regenerative adsorption tank is by the independent inert gas purge circulatory system to being saturated absorption
Adsorbent carries out desorption and regeneration；Regenerative adsorption tank realizes that mutual circulation is converted with adsorption tanks are detached by switching.
Inert gas of the present invention is industry term, refers to chemical property stabilization, do not react with raw material and under normal pressure not
The gas easily condensed, such as nitrogen.
Compared with the background art, it has the following advantages that the technical program：
1. the present invention solves azeotropic using the circulatory system of the separation of simple cryogenic absorption and alternating temperature purging desorption and regeneration
Object is difficult to the problem of detaching so that production is stablized.
2. the inert gas that the present invention uses recycles in the entire system, the consumption of a large amount of carrier gas is avoided.
3. the present invention has directly used inert gas in alternating temperature regenerates desorption process, relative to making in traditional temp.-changing adsorption
It is regenerated with superheated steam, saves a large amount of energy.
4. the temperature of desorption and regeneration of the present invention is 100~300 DEG C, opposite traditional handicraft temperature is relatively low, reduces energy consumption.
5. using the present invention, to the organic-aqueous mixture of bi-component, (containing only target product in i.e. organic-aqueous mixture has
Machine object and water) it is detached, the purity of target product organic matter can reach 99.8% or more；To the organic-aqueous mixture of multicomponent
(containing target product organic matter, water and other a small amount of impurity organic matters in i.e. organic-aqueous mixture) is detached, target production
The purity of product organic matter can reach 99.5% or more.
Description of the drawings
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is used to illustrate the process flow diagram of one embodiment of the invention.
Fig. 2 is used to illustrate the process flow diagram of another embodiment of the present invention.
Reference numeral：1- conditioning Towers, 2- regenerative adsorption tanks, 3- detach adsorption tanks, the centres 4- knockout drum, 5- gas-liquid separations
Tank, 6- gas compressors, 7- primary heaters, 8- secondary heaters, the first condensers of 9-, the second condensers of 10-, 11- air blast
Machine；The organic-aqueous mixtures of A-, B- inert gases, C- are rich in water mixed solution, D- high-purity target product organic matters, and E- gives up
Liquid.
Specific implementation mode
Present disclosure is illustrated below by embodiment：
Using the present invention a kind of organic-aqueous mixture carry out dehydration purification method, from the waste liquid containing methyl acetate/
High-purity methyl acetate in exhaust gas, in the waste liquid/exhaust gas containing methyl acetate, target product organic matter is tumer
The mass fraction of ester, water is 1.5~10%, further includes a small amount of impurity organic matter such as benzene class and alcohols etc..
Fig. 1 is please referred to, concrete technology flow process is as follows：
1) inert gas is humidified：It is sent into from 1 bottom of conditioning Tower after inert gas B is pressurized with gas compressor 6, gas pressure
The heating for inert gas of primary heater 7 is equipped with after contracting machine 6；Organic-aqueous mixture A (is to contain acetic acid in the present embodiment
Waste liquid/exhaust gas of methyl esters) enter from 1 top of conditioning Tower, it is changed into gas phase simultaneously after conditioning Tower 1 is interior by fluid distribution means
It is evenly distributed in inert gas B, using the organic-aqueous mixture A to inert gas B humidifications to obtain organic-aqueous mixing
The humidification mixed gas of object A and inert gas B, which is saturated gas and dew-point temperature≤100 DEG C, from humidification
1 tower top of tower is sent out；Tower reactor waste liquid E sends out otherwise processed；
2) desorption and regeneration and the cooling of the regenerative adsorption tank of heat：The mixed gas that is humidified is after the submitting of 1 tower top of conditioning Tower by second
Heater 8 is heated to 100~300 DEG C, far above humidification mixed gas dew-point temperature, to make the humidification mixed gas have compared with
The strong desorption and regeneration ability for adsorbent, the mixed gas that is humidified at this time are entered by the bottom of regenerative adsorption tank 2, from the bottom up
By fixed bed of sorbent layer, superficial gas velocity is to be regenerated to the adsorbent of adsorption saturation less than 10m/s；From adsorbent
The upper mixture being desorbed is cold into first together with original humidification mixed gas with gaseous state mainly including water and impurity organic matter
Condenser 9, extremely consistent with 1 Outlet Gas Temperature of conditioning Tower through sub-cooled, obtained liquid phase is rich in water mixed solution C (this reality
Apply in example is the methyl acetate rich in water), it is discharged after being collected in intermediate knockout drum 4, mixed gas after cooling continues to send
It is adsorbed toward adsorbing separation tank 3；
After the completion of desorption and regeneration, the temperature of regenerative adsorption tank is higher, is not suitable for being immediately used to adsorb, with humidification in step 1)
The humidification mixed gas that tower is sent out is sent into hot regenerative adsorption tank 2 and cools down, and takes the humidification mixed gas of heat out of again through the
Separation adsorption tanks 3 are sent to after the cooling of one condenser 9 to be adsorbed；
As needed, regenerative adsorption tank 2 can be standby, that is, the mixed gas that is humidified can be direct after the submitting of 1 tower top of conditioning Tower
Separation adsorption tanks 3 are sent to be adsorbed；
3) Gas Phase Adsorption detaches：Enter separation adsorption tanks from top from the mixed gas after cooling of regenerative adsorption tank 2
3, it is less than 10m/s to pass through fixed bed of sorbent layer, superficial gas velocity from top to bottom, and the adsorbent is to have preferential selection to inhale in water
The porous material of attached effect, the porous material are at least one of activated alumina, molecular sieve, silica gel, zeolite；Institute
It is single adsorption agent fixed bed or the compound fixed bed of a variety of adsorbents to state fixed bed of sorbent layer；Methyl acetate passes through the suction
It is adsorbed when attached dose of fixed bed relative to water and impurity organic matter are less, and the methyl acetate that is adsorbed of part can also be by
Water and impurity organic matter in subsequent gases cement out, i.e. mixed gas by during fixed bed of sorbent layer, water and
Impurity organic matter, which is selectively adsorbed, to be trapped on fixed bed of sorbent layer, remaining inert gas and contain high concentration target
The organic gas of product organic matter then passes through fixed bed of sorbent layer to step 4)；In this step, operation temperature≤150 DEG C, behaviour
Make pressure and is not less than normal pressure；After absorption, stop air inlet, valve transfer, separation adsorption tanks 3 at this time are changed into regeneration suction
Attached tank will subsequently enter from the humidification mixed gas of conditioning Tower 1 from the bottom up, and the adsorbent of adsorption saturation will be mixed with the humidification
It closes gas and carries out desorption and regeneration；That is, the step 2) desorption and regeneration uses two phases with step 3) Gas Phase Adsorption separation process
Same adsorption tanks compose in parallel absorbing unit to carry out, and adsorption process is using continuous absorption, and two adsorption tanks by setting in advance
Fixed digital relay and solenoid valve control switching in regenerative adsorption tank to convert with detaching to recycle between adsorption tanks, an absorption
Another adsorption tanks carries out desorption and regeneration as regenerative adsorption tank while tank carries out Gas Phase Adsorption separation as separation adsorption tanks；
It is used alternatingly by two the rational of adsorption tanks, to realize the continuous production of high-purity methyl acetate.
4) cryogenic condensation：Mixed gas enters the second condenser 10, remaining inertia after adsorbent adsorbs in step 3)
Gas and organic gas containing high concentration target product organic matter enter knockout drum 5 and carry out gas-liquid separation after cooling,
Obtained liquid phase is that dewatered high-purity target product organic matter D (is high-purity methyl acetate in the present embodiment, through inspection
Survey, purity is >=99.5%, and water content is reduced to≤0.5%), obtained gas phase is inert gas B；
5) inert gas recycles：The inert gas B that step 4) obtains returns to step 1) through the supercharging of gas compressor 6 and is followed
Ring recycles, which regards using energy source situation, and any position being configurable in the circulatory system carries out
Supercharging, and be not limited to this embodiment.
Fig. 2 show another embodiment of the present invention, it with the present embodiment institute the difference is that：Step 2) desorption and regeneration
Being detached with step 3) Gas Phase Adsorption can be carried out at the same time by way of in parallel：The mixed gas that is humidified is direct after conditioning Tower submitting
Gas Phase Adsorption separation is carried out into separation adsorption tanks；In the step 2) desorption and regeneration, regenerative adsorption tank is by independent indifferent gas
Body purges the circulatory system and carries out desorption and regeneration to the adsorbent for being saturated absorption；Regenerative adsorption tank with detach adsorption tanks by cutting
It changes to realize that mutual circulation is converted.Fig. 2 is please referred to, procedure declaration is as follows：
Humidification mixed gas is directly entered separation adsorption tanks 3 after the submitting of 1 tower top of conditioning Tower, passes through adsorbent from bottom to top
Fixed bed, superficial gas velocity are to be selectively adsorbed less than 10m/s, water and impurity organic matter and be trapped in fixed bed of sorbent layer
On, obtained mixed gas enters the second condenser 10, and entering knockout drum 5 after cooling carries out gas-liquid separation, obtains
Liquid phase is dewatered high-purity target product organic matter D, and obtained gas phase is inert gas B, be can transport to gas pressure
Contracting machine 6 is to recycle in step 1) inert gas humidification.
Regenerative adsorption tank 2 is regenerated by inert gas B while adsorbing separation.Inert gas B is sent through air blower 11
Enter secondary heater 8 and be heated to 100~250 DEG C, enters regenerative adsorption tank 2 later from top to bottom by being saturated the suction of absorption
Attached dose of fixed bed, regenerates adsorbent, and superficial gas velocity is less than 10m/s.Obtained gas is cold through the first condenser 9
But after, the recycling of air blower 11 is entered after isolating liquid phase by intermediate knockout drum 4.
Certainly, the desorption mode of other well-known dried-air driers can also be used in the regeneration of regenerative adsorption tank,
It is not limited with the embodiment of the present invention, such as is regenerated with the exit gas of a small amount of separation adsorption tanks, detaches adsorption tanks
Exit gas distribute that a small amount of carry out can be to being saturated the adsorbent bed of absorption after heating under reduced pressure in regenerative adsorption tank
Desorption and regeneration is carried out, isolates the mixing liquid rich in water after obtained mixed gas is condensed, gas will be discharged.Due to row
Organic gas can be contained in the gas put, need for further processing or recycling, so it is not recommended that in this way to bed into
Row desorption and regeneration.
The method that a kind of organic-aqueous mixture of the present invention carries out dehydration purification overcomes organic matter and water forms azeotropic
The separation bottleneck of object, can be easily and efficiently from waste liquid/exhaust gas containing methyl acetate of the industry such as polyvinyl alcohol, terephthalic acid (TPA)
Middle high-purity methyl acetate, realizes the continuous production of high-purity methyl acetate, is carried for the production of high-purity methyl acetate
A new path is supplied.
The method that a kind of organic-aqueous mixture of the present invention carries out dehydration purification, for the organic-aqueous mixture of bi-component
(containing only target product organic matter and water in i.e. organic-aqueous mixture) is detached, and the purity of target product organic matter is reachable
To 99.8% or more；(target product organic matter, water are contained for the organic-aqueous mixture of multicomponent in i.e. organic-aqueous mixture
With other a small amount of impurity organic matters) it is detached, the purity of target product organic matter can reach 99.5% or more.
The above, only present pre-ferred embodiments, therefore cannot limit the scope of implementation of the present invention according to this, i.e., according to
Equivalent changes and modifications made by the scope of the claims of the present invention and description all should still belong in the range of the present invention covers.
Claims (10)
1. a kind of method that organic-aqueous mixture carries out dehydration purification, it is characterised in that：Including：
1) inert gas is humidified：It is sent into from humidification tower bottom after inert gas supercharging, organic-aqueous mixture is at the top of conditioning Tower
Into organic-aqueous mixture is changed into gas phase in conditioning Tower and is evenly distributed in inert gas, organic-aqueous using this
Mixture is humidified to obtain the humidification mixed gas of organic-aqueous mixture and inert gas to inert gas, and from conditioning Tower tower
It sends out on top；
2) desorption and regeneration and the cooling of the regenerative adsorption tank of heat：Humidification mixed gas heats after being sent out from humidification column overhead, enters back into
Regenerative adsorption tank, by fixed bed of sorbent layer to carry out desorption and regeneration, the temperature of desorption and regeneration to the adsorbent for being saturated absorption
Degree is 100~300 DEG C；Be desorbed from adsorbent the mixture that gets off with gaseous state together with humidification mixed gas through cooling, obtain
Liquid phase be rich in water mixed solution, mixed gas after cooling continues to be sent to separation adsorption tanks and is adsorbed；Desorption and regeneration is complete
The humidification mixed gas that the regenerative adsorption tank of Cheng Houre is sent out with conditioning Tower cools down, and takes the humidification mixed gas warp of heat out of
Continue to be sent to separation adsorption tanks after cooling to be adsorbed；
3) Gas Phase Adsorption detaches：The mixed gas after cooling come from regenerative adsorption tank enters separation adsorption tanks, passes through adsorbent
Fixed bed, the water in mixed gas are adsorbed by adsorbent, 4) remaining inert gas and organic gas enter step；
4) cryogenic condensation：Mixed gas is after adsorbent adsorbs in step 3), remaining inert gas and organic gas are through low temperature
It cools down and enters knockout drum and carry out gas-liquid separation, obtained liquid phase is dewatered high-purity target product organic matter, is obtained
The gas phase arrived is the inert gas containing micro-content organism；
5) inert gas recycles：Inert gas of the step 4) containing micro-content organism returns to step 1) through supercharging and is recycled profit again
With.
2. the method that a kind of organic-aqueous mixture according to claim 1 carries out dehydration purification, it is characterised in that：It is described
Step 2) desorption and regeneration composes in parallel absorption list with step 3) Gas Phase Adsorption separation process using at least two identical adsorption tanks
Member carries out, which is converted in regenerative adsorption tank with detaching to recycle between adsorption tanks by switching, and part is inhaled
Rest part adsorption tanks are desorbed as regenerative adsorption tank while attached tank carries out Gas Phase Adsorption separation as separation adsorption tanks
Regeneration.
3. the method that a kind of organic-aqueous mixture according to claim 1 carries out dehydration purification, it is characterised in that：It is described
Organic-aqueous mixture at least contains target product organic matter and water, mass fraction≤20% of water, and the organic-aqueous mixing
Object is liquid phase or gas phase.
4. the method that a kind of organic-aqueous mixture according to claim 3 carries out dehydration purification, it is characterised in that：It is described
In organic-aqueous mixture, target product organic matter is the organic matter that azeotropic can be generated with water.
5. the method that a kind of organic-aqueous mixture according to claim 4 carries out dehydration purification, it is characterised in that：It is described
In organic-aqueous mixture, target product organic matter is methyl acetate, and the mass fraction of water is 1.5~10%, described organic to contain
It further include impurity organic matter in aqueous mixtures.
6. the method that a kind of organic-aqueous mixture according to claim 1 carries out dehydration purification, it is characterised in that：It is described
Dew-point temperature≤150 DEG C of step 1) humidification mixed gas.
7. the method that a kind of organic-aqueous mixture according to claim 6 carries out dehydration purification, it is characterised in that：It is described
The temperature of step 2) desorption and regeneration is 100~300 DEG C and higher than the dew-point temperature of the humidification mixed gas described in claim 6.
8. the method that a kind of organic-aqueous mixture according to claim 1 carries out dehydration purification, it is characterised in that：It is described
Adsorbent be to water have preferentially selective sorption act on porous material, the porous material be activated alumina, molecular sieve,
At least one of silica gel, zeolite；The fixed bed of sorbent layer is that single adsorption agent fixed bed or a variety of adsorbents are compound
Fixed bed.
9. the method that a kind of organic-aqueous mixture according to claim 1 carries out dehydration purification, it is characterised in that：It is described
Operation temperature≤150 DEG C of step 3) Gas Phase Adsorption separation, operating pressure are not less than normal pressure.
10. the method that a kind of organic-aqueous mixture according to claim 1 carries out dehydration purification, it is characterised in that：Increase
Wet mixture body is directly entered separation adsorption tanks after conditioning Tower submitting and carries out Gas Phase Adsorption separation；Step 2) the desorption and regeneration
In, regenerative adsorption tank carries out desorption and regeneration by the independent inert gas purge circulatory system to the adsorbent for being saturated absorption；Again
Raw adsorption tanks realize that mutual circulation is converted with adsorption tanks are detached by switching.
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