CN105732378A - Organic water-containing mixture dehydration purification method - Google Patents

Organic water-containing mixture dehydration purification method Download PDF

Info

Publication number
CN105732378A
CN105732378A CN201410742615.1A CN201410742615A CN105732378A CN 105732378 A CN105732378 A CN 105732378A CN 201410742615 A CN201410742615 A CN 201410742615A CN 105732378 A CN105732378 A CN 105732378A
Authority
CN
China
Prior art keywords
organic
gas
aqueous mixture
adsorption
desorption
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201410742615.1A
Other languages
Chinese (zh)
Other versions
CN105732378B (en
Inventor
谭伟业
庄庆彬
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xiamen Weijie Chemical Industry Engineering Co Ltd
Original Assignee
Xiamen Weijie Chemical Industry Engineering Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xiamen Weijie Chemical Industry Engineering Co Ltd filed Critical Xiamen Weijie Chemical Industry Engineering Co Ltd
Priority to CN201410742615.1A priority Critical patent/CN105732378B/en
Publication of CN105732378A publication Critical patent/CN105732378A/en
Application granted granted Critical
Publication of CN105732378B publication Critical patent/CN105732378B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Separation Of Gases By Adsorption (AREA)
  • Drying Of Gases (AREA)

Abstract

The invention discloses an organic water-containing mixture dehydration purification method and belongs to the technical field of organic material preparation. According to the method, a high purity micro-water organic material is prepared through circulation inert gas as a carrier and a closed circulation system of inert gas humidification, desorption regeneration, gas phase adsorption separation and low temperature condensation, and two or more parallel adsorption tank cyclic switching realizes desorption regeneration and gas phase adsorption separation. The method is especially suitable for dehydration of azeotrope of water and organic matters such as methyl acetate or isopropanol, solves the problem that dehydration purification is not finished by distillation because of azeotropy and the traditional pure liquid phase adsorption dehydration method has large energy consumption and a short adsorbent life, and provides a treatment process with the advantages of no gas phase discharge, environmental friendliness, simpleness, high efficiency and low price.

Description

A kind of method that organic-aqueous mixture carries out dehydration purification
Technical field
The invention belongs to organic material preparation technique scope, the method that especially a kind of organic-aqueous mixture carries out dehydration purification.
Background technology
Commercial production has in a lot of raw material, intermediate product and product and all contain water and the moisture reason being to cause further processing procedure high energy consumption, poor efficiency, difficult treatment.For the organic-aqueous mixture of liquid phase, traditional processing method has rectification, extraction, absorption etc., but for some special systems, Organic substance and water can form azeotropic mixture, cause difficult treatment or feasible separating technology complexity, energy consumption is high, it is difficult to obtain highly purified Organic substance.
Existing patent and document one are to utilize liquid phase adsorption process, the separation of the organic-aqueous mixture of liquid phase can be realized, its technique mainly includes adsorbing separation, alternating temperature purges two parts of desorption and regeneration, its process is: mixture enters adsorption tower, by having the bed of selective absorption, moisture therein is selectively adsorbed, and obtains the organic products that purity is higher;Saturated adsorbent bed first emptying is replaced with water or steam again, then with hot dry air, adsorbent is regenerated, can adsorb again after cooling.Utilizing the method to process moisture organic mixture, having the drawback that in process to produce substantial amounts of organic liquid mixture needs recycling, and vapours consumption is big, and the temperature of desorption and regeneration is higher.
Another kind is to utilize superheated steam phase adsorption method, the separation of the organic-aqueous mixture of vapor phase can be realized, its technique mainly includes adsorbing separation condensation and obtains product and two parts of desorption and regeneration, technological process relative to liquid phase adsorption, solve in liquid phase adsorption regeneration and produce the problem that substantial amounts of organic liquid mixture needs recycling, the factors such as single consideration system pressure drop is overheated with vaporization, therefore can only adsorb at the temperature higher than organic mixture boiling point.Be limited to the adsorbent restriction that absorbability is low when high temperature, also therefore can organic liquid mixture also restrained.
For methyl acetate: methyl acetate is a kind of important solvent and Organic Chemicals, often occur in a large number with the form of side-product in the industry, such as in the industrial processes of p-phthalic acid (PTA), all can produce to contain in a large number the industrial wastes/waste gas of methyl acetate.Generally, the production of polyvinyl alcohol per ton all can the methyl acetate of by-product 1.7 tons, the PTA process units of every 1 ton all can produce the methyl acetate of 6 kilograms forming with the azeotropic of about 95% purity to be existed.The many employings of factory are back to the mode of technique and reclaim, and too much then entrance waste gas removes to CC Catalytic Converter, also have part factory to use hydrolysis to manufacture the output value compared with the acetic acid of methyl acetate its cheap market price and methanol.The purity of the methyl acetate required in the market is more than 99.5%, the market price of this high-purity methyl acetate of 99.5% is high compared to the methyl acetate of about 95% purity 30~40%, so separating and recovering methyl acetate from industry byproduct, existing important environment protection significance, has again good using value and economic benefit.But possibly together with impurity such as first alcohol and waters in these methyl acetate waste liquid/waste gas, owing to methyl acetate and water, methanol are easily formed azeotropic mixture, it are difficult to separation with common rectificating method and obtain highly purified methyl acetate.At present, for the recoverying and utilizing method of polyvinyl alcohol and p-phthalic acid's production process by-product methyl acetate, mainly there are 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 the market demand that the raw material of the commercial synthesis of methyl acetate is exactly acetic acid and methanol and high-purity methyl acetate day by day increases, and the method does not have what economic benefit and social benefit;Extraction fractional distillation energy consumption is high, and Solvent quantity is big, and purity is not high;Salt separation method separating effect is better and energy consumption is relatively low, but complex process;Utilize membrane separation technique to be also difficult to obtain high-purity methyl acetate, utilize traditional Temp .-changing adsorption method, it is necessary to use substantial amounts of steam to hot-air, adsorbent to be regenerated, so energy consumption aspect is also of a relatively high.Therefore, the environmental protection needing a kind of mixture forming azeotropic mixture for organic-aqueous mixture, particularly Organic substance and water badly is simple, the dehydration purification processes technique of high efficiency low cost, to solve current industrial preparation high-purity Organic substance technical barrier.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art part, provide a kind of method that organic-aqueous mixture carries out dehydration purification, the method overcome Organic substance and water and form azeotropic mixture thus being difficult to the bottleneck separated, and there is the advantages such as low energy consumption, small investment, technique are simple.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of method that organic-aqueous mixture carries out dehydration purification, including:
1) noble gas humidification: noble gas is sent into bottom conditioning Tower with after gas compressor supercharging, organic-aqueous mixture enters from conditioning Tower top, organic-aqueous mixture is all changed into gas phase by after fluid distribution means and is evenly distributed in noble gas in conditioning Tower, utilize this organic-aqueous mixture to the noble gas humidification humidification mixing gas to obtain organic-aqueous mixture and noble gas, and send from conditioning Tower tower top;Tower reactor waste liquid sends otherwise processed;
2) the regenerative adsorption tank cooling of desorption and regeneration and heat: humidification mixing gas is heated by heater after sending from conditioning Tower tower top, so that this humidification mixing gas has the stronger desorption and regeneration ability for adsorbent, now humidification mixing gas enters regenerative adsorption tank, by fixed bed of sorbent layer, desorption and regeneration is carried out with the adsorbent to saturated absorption, the mixture got off from desorption adsorbent enters condenser with gaseous state together with humidification mixing gas, the cooled liquid phase obtained is for rich in water mixed solution, discharge after collecting in middle knockout drum, mixing gas after cooling continues to be sent to separation adsorption tanks and adsorbs;Desorption and regeneration completes the humidification mixing gas that the regenerative adsorption tank conditioning Tower of after heat sends and lowers the temperature, and continues to be sent to separation adsorption tanks and adsorb after taking the condensed device cooling of humidification mixing gas of heat out of;
As required, regenerative adsorption tank can be standby, and the mixing gas that is namely humidified can be routed directly to separation adsorption tanks after sending from conditioning Tower tower top and adsorb;
3) Gas Phase Adsorption separates: the mixing gas after the cooling that regenerative adsorption tank comes enters and separates adsorption tanks, through fixed bed of sorbent layer, when mixing gas is by this fixed bed of sorbent layer, Organic substance is less relative to water and impurity Organic substance adsorbed, and the Organic substance that part is adsorbed can also be cemented out by the water in subsequent gases and impurity Organic substance, namely mixing gas is in the process of fixed bed of sorbent layer, water and impurity Organic substance are selectively adsorbed and are trapped on fixed bed of sorbent layer, remaining noble gas and then pass through fixed bed of sorbent layer to step 4 containing the organic organic gas of high concentration target product);Absorption is adsorbed saturated adsorbent and will be carried out desorption and regeneration after terminating;
4) condensation at low temperature: step 3) in mixing gas after adsorbent, enter condenser, remaining noble gas and through sub-cooled containing the organic organic gas of high concentration target product and enter knockout drum and carry out gas-liquid separation, the liquid phase obtained is the high-purity target product Organic substance after dehydration, and the gas phase obtained is the noble gas containing micro-content organism;
5) noble gas circulation: step 4) noble gas containing micro-content organism returns to step 1 through gas compressor supercharging) it is circulated recycling.
In one embodiment: described step 2) desorption and regeneration and step 3) Gas Phase Adsorption separation process adopts the adsorption tanks that at least two is identical to compose in parallel absorbing unit to carry out, these at least two adsorption tanks are by switching to change with separating circulation between adsorption tanks at regenerative adsorption tank, and partial adsorbates tank carries out desorption and regeneration as separating remainder adsorption tanks while adsorption tanks carry out Gas Phase Adsorption separation as regenerative adsorption tank;Adsorption time can determine according to the different combined situation of adsorbent, the amount of fill of adsorbent and the situation of gas, and this determining method is industry routine techniques.
In one embodiment: described organic-aqueous mixture at least contains target product Organic substance and water, mass fraction≤20% of water, and this organic-aqueous mixture is liquid phase or gas phase.
In one embodiment: in described organic-aqueous mixture, target product Organic substance is can produce the Organic substance of azeotropic with water, for instance methyl acetate, isopropanol.
In one embodiment: in described organic-aqueous mixture, target product Organic substance is methyl acetate, and the mass fraction of water is 1.5~10%, also includes impurity Organic substance, for instance benzene class and alcohols etc. in described organic-aqueous mixture.
In one embodiment: described step 1) being humidified mixes dew point temperature≤150 DEG C of gas, and gas dew point is regulated and controled by temperature control device.
In one embodiment: described step 2) temperature of desorption and regeneration is 100~300 DEG C and dew point temperature higher than humidification mixing gas.
In one embodiment: described adsorbent is the porous material that water has preferentially selective sorption effect, and described porous material is at least one in activated alumina, molecular sieve, silica gel, zeolite;Described fixed bed of sorbent layer is single adsorption agent fixed bed or multiple adsorbent compound fixed bed.
In one embodiment: described step 3) Gas Phase Adsorption separate operation temperature≤150 DEG C, operation pressure be not less than normal pressure.
In one embodiment: humidification mixing gas is directly entered separation adsorption tanks after sending from conditioning Tower and carries out Gas Phase Adsorption separation;Described step 2) in desorption and regeneration, the adsorbent of saturated absorption is carried out desorption and regeneration by independent inert gas purge blood circulation by regenerative adsorption tank;Regenerative adsorption tank is changed to realize mutual circulation by switching with separating adsorption tanks.
Noble gas of the present invention is industry term, refers to stable chemical nature, not with the gas that not easily condenses under raw material reaction and normal pressure, such as nitrogen etc..
The technical program is compared with background technology, and it has the advantage that
1. the present invention adopts simple cryogenic absorption to separate and the blood circulation of alternating temperature purging desorption and regeneration, solves the problem that azeotropic mixture is difficult to separate so that produce stable.
2. the noble gas that the present invention adopts recycles in the entire system, it is to avoid the consumption of a large amount of carrier gas.
3. the present invention regenerates in desorption process at alternating temperature and directly employs noble gas, uses superheated steam to regenerate relative in tradition Temp .-changing adsorption, saves the substantial amounts of energy.
4. the temperature of desorption and regeneration of the present invention is 100~300 DEG C, and relatively conventional technological temperature is relatively low, reduces energy consumption.
5. utilizing the present invention that the organic-aqueous mixture of bi-component (namely containing only having target product Organic substance and water in organic-aqueous mixture) is easily separated, the organic purity of target product can reach more than 99.8%;The organic-aqueous mixture of multicomponent (namely containing target product Organic substance, water and other a small amount of impurity Organic substances in organic-aqueous mixture) is easily separated, and the organic purity of target product can reach more than 99.5%.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described.
Fig. 1 is for illustrating the process flow diagram of one embodiment of the invention.
Fig. 2 is for illustrating the process flow diagram of another embodiment of the present invention.
Accompanying drawing labelling: 1-conditioning Tower, 2-regenerative adsorption tank, 3-separates adsorption tanks, knockout drum in the middle of 4-, 5-knockout drum, 6-gas compressor, 7-primary heater, 8-secondary heater, 9-the first condenser, 10-the second condenser, 11-aerator;The organic-aqueous mixture of A-, B-noble gas, C-is rich in water mixed solution, D-high-purity target product Organic substance, E-waste liquid.
Detailed description of the invention
Illustrate present disclosure by the examples below:
Utilize the method that a kind of organic-aqueous mixture of the present invention carries out dehydration purification, high-purity methyl acetate from the waste liquid/waste gas containing methyl acetate, in described waste liquid/waste gas containing methyl acetate, target product Organic substance is methyl acetate, the mass fraction of water is 1.5~10%, also includes a small amount of impurity Organic substance such as benzene class and alcohols etc..
Refer to Fig. 1, concrete technology flow process is as follows:
1) noble gas humidification: noble gas B is sent into after gas compressor 6 supercharging bottom conditioning Tower 1, is provided with primary heater 7 heating for noble gas after gas compressor 6;Organic-aqueous mixture A (is the waste liquid/waste gas containing methyl acetate) and enters from conditioning Tower 1 top in the present embodiment, all it is changed into gas phase by after fluid distribution means and is evenly distributed in noble gas B in conditioning Tower 1, utilize this organic-aqueous mixture A to the noble gas B humidification humidification mixing gas to obtain organic-aqueous mixture A and noble gas B, this humidification mixing gas is saturated gas and dew point temperature≤100 DEG C, sends from conditioning Tower 1 tower top;Tower reactor waste liquid E sends otherwise processed;
2) the regenerative adsorption tank cooling of desorption and regeneration and heat: humidification mixing gas is heated to 100~300 DEG C by secondary heater 8 after sending from conditioning Tower 1 tower top, dew point temperature far above humidification mixing gas, so that this humidification mixing gas has the stronger desorption and regeneration ability for adsorbent, now humidification mixing gas is entered by the bottom of regenerative adsorption tank 2, from the bottom up by fixed bed of sorbent layer, superficial gas velocity is less than 10m/s, regenerates adsorbing saturated adsorbent;The mixture that desorption gets off from adsorbent mainly includes water and impurity Organic substance, the first condenser 9 is entered together with former humidification mixing gas with gaseous state, through sub-cooled to consistent with conditioning Tower 1 Outlet Gas Temperature, the liquid phase obtained is rich in water mixed solution C (being the methyl acetate rich in water in the present embodiment), discharge after collecting in middle knockout drum 4, the mixing gas after cooling continues to be sent to adsorbing separation tank 3 and adsorbs;
After desorption and regeneration completes, the temperature of regenerative adsorption tank is higher, it is not suitable for being immediately used to absorption, by step 1) in the humidification mixing gas sent of conditioning Tower send into the regenerative adsorption tank 2 of heat and lower the temperature, take the humidification mixing gas of heat out of and separate adsorption tanks 3 adsorb then through being sent to after the first condenser 9 cooling;
As required, regenerative adsorption tank 2 can be standby, and the mixing gas that is namely humidified can be routed directly to separation adsorption tanks 3 after sending from conditioning Tower 1 tower top and adsorb;
3) Gas Phase Adsorption separates: enters from the mixing gas after the cooling of regenerative adsorption tank 2 from top and separates adsorption tanks 3, from top to bottom through fixed bed of sorbent layer, superficial gas velocity is less than 10m/s, described adsorbent is the porous material that water has preferentially selective sorption effect, and described porous material is at least one in activated alumina, molecular sieve, silica gel, zeolite;Described fixed bed of sorbent layer is single adsorption agent fixed bed or multiple adsorbent compound fixed bed;Methyl acetate passes through during this fixed bed of sorbent layer less relative to water and impurity Organic substance adsorbed, and the methyl acetate that part is adsorbed can also be cemented out by the water in subsequent gases and impurity Organic substance, namely mixing gas is in the process of fixed bed of sorbent layer, water and impurity Organic substance are selectively adsorbed and are trapped on fixed bed of sorbent layer, remaining noble gas and then pass through fixed bed of sorbent layer to step 4 containing the organic organic gas of high concentration target product);In this step, operating temperature≤150 DEG C, operation pressure is not less than normal pressure;After absorption terminates, stopping air inlet, valve transfer, namely separation adsorption tanks 3 now are changed into regenerative adsorption tank, and the follow-up humidification mixing gas from conditioning Tower 1 will enter from the bottom up, and adsorbing saturated adsorbent will carry out desorption and regeneration with this humidification mixing gas;Namely, described step 2) desorption and regeneration and step 3) Gas Phase Adsorption separation process adopts two identical adsorption tanks to compose in parallel absorbing unit to carry out, adsorption process adopts absorption continuously, these two adsorption tanks control switching to change with separating circulation between adsorption tanks at regenerative adsorption tank by digital relay set in advance and electromagnetic valve, and adsorption tanks carry out desorption and regeneration as separating another adsorption tanks while adsorption tanks carry out Gas Phase Adsorption separation as regenerative adsorption tank;By being reasonably used alternatingly of two adsorption tanks, thus realizing the continuous production of high-purity methyl acetate.
4) condensation at low temperature: step 3) in mixing gas after adsorbent, enter the second condenser 10, remaining noble gas and enter knockout drum 5 after cooling carry out gas-liquid separation containing the organic organic gas of high concentration target product, the liquid phase obtained be dehydration after high-purity target product Organic substance D (the present embodiment is high-purity methyl acetate, after testing, purity is >=99.5%, water content is reduced to≤0.5%), the gas phase obtained is noble gas B;
5) noble gas circulation: step 4) the noble gas B that obtains returns to step 1 through gas compressor 6 supercharging) it is circulated recycling, utilization of energy situation looked by this pressurizer gas compressor 6, it is configurable on the optional position in blood circulation and carries out supercharging, be not limited with the present embodiment.
Fig. 2 show another embodiment of the present invention, and it is different in that with the present embodiment: step 2) desorption and regeneration and step 3) Gas Phase Adsorption separates and can mode in parallel carry out simultaneously: humidification mixing gas is directly entered separation adsorption tanks after sending from conditioning Tower and carries out Gas Phase Adsorption separation;Described step 2) in desorption and regeneration, the adsorbent of saturated absorption is carried out desorption and regeneration by independent inert gas purge blood circulation by regenerative adsorption tank;Regenerative adsorption tank is changed to realize mutual circulation by switching with separating adsorption tanks.Refer to Fig. 2, procedure declaration is as follows:
Humidification mixing gas is directly entered separation adsorption tanks 3 after sending from conditioning Tower 1 tower top, from bottom to top through fixed bed of sorbent layer, superficial gas velocity is less than 10m/s, water and impurity Organic substance are selectively adsorbed and are trapped on fixed bed of sorbent layer, obtained mixing gas enters the second condenser 10, enter knockout drum 5 after cooling and carry out gas-liquid separation, the liquid phase obtained is the high-purity target product Organic substance D after dehydration, the gas phase obtained is noble gas B, can be delivered to gas compressor 6 to be cycled to used in step 1) noble gas humidification in.
While adsorbing separation, regenerative adsorption tank 2 is regenerated by noble gas B.Noble gas B sends into secondary heater 8 through aerator 11 and heats to 100~250 DEG C, enters regenerative adsorption tank 2 afterwards from top to bottom by the fixed bed of sorbent layer of saturated absorption, adsorbent is regenerated, and superficial gas velocity is less than 10m/s.Obtained gas, after the first condenser 9 cooling, enters into aerator 11 after isolating liquid phase by middle knockout drum 4 and recycles.
Certainly, the regeneration of regenerative adsorption tank may be used without the desorption mode of other well-known dried-air driers, it is not limited with embodiments of the invention, such as regenerate with a small amount of exit gas separating adsorption tanks, the exit gas of separation adsorption tanks distributes after carrying out heating under reduced pressure on a small quantity can carry out desorption and regeneration to the adsorbent bed of saturated absorption in regenerative adsorption tank, obtain mixing gas condensed after isolate the mixing liquid rich in water, gas will be discharged.Owing to the gas of discharge can contain organic gas, it is necessary to be for further processing or reclaim, so it is not recommended that in this way bed being carried out desorption and regeneration.
A kind of organic-aqueous mixture of the present invention carries out the method for dehydration purification and overcomes Organic substance and the separation bottleneck of water formation azeotropic mixture, can easily and efficiently from polyvinyl alcohol, p-phthalic acid etc. industry the waste liquid/waste gas containing methyl acetate high-purity methyl acetate, achieving the continuous production of high-purity methyl acetate, the production for high-purity methyl acetate provides a new path.
The method that a kind of organic-aqueous mixture of the present invention carries out dehydration purification, being easily separated for the organic-aqueous mixture of bi-component (namely containing only having target product Organic substance and water in organic-aqueous mixture), the organic purity of target product can reach more than 99.8%;Being easily separated for the organic-aqueous mixture of multicomponent (namely containing target product Organic substance, water and other a small amount of impurity Organic substances in organic-aqueous mixture), the organic purity of target product can reach more than 99.5%.
The above, be only present pre-ferred embodiments, therefore can not limit scope of the invention process according to this, and the equivalence namely made according to the scope of the claims of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.

Claims (10)

1. the method that an organic-aqueous mixture carries out dehydration purification, it is characterised in that: including:
1) noble gas humidification: send into bottom conditioning Tower after noble gas supercharging, organic-aqueous mixture enters from conditioning Tower top, organic-aqueous mixture is changed into gas phase in conditioning Tower and is evenly distributed in noble gas, utilize this organic-aqueous mixture to the noble gas humidification humidification mixing gas to obtain organic-aqueous mixture and noble gas, and send from conditioning Tower tower top;
2) the regenerative adsorption tank cooling of desorption and regeneration and heat: humidification mixing gas sends post-heating from conditioning Tower tower top, enter back into regenerative adsorption tank, desorption and regeneration is carried out with the adsorbent to saturated absorption by fixed bed of sorbent layer, the mixture got off from desorption adsorbent mixes together with gas cooled with gaseous state with humidification, the liquid phase obtained is for rich in water mixed solution, and the mixing gas after cooling continues to be sent to separation adsorption tanks and adsorbs;Desorption and regeneration completes the humidification mixing gas that the regenerative adsorption tank conditioning Tower of after heat sends and lowers the temperature, and takes the humidification mixing gas of heat out of and continues to be sent to separation adsorption tanks after cooling and adsorb;
3) Gas Phase Adsorption separates: the mixing gas after the cooling that regenerative adsorption tank comes enters and separates adsorption tanks, and through fixed bed of sorbent layer, the adsorbed agent absorption of water in mixing gas, remaining noble gas and organic gas enter step 4);
4) condensation at low temperature: step 3) in mixing gas after adsorbent, remaining noble gas and organic gas are through sub-cooled and enter knockout drum and carry out gas-liquid separation, the liquid phase obtained is the high-purity target product Organic substance after dehydration, and the gas phase obtained is the noble gas containing micro-content organism;
5) noble gas circulation: step 4) noble gas containing micro-content organism is intensified returns to step 1) it is circulated recycling.
2. the method that a kind of organic-aqueous mixture according to claim 1 carries out dehydration purification, it is characterized in that: described step 2) desorption and regeneration and step 3) Gas Phase Adsorption separation process adopts the adsorption tanks that at least two is identical to compose in parallel absorbing unit to carry out, these at least two adsorption tanks are by switching to change with separating circulation between adsorption tanks at regenerative adsorption tank, and partial adsorbates tank carries out desorption and regeneration as separating remainder adsorption tanks while adsorption tanks carry out Gas Phase Adsorption separation as regenerative adsorption tank.
3. the method that a kind of organic-aqueous mixture according to claim 1 carries out dehydration purification, it is characterized in that: described organic-aqueous mixture at least contains target product Organic substance and water, mass fraction≤20% of water, and this organic-aqueous mixture 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: in described organic-aqueous mixture, target product Organic substance is can produce the Organic substance of azeotropic with water.
5. the method that a kind of organic-aqueous mixture according to claim 4 carries out dehydration purification, it is characterized in that: in described organic-aqueous mixture, target product Organic substance is methyl acetate, and the mass fraction of water is 1.5~10%, also includes impurity Organic substance in described organic-aqueous mixture.
6. the method that a kind of organic-aqueous mixture according to claim 1 carries out dehydration purification, it is characterised in that: described step 1) being humidified mixes dew point temperature≤150 DEG C of gas.
7. the method that a kind of organic-aqueous mixture according to claim 6 carries out dehydration purification, it is characterised in that: described step 2) temperature of desorption and regeneration is 100~300 DEG C and dew point temperature higher than the humidification mixing 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 characterized in that: described adsorbent is the porous material that water has preferentially selective sorption effect, and described porous material is at least one in activated alumina, molecular sieve, silica gel, zeolite;Described fixed bed of sorbent layer is single adsorption agent fixed bed or multiple adsorbent 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: described step 3) Gas Phase Adsorption separate operation temperature≤150 DEG C, operation pressure be 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: humidification mixing gas is directly entered separation adsorption tanks after sending from conditioning Tower and carries out Gas Phase Adsorption separation;Described step 2) in desorption and regeneration, the adsorbent of saturated absorption is carried out desorption and regeneration by independent inert gas purge blood circulation by regenerative adsorption tank;Regenerative adsorption tank is changed to realize mutual circulation by switching with separating adsorption tanks.
CN201410742615.1A 2014-12-08 2014-12-08 A kind of method that organic-aqueous mixture carries out dehydration purification Active CN105732378B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410742615.1A CN105732378B (en) 2014-12-08 2014-12-08 A kind of method that organic-aqueous mixture carries out dehydration purification

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410742615.1A CN105732378B (en) 2014-12-08 2014-12-08 A kind of method that organic-aqueous mixture carries out dehydration purification

Publications (2)

Publication Number Publication Date
CN105732378A true CN105732378A (en) 2016-07-06
CN105732378B CN105732378B (en) 2018-09-07

Family

ID=56236876

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410742615.1A Active CN105732378B (en) 2014-12-08 2014-12-08 A kind of method that organic-aqueous mixture carries out dehydration purification

Country Status (1)

Country Link
CN (1) CN105732378B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107365246A (en) * 2017-07-26 2017-11-21 四川天采科技有限责任公司 A kind of full temperature journey sorption extraction purification method of hyperpure isopropyl alcohol
CN109970512A (en) * 2017-12-28 2019-07-05 内蒙古伊泰煤基新材料研究院有限公司 The aqueous continuous adsorption dewatering device and method of light alcohol
CN113680171A (en) * 2021-08-27 2021-11-23 惠州市万绿启佳环保科技有限公司 Organic waste gas purification process

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05140036A (en) * 1991-11-15 1993-06-08 Showa Denko Kk Method for purifying ethyl acetate
CN1221775A (en) * 1997-12-31 1999-07-07 中国科学院大连化学物理研究所 Dewatering tech. for microwater in organic solvent
US20020014457A1 (en) * 1998-12-10 2002-02-07 Coker Eric Nicholas Method of dewatering organic liquids
CN102992934A (en) * 2011-09-17 2013-03-27 天华化工机械及自动化研究设计院有限公司 Nitrogen closed-loop cyclic regeneration type propylene dehydration method and device

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2143758A1 (en) * 2008-07-11 2010-01-13 Rohm and Haas Company Process for Making Polymer Composites Having Thermoplastic Properties

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05140036A (en) * 1991-11-15 1993-06-08 Showa Denko Kk Method for purifying ethyl acetate
CN1221775A (en) * 1997-12-31 1999-07-07 中国科学院大连化学物理研究所 Dewatering tech. for microwater in organic solvent
US20020014457A1 (en) * 1998-12-10 2002-02-07 Coker Eric Nicholas Method of dewatering organic liquids
CN102992934A (en) * 2011-09-17 2013-03-27 天华化工机械及自动化研究设计院有限公司 Nitrogen closed-loop cyclic regeneration type propylene dehydration method and device

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107365246A (en) * 2017-07-26 2017-11-21 四川天采科技有限责任公司 A kind of full temperature journey sorption extraction purification method of hyperpure isopropyl alcohol
CN107365246B (en) * 2017-07-26 2020-12-01 四川天采科技有限责任公司 Full-temperature-range adsorption extraction purification method of ultrapure isopropanol
CN109970512A (en) * 2017-12-28 2019-07-05 内蒙古伊泰煤基新材料研究院有限公司 The aqueous continuous adsorption dewatering device and method of light alcohol
CN113680171A (en) * 2021-08-27 2021-11-23 惠州市万绿启佳环保科技有限公司 Organic waste gas purification process

Also Published As

Publication number Publication date
CN105732378B (en) 2018-09-07

Similar Documents

Publication Publication Date Title
CN102179129B (en) Treatment process for absorbed condensate waste gas
CN103447015A (en) Desorption and regeneration method for organic matter adsorbent
CN109126392B (en) Method for carrying out CO (carbon monoxide) in flue gas by adopting ionic liquid2Trapping device and process
CN108744889B (en) VOCs waste gas treatment method combining absorption and adsorption
CN101703869B (en) New method and device for recovering organic solvent from waste gas
CN102049189B (en) Method for purifying organic waste gas
CN102951999B (en) Dewatering method for glycol production process
CN102202761A (en) Recovery and purification process for organic molecules
CN100364643C (en) Method and device for absorbing, recovering and purifying organic from exhaust gas
CN105732378A (en) Organic water-containing mixture dehydration purification method
CN109999618A (en) The separation system and method for carbon dioxide in a kind of mesohigh gas source
CN101555415A (en) Method and apparatus for recovering oil product from oil-containing mixed gas
CN103055655B (en) A kind of processing method of cyclohexane oxidation system tail gas
CN108821253A (en) A kind of purification system and processing method of electron level phosphine
CN103058187A (en) Method for producing improved food-grade liquid carbon dioxide product
CN107774092A (en) A kind of method of sorption extraction separation and purification
CN106866375A (en) A kind of adsorption separating method of the close polyol blends of boiling point
CN218025747U (en) Device for separating and purifying hydrogen isotope wastewater
CN208814656U (en) A kind of purification device of water treatment agent by-product hydrogen chloride
CN104673417B (en) The system and method for precooling and dry decontamination for natural gas from coal
CN102410704B (en) Production method of food grade liquid carbon dioxide product for recycling resurgent gases
CN105771543A (en) Dry purification and recovery device of organic waste gas
JP2012081411A (en) Solvent dehydrator
CN205774203U (en) Organic recovery device in a kind of Synthetic Leather waste gas
CN205570038U (en) Dry cleaning retrieves organic waste gas's device

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant