CN103402596B - Dehydration of organic solvent device - Google Patents
Dehydration of organic solvent device Download PDFInfo
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- CN103402596B CN103402596B CN201280009817.4A CN201280009817A CN103402596B CN 103402596 B CN103402596 B CN 103402596B CN 201280009817 A CN201280009817 A CN 201280009817A CN 103402596 B CN103402596 B CN 103402596B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/08—Thickening liquid suspensions by filtration
- B01D17/10—Thickening liquid suspensions by filtration with stationary filtering elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/08—Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/16—Organic material
- B01J39/18—Macromolecular compounds
- B01J39/20—Macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
- B01D15/361—Ion-exchange
- B01D15/362—Cation-exchange
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Abstract
[problem] provide can realize organic solvent continuous treating, substantially do not need change dehydrating material and from a large amount of organic solvents, stably can remove the device of moisture.[solution] this dehydration of organic solvent device is by importing to dehydrating material by the processed organic solvent containing moisture and making described processed organic solvent contact with described dehydrating material, moisture contained in processed organic solvent is removed in dehydration, wherein, dehydrating material comprises the cationic ion-exchange resin with spherical shape, in dehydrating material, the particle diameter of cationic ion-exchange resin is the particle rate of below 0.4mm is more than 90%.
Description
Technical field
The present invention relates to the device sloughing moisture from organic solvent, especially at the dehydration of organic solvent device using solvent recovery unit to use from the dehydration of the organic solvent reclaimed containing organic solvent gas produced by various factory, research facilities etc.
Background technology
All the time, by the device of solvent dehydration, distillation refining plant is widely used as removing moisture from organic solvent.Namely following device: solvothermal is evaporated, utilizes the difference of boiling point by organic solvent and moisture fractionation, thus the high organic solvent of purity can be obtained.
Distillation refining plant is large-scale device, and therefore need broad installation space, and initial cost, operating cost are all high, this becomes problem.In order to solve the problem, known being passed to by organic solvent in the drench pit being filled with the dehydrating materials such as zeolite, ion exchange resin, molecular sieve, activated alumina carrys out dewatered method (for example, referring to patent document 1).
But from a large amount of organic solvent Separation of Water timesharing, need a large amount of dehydrating materials, dehydrating material becomes when penetrating state, need to change dehydrating material, thus, the replacing labour of dehydrating material and operating cost increase.Therefore, although said method is effective means for laboratory rank, the separation carrying out moisture from a large amount of organic solvent reclaimed from factory, research facilities etc. can not be met.
Therefore, a kind of dehydration of organic solvent device is proposed in following patent document 2, it has following operation: dehydration procedure, by organic solvent being passed to the dehydrating material be filled in drench pit (adsorption tower), makes water adsorption contained in organic solvent in this dehydrating material; Drying process, by non-active gas or air circulation to dehydrating material, will be adsorbed in the moisture drying of dehydrating material, cationic ion-exchange resin is used for dehydrating material by this dehydration of organic solvent device.
Prior art document
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2000-225316 publication
Patent document 2: Japanese Unexamined Patent Publication 2009-291676 publication
Summary of the invention
the problem that invention will solve
But when ion exchange resin etc. is used for dehydrating material, during the dehydrating material after dehydration procedure dry, if improve rate of drying, then due to the difference of the water content of the ectonexine of dehydrating material, dehydrating material is destroyed.Its result, likely causes the filter being arranged at drench pit to block because of the fragment of dehydrating material, thus reduces the water separation capability of dehydration of organic solvent device.
The present invention makes for background with the problem of prior art, and therefore its problem is, provides the dehydration of organic solvent device of the formation possessing the water separation capability that can not reduce dehydration of organic solvent device.
for the scheme of dealing with problems
Based in dehydration of organic solvent device of the present invention, by the processed organic solvent containing moisture being imported to dehydrating material and making above-mentioned processed organic solvent contact with above-mentioned dehydrating material, moisture contained in above-mentioned processed organic solvent is removed in dehydration, wherein, above-mentioned dehydrating material comprises the cationic ion-exchange resin with spherical shape, in above-mentioned dehydrating material, the particle diameter of above-mentioned cationic ion-exchange resin is the particle rate of below 0.4mm is more than 90%.
In other embodiments, the basal body structure of above-mentioned cationic ion-exchange resin is be selected from least one in the group that is made up of acrylic polymer, methacrylic polymer and styrene diethylene benzene copoly mer, and imparts carboxylic acid Ca group or sulfonic acid Na group to above-mentioned basal body structure.
In other embodiments, above-mentioned dehydration of organic solvent device comprises: for fill above-mentioned dehydrating material drench pit, for above-mentioned processed organic solvent is imported to above-mentioned drench pit processed organic solvent lead-in path, be used for non-active gas to import to above-mentioned drench pit non-active gas lead-in path, be used for desiccant air to import to above-mentioned drench pit dry air import path.
In other embodiments, above-mentioned dehydration of organic solvent device also comprises: for rinse water being imported to the rinse water lead-in path of above-mentioned drench pit, being used for discharging from above-mentioned drench pit the rinse water discharge path of above-mentioned rinse water.
In other embodiments, above-mentioned rinse water lead-in path has the rinse water circulating path above-mentioned rinse water being discharged to above-mentioned rinse water discharge path being imported to above-mentioned rinse water lead-in path.
In other embodiments, above-mentioned drench pit comprises the first drench pit and the second drench pit, when desiccant air being imported to above-mentioned first drench pit from above-mentioned dry air importing path, from above-mentioned processed organic solvent lead-in path, above-mentioned processed organic solvent is imported to above-mentioned second drench pit, when desiccant air being imported to above-mentioned second drench pit from above-mentioned dry air importing path, from above-mentioned processed organic solvent lead-in path, above-mentioned processed organic solvent is imported to above-mentioned first drench pit, thus continuously above-mentioned processed organic solvent is imported to dehydrating material and above-mentioned processed organic solvent is contacted with above-mentioned dehydrating material, can dewater thus and remove moisture contained in above-mentioned processed organic solvent.
the effect of invention
According to based on dehydration of organic solvent device of the present invention, the dehydration of organic solvent device possessing the formation that can not reduce water separation capability can be provided.
Accompanying drawing explanation
The figure of Fig. 1 to be the drench pit illustrated in embodiment be dehydration of organic solvent device of the mode of 1 tower.
The figure of Fig. 2 to be the drench pit illustrated in other embodiment be dehydration of organic solvent device of the mode of 2 towers.
Fig. 3 is the figure of the organic solvent recycling and processing device of the use activated carbon fiber illustrated in other embodiment.
Fig. 4 is the figure of each condition that the dehydrating material used in embodiment 1 ~ embodiment 3 and comparative example 1 ~ comparative example 3 is shown.
description of reference numerals
1 drench pit, 2 processed organic solvent tanks, 3 processed organic solvents import circuit, 4,13,22,24,27,52 flashboards, 6 refining organic solvent pumping-out lines, 7 refining organic solvent tanks, 11 water pots, 12 water pumps, 21 compressors, 23 dry airs import circuit, 26 dry air pumping-out lines, 28 return lines, 41 processed gases, 42 air blasts, 43 adsorption towers, 44 NACF elements, 45 steam, 46 clean airs, 47 condensers, 48 separators, 49 recycling design, 51 rinse water circulating paths.
Detailed description of the invention
Below, with reference to accompanying drawing, embodiments of the present invention are described in detail.It should be noted that, in embodiment shown below, mark identical Reference numeral in the drawings to identical or corresponding part, its explanation no longer repeats sometimes.In addition, in the embodiment of following explanation, when mentioning number, amount etc., except having special situation about recording, scope of the present invention is not necessarily defined in this number, amount etc.
Following dehydration of organic solvent device is preferably based on dehydration of organic solvent device of the present invention, namely this dehydration of organic solvent device possesses: dehydration procedure equipment, organic solvent containing moisture is passed to the dehydrating material be filled in drench pit, makes water adsorption in this dehydrating material; Drying process equipment, is passed to dehydrating material by dry air, will be adsorbed in the moisture drying of dehydrating material, the above-mentioned operation and this dehydration of organic solvent device hockets.This is because, by adopting above-mentioned structure, can process continuously.
As the structure of preferred device, be following dehydration of organic solvent device: dehydrating material is divided into some parts, their dehydration procedure and drying process utilize flashboard etc. to carry out handover operation, carry out continuously dewatering and drying; Or there is the dehydration of organic solvent device of following structure: dehydrating material can rotate, and the position of having adsorbed moisture in dehydration procedure of dehydrating material is moved to drying process by the rotation of dehydrating material.
Below, with reference to accompanying drawing, dehydration of organic solvent device of the present invention is described in detail.Fig. 1 is an example preferred embodiment of the present invention.The dehydration of organic solvent device exemplified in Fig. 1 has absorption process, in described absorption process, when flashboard 4,5 is opened, the organic solvent had containing moisture is imported circuit 3 from the processed organic solvent tank 2 containing the organic solvent of moisture stored with this by processed organic solvent and is transported to the drench pit 1 being filled with dehydrating material, the organic solvent refined is transported to refining organic solvent tank 7 by refining organic solvent pumping-out line 6, thus utilize dehydrating material Adsorption moisture, refining organic solvent.
On the other hand, preferably there is water matting, in described water matting, when flashboard 4,5 cuts out and flashboard 24,25 is opened, when flashboard 13 is opened, use water pump 12 to import circuit 23 from water pot 11 by water or dry air and water is transported to drench pit 1, thus the organic solvent utilizing the circulation of water attachment to be residued in dehydrating material surface is removed.This is because, the non-active gas as nitrogen such as also can be used to carry out aftermentioned drying process, and do not carry out water matting, but, by removing organic solvent, the non-active gas just no longer needing use cost high during drying process with water cleaning.
In water matting, the rinse water of discharging from water or dry air pumping-out line 26 comprises organic solvent, can collect and burn etc., but preferably, opening flashboard 27, turning back to processed organic solvent tank 2 from return line 28.This is because according to said method, can save process number, be efficient.
In addition, preferably, in the subsequent handling of water matting, there is drying process, in described drying process, close flashboard 13 and open flashboard 22, import circuit 23 by water or dry air and dry air is transported to drench pit 1, thus utilize the circulation of dry air to be adsorbed in the moisture drying of dehydrating material.The gas produced by drying process contains the organic solvent of trace, can utilize the burners such as direct burner, catalytic combustion system, heat accumulating burner capable, use the normally used gas treatment equipments such as the solvent recovery unit of activated carbon fiber to process the gas of discharging from water or dry air pumping-out line 26.
Preferably, in drying process, when the temperature of dry air is 5 ~ 30 DEG C, the dew point of dry air is negative.This is because the air of the drying that dew point is lower more can shorten by the drying time of the dry moisture of dehydrating material.In order to reduce dew point, preferably use compressor 21.In addition, it is further preferred that by arranging in the downstream of compressor 21 dew point that air dryer etc. reduces drying air further.Or, it is further preferred that drying air is heated to 40 ~ 80 DEG C by arranging heater etc. in the downstream of compressor 21.And then, further preferably, by combinations such as air dryer etc. and heaters, use dew point low add hot-air as dry gas.
Becoming can by repeating above-mentioned dehydration procedure → water matting → drying process and from the organic solvent containing moisture by moisture efficiently and the device of removal of dewatering economically continuously.By above-mentioned continuous print dehydration-air oxygen detrition, stably the moisture in organic solvent can be removed with ability with low cost.
Preferably, the dehydrating material in present embodiment comprises the cationic ion-exchange resin with spherical shape, and in dehydrating material, the particle diameter of cationic ion-exchange resin is the particle rate of below 0.4mm is more than 90%.Saidly herein spherically to refer to, not only mean geometric proper sphere shape, and spheroid also can, but more preferably close to the shape of proper sphere shape.During for spheroid, diameter (major axis footpath) the longest in three preferably orthogonal diameters and the ratio of the shortest diameter (short shaft diameter) are the spheroid of less than 2, and preferably the ratio of major axis footpath and short shaft diameter is the spheroid of less than 1.3 further.It should be noted that, particle rate refers to, by the ratio that there is quantity of the particle of specified particle diameter contained in this cationic ion-exchange resin of forming when whole cationic ion-exchange resin (being filled in the cationic ion-exchange resin in drench pit 1) of dehydrating material is set to 100%.
Preferably, the basal body structure of cationic ion-exchange resin is be selected from least one in the group that is made up of acrylic polymer, methacrylic polymer and styrene diethylene benzene copoly mer, and imparts carboxylic acid Ca group or sulfonic acid Na group to this basal body structure.
The running of the dehydrating material in present embodiment preferably adopts the system that can remove continuously being provided with two or more drench pit as shown in Figure 2, considers the amount etc. of the amount containing moisture wishing to remove, processed organic solvent, also can be set to intermittent running.This is because, under the condition that the amount of the amount containing moisture or processed organic solvent is few, be unlikely to need continuous running, can operating cost be reduced.
In present embodiment, the organic solvent that can dewater is not particularly limited in ethyl acetate, methyl acetate, toluene, dimethylbenzene, MEK, methyl iso-butyl ketone (MIBK), carrene (methylene dichloride), chloroform, carrene (dichloromethane) etc., can be adapted to multiple organic solvent.
In present embodiment, the organic solvent that can dewater can also be adapted to the organic solvent using solvent recovery treating apparatus to reclaim the gas of the organic solvent of discharging containing the factory etc. from the dry lamination operation of laminate film etc., multiple fields.
Such as, organic solvent recycling and processing device as shown in figure 3 is following system, namely, this system has: absorption process, air blast 42 is utilized to import processed gas 41, utilize NACF element 44 absorbing organic solvent be filled in adsorption tower 43, be discharged to outside air as clean air 46; Desorption operation, by steam 45 is imported to NACF element 44, makes organic solvent desorption, with condenser 47 condensation knot, be separated into solvent and water with separator 48, recycling design 49 is reclaimed, this system, by absorption process and the desorption operation of hocketing, can process continuously.
Moisture, owing to using steam in desorption, carry out condensation knot and causing being mixed in recycling design moisture, thus, by the dehydration of organic solvent device in application present embodiment, can be removed from recycling design by the solvent recovery treating apparatus of the type efficiently.
In addition, in the dehydration of organic solvent device shown in Fig. 1 and Fig. 2, import circuit 23 to the rinse water being discharged to rinse water discharge path and water or dry air pumping-out line 26 be imported to rinse water lead-in path and water or dry air, the rinse water circulating path 51 from dry air pumping-out line 26 to water pot 11 branch also can be set.The opening and closing of the circuit of rinse water circulating path 51 is controlled by flashboard 52.
Embodiment
Below, utilize each embodiment 1 ~ 3 and comparative example 1 ~ 3 to further illustrate details based on the dehydration of organic solvent device in embodiments of the present invention, but the present invention is not limited to these embodiments.It should be noted that, each condition of the dehydrating material used in the 1 ~ embodiment of embodiment shown in Fig. 43 and comparative example 1 ~ comparative example 3.
(embodiment 1)
In the dehydration of organic solvent device shown in Fig. 1, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that dehydrating material use is basal body structure with the styrene diethylene benzene copoly mer that frame strength is 8%, particle size range is 0.2mm ~ 0.5mm, and the particle rate that particle diameter is below 0.4mm is 90%.It should be noted that, the mensuration of spherical cationic ion-exchange resin is carried out according to regulation " granularmetric analysis laser diffractometry ", use sedimentograph (HORIBA LA-950V2) in Japanese Industrial Standards (JIS Z8825-1).
This cationic ion-exchange resin of 19kg is filled into drench pit 1, as solvent dehydration operation, is 3 quality % by moisture, mixed liquor that ethyl acetate is 97 quality % imports circuit 3 with 200L/hr from processed organic solvent and import to drench pit 1.Now, adsorption temp is 30 DEG C.
Then, as water matting, the running water of 20L/min is imported circuit 23 by water or dry air and imports to drench pit 1, the solvent being attached to dehydrating material is cleaned.Then, as drying process, the mode being no more than 90kPa with the maximum crushing of drench pit 1 regulates air quantity, and the dry heat air of 100 DEG C, 0 DEG C DP (Dew Point (dew point)) is imported to drench pit 1.
This solvent dehydration operation → water matting → drying process needs 4.5hr, after this operation being repeated 20 circulations, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet be reduced to 0.9 quality %, dry air quantity during drying process is now 180m
3/ hr.
And then, after this operation being repeated 200 circulations, with above-mentioned 20 circulation times identical, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet be reduced to 0.9 quality %, dry air quantity during drying process is now 180m
3/ hr.In the present embodiment 1, even if repeat solvent dehydration operation → water matting → drying process, for utilizing the mixed solvent of dehydration of organic solvent device processed, also the outlet average moisture concentration in the mixed solvent by processed 0.9 quality % can be maintained, stably can carry out processed with high efficiency, and performance can not reduce.
Can think this result be because, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that dehydrating material is is basal body structure with the frame strength styrene diethylene benzene copoly mer that is 8%, particle size range is 0.2 ~ 0.5mm, and the particle rate that particle diameter is below 0.4mm is 90%, therefore, even if in drying process, cationic ion-exchange resin is not also almost destroyed, the filter being arranged at drench pit can not be caused to block because of the fragment of dehydrating material, the water separation capability of dehydration of organic solvent device is maintained.
(embodiment 2)
In the dehydration of organic solvent device shown in Fig. 1, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that it is basal body structure that dehydrating material uses with the frame strength styrene diethylene benzene copoly mer that is 8% in a large number, particle size range is 0.1mm ~ 1.0mm, and the particle rate that particle diameter is below 0.4mm is 90%.It should be noted that, the mensuration of spherical cationic ion-exchange resin is carried out according to regulation " granularmetric analysis laser diffractometry ", use sedimentograph (HORIBA LA-950V2) in Japanese Industrial Standards (JIS Z8825-1).
This cationic ion-exchange resin of 19kg is filled into drench pit 1, as solvent dehydration operation, be 3 quality % by moisture, ethyl acetate is 80 quality %, mixed liquor that n-propyl acetate is 17 quality % imports circuit 3 with 200L/hr from processed organic solvent and import to drench pit 1.Now, adsorption temp is 30 DEG C.
Then, as water matting, the running water of 20L/min is imported circuit 23 by water or dry air and imports to drench pit 1, the solvent being attached to dehydrating material is cleaned.Then, as drying process, the mode being no more than 90kPa with the maximum crushing of drench pit 1 regulates air quantity, and the dry heat air of 100 DEG C, 0 DEG C DP (Dew Point (dew point)) is imported to drench pit 1.
This solvent dehydration operation → water matting → drying process needs 4.5hr, after this operation being repeated 20 circulations, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet be reduced to 0.95 quality %, dry air quantity during drying process is now 160m
3/ hr.
And then, after this operation being repeated 200 circulations, with above-mentioned 20 circulation times identical, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet be reduced to 0.95 quality %, dry air quantity during drying process is now 160m
3/ hr.In the present embodiment 2, even if repeat solvent dehydration operation → water matting → drying process, for utilizing the mixed solvent of dehydration of organic solvent device processed, also the outlet average moisture concentration in the mixed solvent by processed 0.95 quality % can be maintained, stably can carry out processed with high efficiency, and performance can not reduce.
Can think this result be because, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that dehydrating material is is basal body structure with the frame strength styrene diethylene benzene copoly mer that is 8%, particle size range is 0.1 ~ 1.0mm, and the particle rate that particle diameter is below 0.4mm is 90%, therefore, even if in drying process, cationic ion-exchange resin is almost not destroyed yet, the filter being arranged at drench pit can not be caused to block because of the fragment of dehydrating material, the water separation capability of dehydration of organic solvent device is maintained.
(embodiment 3)
In the dehydration of organic solvent device shown in Fig. 1, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that it is basal body structure that dehydrating material uses with the frame strength styrene diethylene benzene copoly mer that is 8% in a large number, particle size range is 0.38mm ~ 0.4mm, and the particle rate that particle diameter is below 0.4mm is 100%.It should be noted that, the mensuration of spherical cationic ion-exchange resin is carried out according to regulation " granularmetric analysis laser diffractometry ", use sedimentograph (HORIBA LA-950V2) in Japanese Industrial Standards (JIS Z8825-1).
This cationic ion-exchange resin of 19kg is filled into drench pit 1, as solvent dehydration operation, be 2 quality % by moisture, carrene is 88 quality %, mixed liquor that methyl alcohol is 10 quality % imports circuit 3 with 200L/hr from processed organic solvent and import to drench pit 1.Now, adsorption temp is 30 DEG C.
Then, as water matting, the running water of 20L/min is imported circuit 23 by water or dry air and imports to drench pit 1, the solvent being attached to dehydrating material is cleaned.Then, as drying process, the mode being no more than 90kPa with the maximum crushing of drench pit 1 regulates air quantity, and the dry heat air of 100 DEG C, 0 DEG C DP (Dew Point (dew point)) is imported to drench pit 1.
This solvent dehydration operation → water matting → drying process needs 4.5hr, after this operation being repeated 20 circulations, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet be reduced to 0.5 quality %, dry air quantity during drying process is now 220m
3/ hr.
And then, after this operation being repeated 200 circulations, with above-mentioned 20 circulation times identical, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet be reduced to 0.5 quality %, dry air quantity during drying process is now 220m
3/ hr.In the present embodiment 3, even if repeat solvent dehydration operation → water matting → drying process, for utilizing the mixed solvent of dehydration of organic solvent device processed, also the outlet average moisture concentration in the mixed solvent by processed 0.5 quality % can be maintained, stably can carry out processed with high efficiency, and performance can not reduce.
Can think this result be because, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that dehydrating material is is basal body structure with the frame strength styrene diethylene benzene copoly mer that is 8%, particle size range is 0.38 ~ 0.4mm, and the particle rate that particle diameter is below 0.4mm is 100%, therefore, even if in drying process, cationic ion-exchange resin is almost not destroyed yet, the filter being arranged at drench pit can not be caused to block because of the fragment of dehydrating material, the water separation capability of dehydration of organic solvent device is maintained.
(comparative example 1)
In the dehydration of organic solvent device shown in Fig. 1, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that it is basal body structure that dehydrating material uses with the frame strength styrene diethylene benzene copoly mer that is 8% in a large number, particle size range is 0.6mm ~ 0.7mm, and the particle rate that particle diameter is below 0.4mm is 0%.It should be noted that, the mensuration of spherical cationic ion-exchange resin is carried out according to regulation " granularmetric analysis laser diffractometry ", use sedimentograph (HORIBA LA-950V2) in Japanese Industrial Standards (JIS Z8825-1).
This cationic ion-exchange resin of 19kg is filled into drench pit 1, as solvent dehydration operation, is 3 quality % by moisture, mixed liquor that ethyl acetate is 97 quality % imports circuit 3 with 200L/hr from processed organic solvent and import to drench pit 1.Now, adsorption temp is 30 DEG C.
Then, as water matting, the running water of 20L/min is imported circuit 23 by water or dry air and imports to drench pit 1, the solvent being attached to dehydrating material is cleaned.Then, as drying process, the mode being no more than 90kPa with the maximum crushing of drench pit 1 regulates air quantity, and the dry heat air of 100 DEG C, 0 DEG C DP (Dew Point (dew point)) is imported to drench pit 1.
This solvent dehydration operation → water matting → drying process needs 4.5hr, after this operation being repeated 20 circulations, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet be reduced to 0.9 quality %, dry air quantity during drying process is now 180m
3/ hr.
And then, after this operation being repeated 200 circulations, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet rise to 1.8 quality %, dry air quantity during drying process is now 100m
3/ hr.In this comparative example 1, when being repeated solvent dehydration operation → water matting → drying process, for utilize the mixed solvent of dehydration of organic solvent device processed, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet rise.
Can think this is because, about dehydrating material, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that it is basal body structure that dehydrating material uses with the frame strength styrene diethylene benzene copoly mer that is 8% in a large number, particle size range is 0.6mm ~ 0.7mm, and the particle rate that particle diameter is below 0.4mm is 0%, therefore, the granule number of cationic ion-exchange resin destroyed in drying process exists in a large number, therefore, cause the filter being arranged at drench pit to block because of the fragment of dehydrating material, the water separation capability of result dehydration of organic solvent device reduces.
(comparative example 2)
In the dehydration of organic solvent device shown in Fig. 1, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that it is basal body structure that dehydrating material uses with the frame strength styrene diethylene benzene copoly mer that is 8% in a large number, particle size range is 0.35mm ~ 0.5mm, and the particle rate that particle diameter is below 0.4mm is 80%.It should be noted that, the mensuration of spherical cationic ion-exchange resin is carried out according to regulation " granularmetric analysis laser diffractometry ", use sedimentograph (HORIBA LA-950V2) in Japanese Industrial Standards (JIS Z8825-1).
This cationic ion-exchange resin of 19kg is filled into drench pit 1, as solvent dehydration operation, be 3 quality % by moisture, ethyl acetate is 80 quality %, mixed liquor that n-propyl acetate is 17 quality % imports circuit 3 with 200L/hr from processed organic solvent and import to drench pit 1.Now, adsorption temp is 30 DEG C.
Then, as water matting, the running water of 20L/min is imported circuit 23 by water or dry air and imports to drench pit 1, the solvent being attached to dehydrating material is cleaned.Then, as drying process, the mode being no more than 90kPa with the maximum crushing of drench pit 1 regulates air quantity, and the dry heat air of 100 DEG C, 0 DEG C DP (Dew Point (dew point)) is imported to drench pit 1.
This solvent dehydration operation → water matting → drying process needs 4.5hr, after this operation being repeated 20 circulations, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet be reduced to 0.85 quality %, dry air quantity during drying process is now 200m
3/ hr.
And then, after this operation being repeated 200 circulations, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet rise to 1.3 quality %, dry air quantity during drying process is now 150m
3/ hr.In this comparative example 2, when being repeated solvent dehydration operation → water matting → drying process, for utilize the mixed solvent of dehydration of organic solvent device processed, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet rise.
Can think this is because, about dehydrating material, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that it is basal body structure that dehydrating material uses with the frame strength styrene diethylene benzene copoly mer that is 8% in a large number, particle size range is 0.35mm ~ 0.5mm, and the particle rate that particle diameter is below 0.4mm is 80%, the granule number of cationic ion-exchange resin destroyed in drying process exists in a large number, therefore, cause the filter being arranged at drench pit to block because of the fragment of dehydrating material, the water separation capability of result dehydration of organic solvent device reduces.
(comparative example 3)
In the dehydration of organic solvent device shown in Fig. 1, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that it is basal body structure that dehydrating material uses with the frame strength styrene diethylene benzene copoly mer that is 8% in a large number, particle size range is 0.1mm ~ 1.0mm, and the particle rate that particle diameter is below 0.4mm is 80%.It should be noted that, the mensuration of spherical cationic ion-exchange resin is carried out according to regulation " granularmetric analysis laser diffractometry ", use sedimentograph (HORIBALA-950V2) in Japanese Industrial Standards (JISZ8825-1).
This cationic ion-exchange resin of 19kg is filled into drench pit 1, as solvent dehydration operation, be 2 quality % by moisture, carrene is 88 quality %, mixed liquor that methyl alcohol is 10 quality % imports circuit 3 with 200L/hr from processed organic solvent and import to drench pit 1.Now, adsorption temp is 30 DEG C.
Then, as water matting, the running water of 20L/min is imported circuit 23 by water or dry air and imports to drench pit 1, the solvent being attached to dehydrating material is cleaned.Then, as drying process, the mode being no more than 90kPa with the maximum crushing of drench pit 1 regulates air quantity, and the dry heat air of 100 DEG C, 0 DEG C DP (Dew Point (dew point)) is imported to drench pit 1.
This solvent dehydration operation → water matting → drying process needs 4.5hr, after this operation being repeated 20 circulations, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet be reduced to 0.5 quality %, dry air quantity during drying process is now 220m
3/ hr.
And then, after this operation being repeated 200 circulations, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet rise to 0.9 quality %, dry air quantity during drying process is now 170m
3/ hr.In this comparative example 3, when being repeated solvent dehydration operation → water matting → drying process, for utilize the mixed solvent of dehydration of organic solvent device processed, in solvent dehydration operation processed mixed solvent in the average moisture concentration of outlet rise.
Can think this is because, about dehydrating material, the spherical cationic ion-exchange resin being modified with sulfonic acid Na group that it is basal body structure that dehydrating material uses with the frame strength styrene diethylene benzene copoly mer that is 8% in a large number, particle size range is 0.1mm ~ 1.0mm, and the particle rate that particle diameter is below 0.4mm is 80%, therefore, the granule number of cationic ion-exchange resin destroyed in drying process exists in a large number, therefore, cause the filter being arranged at drench pit to block because of the fragment of dehydrating material, the water separation capability of result dehydration of organic solvent device reduces.
The above-described embodiment and examples disclosed by the invention are illustration in all respects, but not determinate.Protection scope of the present invention delimited by claims, and in addition, it comprises and all changes in the meaning of the record equalization of claims and scope.
utilizability in industry
Dehydration of organic solvent device of the present invention can realize the continuous treating of solvent, does not substantially need to change dehydrating material, can efficiently and stably remove large quantity of moisture, therefore, it is possible to omit dehydrating material replacement operation, reduce costs, steady removal moisture, and do not need expansion equipment.Therefore, especially may be used for the dehydration of the solvent using solvent recovery treating apparatus from the exhaust gas recovery by the field generation widely such as research institute, factory, large contribution is made to industrial circle.
Claims (6)
1. a dehydration of organic solvent device, it possesses: dehydration procedure equipment, and the processed organic solvent containing moisture is passed to the dehydrating material be filled in drench pit, makes water adsorption in this dehydrating material; Drying process equipment, is passed to dehydrating material by dry air or non-active gas, will be adsorbed in the moisture drying of dehydrating material, the above-mentioned operation and described dehydration of organic solvent device hockets, wherein,
Described dehydrating material comprises the cationic ion-exchange resin with spherical shape,
In described dehydrating material, the particle diameter of described cationic ion-exchange resin is the particle rate of below 0.4mm is more than 90%.
2. dehydration of organic solvent device according to claim 1, wherein, the basal body structure of described cationic ion-exchange resin is be selected from least one in the group that is made up of acrylic polymer, methacrylic polymer and styrene diethylene benzene copoly mer, and imparts carboxylic acid Ca group or sulfonic acid Na group to described basal body structure.
3. dehydration of organic solvent device according to claim 1 and 2, wherein,
This dehydration of organic solvent device comprises:
For fill described dehydrating material drench pit,
For described processed organic solvent is imported to described drench pit processed organic solvent lead-in path,
For non-active gas is imported to described drench pit non-active gas lead-in path,
Dry air for desiccant air being imported to described drench pit imports path.
4. dehydration of organic solvent device according to claim 3, wherein,
This dehydration of organic solvent device also comprises:
For rinse water is imported to described drench pit rinse water lead-in path,
For discharging the rinse water discharge path of described rinse water from described drench pit.
5. dehydration of organic solvent device according to claim 4, wherein,
Described rinse water lead-in path has the rinse water circulating path for the described rinse water being discharged to described rinse water discharge path being imported to described rinse water lead-in path.
6. dehydration of organic solvent device according to claim 3, wherein,
Described drench pit comprises the first drench pit and the second drench pit,
When desiccant air being imported to described first drench pit from described dry air importing path, from described processed organic solvent lead-in path, described processed organic solvent is imported to described second drench pit,
When desiccant air being imported to described second drench pit from described dry air importing path, from described processed organic solvent lead-in path, described processed organic solvent is imported to described first drench pit, thus continuously described processed organic solvent is imported to dehydrating material and described processed organic solvent is contacted with described dehydrating material, can dewater thus and remove moisture contained in described processed organic solvent.
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| JP2011034626 | 2011-02-21 | ||
| PCT/JP2012/054058 WO2012115081A1 (en) | 2011-02-21 | 2012-02-21 | Organic solvent dehydrating device |
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| CN110255659A (en) * | 2019-07-23 | 2019-09-20 | 山东先声生物制药有限公司 | A kind of device and method thereof of concentration medicine waste liquid |
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| JPS61171507A (en) * | 1985-01-24 | 1986-08-02 | Mitsubishi Chem Ind Ltd | Purification of organic solvent |
| JPS61178929A (en) * | 1985-02-04 | 1986-08-11 | Hitachi Ltd | Totally automatic dehydroator for organic solvent of chlorinated hydrocarbon |
| US4889537A (en) * | 1985-05-10 | 1989-12-26 | Elf France Societe Anonyme | Method for treating a fuel comprising a mixture of hydrocarbons and alcohols, and a selective water-adsorption product |
| JP2000225316A (en) * | 1999-02-05 | 2000-08-15 | Ricoh Co Ltd | Solvent gas recovery method and recovery apparatus |
| JP2009291676A (en) * | 2008-06-03 | 2009-12-17 | Toyobo Co Ltd | Solvent refining apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0440367A (en) * | 1990-06-05 | 1992-02-10 | Mitsui Toatsu Chem Inc | Spherical separating agent |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61171507A (en) * | 1985-01-24 | 1986-08-02 | Mitsubishi Chem Ind Ltd | Purification of organic solvent |
| JPS61178929A (en) * | 1985-02-04 | 1986-08-11 | Hitachi Ltd | Totally automatic dehydroator for organic solvent of chlorinated hydrocarbon |
| US4889537A (en) * | 1985-05-10 | 1989-12-26 | Elf France Societe Anonyme | Method for treating a fuel comprising a mixture of hydrocarbons and alcohols, and a selective water-adsorption product |
| JP2000225316A (en) * | 1999-02-05 | 2000-08-15 | Ricoh Co Ltd | Solvent gas recovery method and recovery apparatus |
| JP2009291676A (en) * | 2008-06-03 | 2009-12-17 | Toyobo Co Ltd | Solvent refining apparatus |
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| KR101762474B1 (en) | 2017-07-27 |
| CN103402596A (en) | 2013-11-20 |
| JP5527447B2 (en) | 2014-06-18 |
| KR20140006895A (en) | 2014-01-16 |
| JP5207014B2 (en) | 2013-06-12 |
| JP2013126664A (en) | 2013-06-27 |
| WO2012115081A1 (en) | 2012-08-30 |
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