CN106237651B - A kind of method and its device of liquid-solid system Dynamic Adsorption - Google Patents
A kind of method and its device of liquid-solid system Dynamic Adsorption Download PDFInfo
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- CN106237651B CN106237651B CN201610776425.0A CN201610776425A CN106237651B CN 106237651 B CN106237651 B CN 106237651B CN 201610776425 A CN201610776425 A CN 201610776425A CN 106237651 B CN106237651 B CN 106237651B
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000007787 solid Substances 0.000 title claims abstract description 27
- 239000003463 adsorbent Substances 0.000 claims abstract description 129
- 239000007790 solid phase Substances 0.000 claims abstract description 58
- 239000000725 suspension Substances 0.000 claims abstract description 38
- 238000010521 absorption reaction Methods 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims description 75
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 21
- 239000011347 resin Substances 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 239000012452 mother liquor Substances 0.000 claims description 9
- 239000002351 wastewater Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 235000013399 edible fruits Nutrition 0.000 claims description 5
- 229930182817 methionine Natural products 0.000 claims description 5
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 claims description 4
- AYFVYJQAPQTCCC-UHFFFAOYSA-N Threonine Natural products CC(O)C(N)C(O)=O AYFVYJQAPQTCCC-UHFFFAOYSA-N 0.000 claims description 4
- 239000004473 Threonine Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000000975 dye Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 3
- 244000060011 Cocos nucifera Species 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- 239000002250 absorbent Substances 0.000 claims 1
- 230000002745 absorbent Effects 0.000 claims 1
- 239000003610 charcoal Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000004042 decolorization Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- -1 charging Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 27
- 239000000047 product Substances 0.000 description 26
- 238000012360 testing method Methods 0.000 description 15
- 238000002835 absorbance Methods 0.000 description 13
- 238000012545 processing Methods 0.000 description 13
- 239000012535 impurity Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 9
- 238000001914 filtration Methods 0.000 description 6
- 238000012805 post-processing Methods 0.000 description 6
- 230000003068 static effect Effects 0.000 description 6
- 238000010924 continuous production Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 125000001360 methionine group Chemical group N[C@@H](CCSC)C(=O)* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
-
- 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
- B01D15/02—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor with moving adsorbents
Abstract
The present invention provides a kind of method of liquid-solid system Dynamic Adsorption, including prepares the suspension containing adsorbent, charging, solid phase Dynamic Adsorption in tower；The present invention also provides a kind of device of liquid-solid system Dynamic Adsorption, described device includes solid phase Dynamic Adsorption tower；Paddle and disk be set in the solid phase Dynamic Adsorption tower, 0.4 ~ 0.6 times of a diameter of solid phase Dynamic Adsorption tower internal diameter of paddle, paddle is set among adjacent discs, paddle be straight leaf, and the ratio of adjacent discs spacing and tower internal diameter is 0.3 2:1.The present invention uses Dynamic Adsorption so that adsorbent comes into full contact with solution, and there is no the phenomenon that adsorption layer saturation is carried out with absorption, it is ensured that product quality is stablized；For the decoloration of solution, the percent of decolourization of every 10 90 minutes detection primary productions, the percent of decolourization of 1000 times, percentage point deviation range is only ± 0.007 ~ ± 0.01；Pressure drop is small, and energy consumption is low, and adsorbent utilization rate is high.
Description
Technical field
The present invention provides a kind of method and its device of liquid-solid system Dynamic Adsorption, belongs to chemical separating field.
Background technology
The refined and decoloration that the adsorption technology of liquid-solid system is at home and abroad used for the industry such as medicine, chemical industry and food has had
Many year history.All play a very important role in terms of chemical, metallurgy, environmental protection and biotechnology.
Application preferably at most Static Adsorption, including traditional ADSORPTION IN A FIXED BED at present, moving bed absorption etc., is to pass through absorption
Bed is adsorbed；Feed liquid flows through absorptive media layers by the liquid distribution trough on column top, flows out and receives from the lower part of pillar
Collection, fluid are adsorbed step by step in the dielectric layer, obtain required product.
The prior art has the following disadvantages：
During Static Adsorption, with the progress of adsorption process, effective adsorbent layer is shorter and shorter, the adsorbent of saturation
More and more, the impurity content of product increases therewith after absorption, causes unstable product quality；For single pillar, absorption
Medium is actionless, and feed liquid treating capacity is bigger, and the amount of adsorbing medium saturation is with regard to more and more, then the product obtained every time
Quality is also unstable；
Static Adsorption loses adsorption capacity when adsorbent saturation, it is necessary to which parking displacement, belongs to intermittently operated, so processing
Amount is few, is not easy to realization and automatically controls.If carry out continuous production, it is necessary to configure multiple devices, carry out spare replacement, equipment
It is of high cost.
Adsorbent needs to carry out the processing such as being desorbed after reaching saturation under static conditions at the same time, if being used for continuous production,
Need to configure more with the spare replacement of pillar progress；
Sometimes for adsorption time is shortened, the method for increase adsorbing medium layer height can be used, but resistance drop can be increased,
Energy consumption increases therewith.
The product of prior art processing, loss of effective components are more.
The content of the invention
To solve the shortcomings of the prior art, the present invention provides a kind of method and its dress of liquid-solid system Dynamic Adsorption
Put, to realize following goal of the invention：
（1）After present invention processing, obtained product quality is stablized；
（2）The present invention can make full use of adsorbent, suitable for continuous production；
（3）The method of the present invention and device, equipment cost is low, and energy consumption is low；
（4）The utilization rate of adsorbent of the present invention is high；
（5）Product after present invention processing, impurity content is low, loss of effective components is few；
In order to solve the above technical problems, the technical solution that the present invention takes is as follows：
A kind of method of liquid-solid system Dynamic Adsorption, it is characterised in that：Including prepare the suspension containing adsorbent, charging,
Solid phase Dynamic Adsorption in tower.
It is that the further of above-mentioned technical proposal is improved below：
Adsorption scheme of the present invention, the technological process being related to are as follows：
The liquid that adsorbent and adsorbent are used cooperatively, into material-compound tank, mixes after metering by stirring evenly
To the suspension containing adsorbent, the suspension containing adsorbent is from the lower endfeed of solid phase Dynamic Adsorption tower A, and feed inlet is positioned at last
The lower end of one disk.Pending feed liquid enters from the bottom of solid phase Dynamic Adsorption tower A.Tower top discharges, into filter E, mistake
Filter obtains the adsorbent and product solution after use.
The suspension of the preparation containing adsorbent, the liquid that adsorbent and adsorbent are used cooperatively is according to 1:The matter of 2-10
Amount ratio mixes, and obtains the suspension containing adsorbent, adsorbent is as decentralized medium, and mixing is in a liquid so that adsorbent one
Directly it is in flow regime.
The adsorbent is activated carbon or absorption resin；The liquid that the adsorbent is used cooperatively is water or material to be processed
Liquid is, it is necessary to ensure that adsorbent cannot dissolve in a liquid.
The activated carbon is one in 20 ~ 40 mesh active fruit shell carbons, powder active fruit shell carbon, 50 ~ 80 mesh cocoanut active charcoals
Kind；The absorption resin adsorbs resin for D315 types, DA201 types adsorb resin, one kind in 213 types absorption resin；It is described to treat
Processing feed liquid is methionine mother liquor, one kind in threonine mother liquor, sucrose solution, waste water from dyestuff, wastewater containing methanol.
Be uniformly mixed at the same time in order to ensure to enter after solid phase Dynamic Adsorption tower with feed liquid, adsorbent will not sink blocking
Feed inlet, it is desirable to which the density of the adsorbent is less than the density for the liquid that adsorbent is used cooperatively；The adsorbent and adsorbent
The mass ratio for the liquid being used cooperatively is less than or equal to 50%.
The charging, adsorbent are 1 with the mass ratio of pending feed liquid:1000 ~ 10000, pending feed liquid and containing suction
Flow velocity is 0.1cm/s-2cm/s in the tower of attached dose of suspension.Suspension containing adsorbent is under solid phase Dynamic Adsorption tower
Endfeed mouth continuous feed, bottom continuous feed of the pending feed liquid from solid phase Dynamic Adsorption tower；Pending feed liquid and containing absorption
The suspension of agent enters solid phase Dynamic Adsorption tower in simultaneously stream mode.
Solid phase Dynamic Adsorption in the tower, stirring, between paddle linear velocity 1m/s-6m/s, by tower inner disk, fully
Contact, mixed material residence time 0.2-1h.Tower top discharging enters filter, and filter leading portion obtains the adsorbent after use,
Filter back segment obtains product solution；Obtained adsorbent can burn, and material-compound tank is put into after can also handling and is continued cycling through makes
With.
A kind of device of liquid-solid system Dynamic Adsorption, described device include solid phase Dynamic Adsorption tower；To realize above-mentioned solid phase
Dynamic Adsorption, comes into full contact with adsorbent and pending solution, and special designing is carried out to solid phase Dynamic Adsorption tower；The solid phase is moved
Paddle and disk are set in state adsorption tower, and disk diameter is equal to solid phase Dynamic Adsorption tower internal diameter, sets and stir among adjacent discs
Leaf is mixed, 0.4 ~ 0.6 times of a diameter of solid phase Dynamic Adsorption tower internal diameter of paddle, paddle is straight leaf, without inclination angle, is avoided
Abrasion is produced to adsorbent 1 in whipping process, while avoids influencing the flow field of upper area.Adjacent discs spacing and tower internal diameter
Ratio be 0.3-2:1.
The disk perforate, opening diameter are at least 10 times of 1 particle of adsorbent, and the opening area of disk is divided into disk
Layer and disk outer layer, using shaft as the center of circle, disc radius 1/2 at be separation, close to the center of circle border circular areas be disk in
Layer, remaining is disk outer layer.
The percent opening of same disk, disk internal layer and disk outer layer is different；If disk internal layer percent opening is 1% ~ 10%,
Disk outer layer percent opening is 10% ~ 20%；
The percent opening of two neighboring disk same layer is different, if the disk internal layer percent opening of upper disk is 1% ~ 10%,
The disk internal layer percent opening of lower disc is 10% ~ 20%.Such a design method can cause the route that mixed solution flows in tower
It is waveform, avoids mixed solution from directly rising along tower, be sufficiently mixed solution adsorbent, while avoids the appearance in dead band.Circle
The specific number of plies of disk is determined by the property of pending feed liquid.
Specific two kinds of opening approach are as follows：
Calculated from tower top, the disk of odd-level, the percent opening of disk internal layer:1%-10%, disk outer layer percent opening are 10%-
20%, the disk internal layer percent opening of odd-level is consistently less than outer layer percent opening；The disk of even level, disk internal layer percent opening：10%-
20%, disk outer layer percent opening：1%-10%, the disk internal layer percent opening of even level are consistently greater than outer layer percent opening；
Alternatively,
Calculated from tower top, the disk of odd-level, disk internal layer percent opening:10%-20%, disk outer layer percent opening：1%-10%,
The disk internal layer percent opening of odd-level is consistently greater than outer layer percent opening.；The disk of even level, disk internal layer percent opening： 1%-
10%, disk outer layer percent opening：10%-20%, the disk internal layer percent opening of even level are consistently less than outer layer percent opening.
Compared with prior art, beneficial effects of the present invention are as follows：
1）The present invention uses Dynamic Adsorption so that adsorbent comes into full contact with solution, and there is no adsorbed with absorption
The phenomenon of layer saturation, it is ensured that product quality is stablized；
Serialization for solution is decolourized, the percent of decolourization of detection primary production, the decoloration that detection is 1000 times per 10-90 minutes
Rate, percentage point deviation range are only ± 0.007 ~ ± 0.01；
Methyl alcohol process is gone in serialization for wastewater containing methanol, was detected a methanol content every 60 minutes, is detected 40 times
Go methanol rate, percentage point deviation range is ± 0.04.
2）The present invention, adsorbent moment keep flow regime, it is not necessary to parking displacement, suitable for continuous production.
3）The present invention uses Dynamic Adsorption, only under agitation so that material is uniformly mixed with adsorbent, it is not necessary to volume
Outer power consumption, is continuously available equal quality product under identical treating capacity, and energy consumption saves 30%.The prior art is in order to carry
High adsorption time, can use the method for increase bed height, but resistance drop can be increased, and power consumption also increases therewith.
4）The Dynamic gas-mixing and adsorption devices of the present invention pass through the uniform mixing of adsorbent and material, adsorbent utilization rate 100%.It is existing
There is technology during the very big Static Adsorption for the treatment of capacity, solution is in flowing, due to the presence of tube wall resistance so that on solution
The arc-shaped evagination in surface, the adsorbent of both sides are not utilized well, and the utilization rate of Static Adsorption adsorbent only has 80% left side
It is right.
5）Product after continuous processing of the present invention, impurity residual is low, and loss of effective components is few, and the product solution of every batch of
In, impurity residual and loss of effective components rate keep stablizing, and fluctuation is small,
Serialization for solution is decolourized, the impurity residual and amino acid loss late of detection primary production per 10-90 minutes,
Detection 1000 times, impurity residual rate scope are 1.25-1.91%, and percentage point deviation range is only ± 0.04 ~ ± 0.06；Detection
1000 times, the loss late of active ingredient is 0.07-2.38%, and percentage point deviation range is only ± 0.02 ~ ± 0.22.
For dye wastewater treatment, the COD removal rates of every 70 minutes detection primary productions, detect 1000 COD removal rates
For 5-5.4%, percentage point deviation range is only ± 0.06.
Brief description of the drawings：
Attached drawing 1：The present invention carries out the flow chart of liquid-solid system Dynamic Adsorption using solid phase Dynamic Adsorption tower；
Attached drawing 2：The overlooking the structure diagram of disk in solid phase Dynamic Adsorption tower（Outer layer percent opening is more than internal layer）；
Attached drawing 3：The overlooking the structure diagram of disk in solid phase Dynamic Adsorption tower（Outer layer percent opening is less than internal layer）；
In figure：
A-solid phase Dynamic Adsorption tower；B-shaft；C-paddle；D-disk；
E-filter；F-material-compound tank；H-disk internal layer；I-disk outer layer；
1-adsorbent；The liquid that 2-adsorbent is used cooperatively；3-the suspension containing adsorbent；4-pending feed liquid；
5-tower top discharges；Adsorbent after 6-use；7-product solution.
Embodiment
The preferred embodiment of the present invention is illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
A kind of method of liquid-solid system Dynamic Adsorption of embodiment 1
Comprise the following steps：
（1）Prepare the suspension containing adsorbent
The liquid 2 that adsorbent 1 and adsorbent are used cooperatively is according to 1:2 ratio（By mass）Into material-compound tank F, warp
Cross the suspension 3 for stirring evenly and being mixed to get containing adsorbent；
The adsorbent 1 is 20 ~ 40 mesh active fruit shell carbons；
The liquid 2 that the adsorbent is used cooperatively is water.
（2）Charging
Suspension 3 containing adsorbent from the lower end feed inlet continuous feed of solid phase Dynamic Adsorption tower A, pending feed liquid 4 from
The bottom continuous feed of solid phase Dynamic Adsorption tower A, adsorbent 1 are 1 with the mass ratio of pending feed liquid 4:1000, material to be processed
Flow velocity is 0.1cm/s in the tower of liquid 4 and suspension 3 containing adsorbent.
The pending feed liquid 4, is methionine mother liquor；
Pending feed liquid before processing, detects absorbance.
（3）Solid phase Dynamic Adsorption in tower
The paddle C linear velocities of solid phase Dynamic Adsorption tower A are 1m/s, and the residence time of mixed material is 0.5h, and tower top goes out
Material 5 enters filter E, the adsorbent after use 6 and product solution 7 is obtained by filtration, the adsorbent 6 after use sends to post processing；
Product solution 7 detected an absorbance, impurity residual, loss of effective components rate every 10 minutes.
A kind of method of liquid-solid system Dynamic Adsorption of embodiment 2
Comprise the following steps：
（1）Prepare the suspension containing adsorbent
The liquid 2 that adsorbent 1 and adsorbent are used cooperatively is according to 3:10 ratio（By mass）Into material-compound tank F, warp
The suspension 3 for stirring evenly and being mixed to get containing adsorbent is crossed,
The adsorbent 1 is powder active fruit shell carbon；
The liquid 2 that the adsorbent is used cooperatively, is threonine mother liquor.
（2）Charging
Suspension 3 containing adsorbent from the lower end feed inlet continuous feed of solid phase Dynamic Adsorption tower A, pending feed liquid 4 from
The bottom of solid phase Dynamic Adsorption tower A continuously enters；Adsorbent 1 is 1 with the mass ratio of pending feed liquid 4:3000, material to be processed
Flow velocity is 0.8cm/s in the tower of liquid 4 and suspension 3 containing adsorbent.
The pending feed liquid 4 is threonine mother liquor；
Pending feed liquid before processing, detects absorbance.
（3）Solid phase Dynamic Adsorption in tower
The paddle C linear velocities of solid phase Dynamic Adsorption tower A are 3m/s, and the residence time of mixed material is 0.3h, and tower top goes out
Material 5 enters filter E, and the adsorbent after use 6 and product solution 7 is obtained by filtration；Adsorbent 6 after use sends to post processing；
Product solution 7 detected an absorbance, impurity residual, loss of effective components rate every 30 minutes.
A kind of method of liquid-solid system Dynamic Adsorption of embodiment 3
Comprise the following steps：
（1）Prepare the suspension containing adsorbent
The liquid 2 that adsorbent 1 and adsorbent are used cooperatively is according to 1:5 ratio（By mass）Into material-compound tank F, pass through
Stir evenly and be mixed to get the suspension 3 containing adsorbent；
The adsorbent 1 adsorbs resin for D315 types；
The liquid 2 that the adsorbent is used cooperatively is water.
（2）Charging
Suspension 3 containing adsorbent from the lower end feed inlet continuous feed of solid phase Dynamic Adsorption tower A, pending feed liquid 4 from
The bottom of solid phase Dynamic Adsorption tower A continuously enters；Adsorbent 1 is 1 with the mass ratio of pending feed liquid 4:5000, material to be processed
Flow velocity is 1.2cm/s in the tower of liquid 4 and suspension 3 containing adsorbent.
The pending feed liquid 4 is sucrose solution；
Pending feed liquid before processing, detects absorbance.
（3）Solid phase Dynamic Adsorption in tower
The paddle C linear velocities of solid phase Dynamic Adsorption tower A are 4m/s, and the residence time of mixed material is 0.2h, and tower top goes out
Material 5 enters filter E, and the adsorbent after use 6 and product solution 7 is obtained by filtration；Adsorbent 6 after use sends to post processing；
Product solution 7 detected an absorbance, impurity residual, loss of effective components rate every 50 minutes.
A kind of method of liquid-solid system Dynamic Adsorption of embodiment 4
Comprise the following steps：
（1）Prepare the suspension containing adsorbent
The liquid 2 that adsorbent 1 and adsorbent are used cooperatively is according to 1:10 ratio（By mass）Into material-compound tank F, warp
Cross the suspension 3 for stirring evenly and being mixed to get containing adsorbent.
The adsorbent 1 adsorbs resin for DA201 types；
The liquid 2 that the adsorbent is used cooperatively is water.
（2）Charging
Suspension 3 containing adsorbent from the lower end feed inlet continuous feed of solid phase Dynamic Adsorption tower A, pending feed liquid 4 from
The bottom of solid phase Dynamic Adsorption tower A continuously enters, and adsorbent 1 is 1 with the mass ratio of pending feed liquid 4:8000, material to be processed
Flow velocity is 1.5cm/s in the tower of liquid 4 and suspension 3 containing adsorbent.
The pending feed liquid 4 is waste water from dyestuff；
Pending feed liquid before processing, detects absorbance.
（3）Solid phase Dynamic Adsorption in tower
The paddle C linear velocities of solid phase Dynamic Adsorption tower A are 4m/s, and the residence time of mixed material is 0.8h, and tower top goes out
Material 5 enters filter E, and the adsorbent after use 6 and product solution 7 is obtained by filtration；Adsorbent 6 after use sends to post processing；
Product solution 7 is every 70 minutes absorbances of detection and COD removal rates.
A kind of method of liquid-solid system Dynamic Adsorption of embodiment 5
Comprise the following steps：
（1）Prepare the suspension containing adsorbent
The liquid 2 that adsorbent 1 and adsorbent are used cooperatively is according to 1:5 ratio（By mass）Into material-compound tank F, pass through
Stir evenly and be mixed to get the suspension 3 containing adsorbent,
The adsorbent 1 adsorbs resin for 213 types；
The liquid 2 that the adsorbent is used cooperatively is methionine mother liquor.
（2）Charging
Suspension 3 containing adsorbent from the lower end feed inlet continuous feed of solid phase Dynamic Adsorption tower A, pending feed liquid 4 from
The bottom of solid phase Dynamic Adsorption tower A continuously enters, and adsorbent 1 is 1 with the mass ratio of pending feed liquid 4:10000, it is pending
Flow velocity is 2cm/s in the tower of feed liquid 4 and suspension 3 containing adsorbent.
The pending feed liquid 4, is methionine mother liquor；
Pending feed liquid before processing, detects absorbance.
（3）Solid phase Dynamic Adsorption in tower
The paddle C linear velocities of solid phase Dynamic Adsorption tower A are 5m/s, and residence time of mixed material is 1h, tower top discharging 5
Into filter E, the adsorbent after use 6 and product solution 7 is obtained by filtration；Adsorbent 6 after use sends to post processing；Product
Solution 7 detected an absorbance, impurity residual, loss of effective components rate every 90 minutes.
Treatment effect predominantly detects the percent of decolourization that index is feed liquid.Percent of decolourization is detected using spectrophotometer.Calculate
Formula is as follows：
Percent of decolourization=（The absorbance of pending feed liquid-product solution absorbance）Absorbance × 100% of/pending feed liquid.
Testing result such as table 1 below.
The adsorption effect of adsorption method described in 1 1-5 of the embodiment of the present invention of table
Deviation *：Refer to using first time test result as standard, since being tested second, each test result is the same as the first time
The deviation percentage point range of test result, the stability of test result is illustrated with this
The present invention also to embodiment 1 into embodiment 5 in pending feed liquid adsorption process, impurity residual and active ingredient damage
Mistake rate is detected, as a result such as table 2 below：
Impurity is remained adsorption method described in 2 1-5 of the embodiment of the present invention of table and the influence of loss of effective components rate
Deviation *：Refer to using first time test result as standard, since being tested second, each test result is the same as the first time
The percentage point deviation range of test result, the stability of test result is illustrated with this.
A kind of method of liquid-solid system Dynamic Adsorption of embodiment 6
Comprise the following steps：
（1）Prepare the suspension containing adsorbent
The liquid 2 that adsorbent 1 and adsorbent are used cooperatively is according to 1:5 ratio（By mass）Into material-compound tank F, pass through
Stir evenly and be mixed to get the suspension 3 containing adsorbent；
The adsorbent 1 is 50 ~ 80 mesh cocoanut active charcoals；
The liquid 2 that the adsorbent is used cooperatively is water；
（2）Charging
Suspension 3 containing adsorbent from the lower end feed inlet continuous feed of solid phase Dynamic Adsorption tower A, pending feed liquid 4 from
The bottom of solid phase Dynamic Adsorption tower A continuously enters；Adsorbent 1 is 1 with the mass ratio of pending feed liquid 4:6000, material to be processed
Flow velocity is 1cm/s in the tower of liquid 4 and suspension 3 containing adsorbent.
The pending feed liquid 4 is wastewater containing methanol；
Pending feed liquid before processing, detects the content of methanol.
（3）Solid phase Dynamic Adsorption in tower
The paddle C linear velocities of solid phase Dynamic Adsorption tower A are 3m/s, and the residence time of mixed material is 0.6h, and tower top goes out
Material 5 enters filter E, and the adsorbent after use 6 and product solution 7 is obtained by filtration；Adsorbent 6 after use sends to post processing；
Product solution 7 detected once every 60 minutes.Testing index be methanol removal rate, testing result such as table 3 below：
The adsorption effect of adsorption method described in 3 embodiment of the present invention 6 of table
Deviation *：Refer to using first time test result as standard, since being tested second, each test result is the same as the first time
The percentage point deviation range of test result, the stability of test result is illustrated with this.
A kind of device of liquid-solid system Dynamic Adsorption of embodiment 7
Paddle C and disk D is set in solid phase Dynamic Adsorption tower A, disk D diameters are equal to solid phase Dynamic Adsorption tower A internal diameters,
Setting paddle C among adjacent discs D, 0.4 ~ 0.6 times of a diameter of solid phase Dynamic Adsorption tower A internal diameters of paddle C, paddle
C is straight leaf, without inclination angle, avoids producing abrasion to adsorbent 1 in whipping process.Adjacent discs D spacing and tower internal diameter ratio
Example is 0.3-2:1.
Disk D perforates, opening diameter are at least 10 times of 1 particle of adsorbent, and the opening area of disk D is divided into disk internal layer
H and disk outer layer I, using shaft B as the center of circle, disk D radiuses 1/2 at be separation, be disk close to the border circular areas in the center of circle
Internal layer H, remaining is disk outer layer I.
The percent opening of same disk D ectonexines is different.Calculated from tower top, 1 layer, 3 layers, 5 layers ... ..., 2n+1 layers（N is big
In the integer equal to 1）Disk internal layer H percent opening:1%≤disk internal layer percent opening≤10%, disk outer layer percent opening：10%
≤ disk outer layer percent opening≤20%.Internal layer percent opening is consistently less than outer layer percent opening.
Calculated from tower top, 2 layers, 4 layers, 6 layers ... ..., 2n layers of disk internal layer H percent openings：10%≤disk internal layer percent opening
≤ 20%, disk outer layer percent opening：1%≤disk outer layer percent opening≤10%.Internal layer percent opening is consistently greater than outer layer percent opening.
A kind of device of liquid-solid system Dynamic Adsorption of embodiment 8
Paddle C and disk D is set in solid phase Dynamic Adsorption tower A, disk D diameters are equal to solid phase Dynamic Adsorption tower A internal diameters,
Setting paddle C among adjacent discs D, 0.4 ~ 0.6 times of a diameter of solid phase Dynamic Adsorption tower A internal diameters of paddle C, paddle
C is straight leaf, without inclination angle, avoids producing abrasion to adsorbent 1 in whipping process.Adjacent discs D spacing and tower internal diameter ratio
Example is 0.3-2:1.Disk D perforates, opening diameter are at least ten times of 1 particle of adsorbent, and the opening area of disk D is divided into disk
Internal layer H and disk outer layer I, is separation using shaft B as the center of circle, at the half of disk D radiuses, close to the circle in the center of circle
Domain is disk internal layer H, remaining is disk outer layer I.
The percent opening of same disk D ectonexines is different.Calculated from tower top, 1 layer, 3 layers, 5 layers ... ..., 2n+1 layers（N is big
In the integer equal to 1）Disk internal layer H percent openings:10%≤disk internal layer percent opening≤20%, disk outer layer I percent openings：1%≤
Disk outer layer percent opening≤10%.Internal layer percent opening is consistently greater than outer layer percent opening.
Calculated from tower top, 2 layers, 4 layers, 6 layers ... ..., 2n layers of disk internal layer H percent openings：1%≤disk internal layer percent opening
≤ 10%, disk outer layer I percent openings：10%≤disk outer layer percent opening≤20%.Internal layer percent opening is consistently less than outer layer percent opening.
It after adsorbent 1 of the present invention filters out, can directly discard, be recycled after can also handling.
It is normal pressure in solid phase Dynamic Adsorption tower A of the present invention, feed liquid is full of whole tower, and upper end discharge method is spilling.
Unless otherwise indicated, the percentage employed in the present invention is mass percent.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To modify to the technical solution described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent replacement, improvement and so on, should be included in the present invention's
Within protection domain.
Claims (9)
- A kind of 1. method of liquid-solid system Dynamic Adsorption, it is characterised in that：Including preparing the suspension containing adsorbent, charging, tower Interior solid phase Dynamic Adsorption；Paddle and disk are set in the tower；Calculated from tower top, the disk of odd-level, the percent opening of disk internal layer:1%-10%, Disk outer layer percent opening is 10%-20%, the disk of odd-level, and internal layer percent opening is consistently less than outer layer percent opening；The disk of even level, disk internal layer percent opening：10%-20%, disk outer layer percent opening：1%-10%, the disk of even level are interior Layer percent opening is consistently greater than outer layer percent opening；Alternatively,Calculated from tower top, the disk of odd-level, disk internal layer percent opening:10%-20%, disk outer layer percent opening：1%-10%, odd number The disk internal layer percent opening of layer is consistently greater than outer layer percent opening；The disk of even level, disk internal layer percent opening：1%-10%, disk Outer layer percent opening：10%-20%, the disk internal layer percent opening of even level are consistently less than outer layer percent opening.
- A kind of 2. method of liquid-solid system Dynamic Adsorption according to claim 1, it is characterised in that：It is described to prepare containing absorption The suspension of agent, the liquid that adsorbent and adsorbent are used cooperatively is according to 1:The mass ratio mixing of 2-10, obtains containing absorption The suspension of agent.
- A kind of 3. method of liquid-solid system Dynamic Adsorption according to claim 2, it is characterised in that：The adsorbent is work Property charcoal or absorption resin；The liquid that the adsorbent is used cooperatively is water or pending feed liquid.
- A kind of 4. method of liquid-solid system Dynamic Adsorption according to claim 3, it is characterised in that：The activated carbon is powder One kind in last active fruit shell carbon, 50 ~ 80 mesh cocoanut active charcoals；The absorption resin adsorbs resin for D315 types, DA201 types are inhaled One kind in attached resin, 213 types absorption resin；The pending feed liquid for methionine mother liquor, threonine mother liquor, sucrose solution, One kind in waste water from dyestuff, wastewater containing methanol.
- A kind of 5. method of liquid-solid system Dynamic Adsorption according to claim 3, it is characterised in that：The adsorbent it is close Degree is less than the density for the liquid that adsorbent is used cooperatively；The mass ratio for the liquid that the adsorbent is used cooperatively with adsorbent is small In equal to 50%.
- A kind of 6. method of liquid-solid system Dynamic Adsorption according to claim 2, it is characterised in that：The charging, absorption Agent is 1 with the mass ratio of pending feed liquid:1000 ~ 10000, flow velocity in the tower of pending feed liquid and the suspension containing adsorbent It is 0.1cm/s-2cm/s.
- A kind of 7. method of liquid-solid system Dynamic Adsorption according to claim 1, it is characterised in that：Solid phase is moved in the tower State is adsorbed, and the linear velocity of the paddle of solid phase Dynamic Adsorption tower is 1m/s-6m/s, and the residence time of mixed material is 0.2-1h.
- A kind of 8. method of liquid-solid system Dynamic Adsorption according to claim 1, it is characterised in that：Described disk diameter etc. In solid phase Dynamic Adsorption tower internal diameter, paddle is set, paddle is straight leaf, a diameter of solid phase of paddle among adjacent discs The ratio of 0.4 ~ 0.6 times of Dynamic Adsorption tower internal diameter, adjacent discs spacing and tower internal diameter is 0.3-2:1.
- A kind of 9. method of liquid-solid system Dynamic Adsorption according to claim 8, it is characterised in that：The disk perforate, Opening diameter is at least 10 times of absorbent particles, and the opening area of disk is divided into disk internal layer and disk outer layer, using shaft as The center of circle, disc radius 1/2 at be separation, be disk internal layer close to the border circular areas in the center of circle, remaining is disk outer layer.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85103972A (en) * | 1984-07-30 | 1986-11-12 | 前进企业公司 | liquid-solid contact device and method |
| CN1174881A (en) * | 1996-05-23 | 1998-03-04 | Ohmi研究和工程技术有限公司 | Method and apparatus for adsorptive cleaning of substances |
| CN101143274A (en) * | 2006-08-08 | 2008-03-19 | Ifp公司 | Process and device for simulated moving bed seperation with a reduced number of valves |
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| JPH10263309A (en) * | 1997-03-26 | 1998-10-06 | Takenori Tanimura | Multistage liquid-solid extraction apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85103972A (en) * | 1984-07-30 | 1986-11-12 | 前进企业公司 | liquid-solid contact device and method |
| CN1174881A (en) * | 1996-05-23 | 1998-03-04 | Ohmi研究和工程技术有限公司 | Method and apparatus for adsorptive cleaning of substances |
| CN101143274A (en) * | 2006-08-08 | 2008-03-19 | Ifp公司 | Process and device for simulated moving bed seperation with a reduced number of valves |
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