CN106237651B - Method and device for dynamic adsorption of liquid-solid system - Google Patents
Method and device for dynamic adsorption of liquid-solid system Download PDFInfo
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000007787 solid Substances 0.000 title claims abstract description 19
- 239000003463 adsorbent Substances 0.000 claims abstract description 140
- 239000007790 solid phase Substances 0.000 claims abstract description 59
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 239000000725 suspension Substances 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims description 89
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- 239000011347 resin Substances 0.000 claims description 13
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 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
- 239000004473 Threonine Substances 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
- 239000002245 particle Substances 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
- 239000005720 sucrose Substances 0.000 claims description 3
- 235000013399 edible fruits Nutrition 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 27
- 238000002835 absorbance Methods 0.000 description 13
- 239000012535 impurity Substances 0.000 description 12
- 238000001914 filtration Methods 0.000 description 7
- 230000003068 static effect Effects 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000004042 decolorization Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 239000002609 medium Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
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- 238000005299 abrasion Methods 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
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- 235000013305 food Nutrition 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
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
- 125000000341 threoninyl group Chemical group [H]OC([H])(C([H])([H])[H])C([H])(N([H])[H])C(*)=O 0.000 description 1
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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
- B01D15/02—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor with moving adsorbents
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Abstract
The invention provides a method for dynamic adsorption of liquid-solid systems, which comprises the steps of preparing suspension containing an adsorbent, feeding, and dynamically adsorbing solid phases in a tower; the invention also provides a device for dynamically adsorbing the liquid-solid system, which comprises a solid-phase dynamic adsorption tower; stirring blades and disks are arranged in the solid phase dynamic adsorption tower, the diameter of each stirring blade is 0.4-0.6 times of the inner diameter of the solid phase dynamic adsorption tower, the stirring blades are arranged in the middle of adjacent disks, each stirring blade is a straight blade, and the ratio of the distance between every two adjacent disks to the inner diameter of the tower is 0.3-2: 1. The invention adopts dynamic adsorption, so that the adsorbent is fully contacted with the solution, the phenomenon of saturation of an adsorption layer along with adsorption does not exist, and the stable product quality can be ensured; the method is used for decoloring the solution, the decoloring rate of the product is detected every 10 to 90 minutes, the decoloring rate is detected for 1000 times, and the deviation range of percentage points is only +/-0.007 to +/-0.01; low pressure drop, low energy consumption and high utilization rate of the adsorbent.
Description
Technical Field
The invention provides a method and a device for dynamic adsorption of a liquid-solid system, belonging to the field of chemical separation.
Background
The adsorption technology of liquid-solid system has been used for many years for refining and decoloring in medicine, chemical industry, food and other industries at home and abroad. Has important functions in the aspects of chemistry and chemical engineering, metallurgy, environmental protection and biotechnology.
At present, the application is mostly static adsorption, including traditional fixed bed adsorption, moving bed adsorption and the like, and adsorption is carried out through an adsorption bed layer; the feed liquid flows through the adsorption medium layer through the liquid distributor on the upper part of the column, flows out from the lower part of the column and is collected, and the fluid is gradually adsorbed in the medium layer to obtain the required product.
The prior art has the following defects:
in the static adsorption process, along with the adsorption process, the effective adsorbent layer is shorter and shorter, the saturated adsorbent is more and more, the impurity content of the adsorbed product is increased, and the product quality is unstable; for a single column, the adsorption medium is static, the larger the treatment capacity of the feed liquid is, the more and more the saturated amount of the adsorption medium is, and the quality of the product obtained each time is also unstable;
static adsorption requires shutdown replacement when the adsorbent is saturated and loses adsorption capacity, and belongs to intermittent operation, so that the treatment capacity is small, and automatic control is not easy to realize. If continuous production is carried out, a plurality of devices must be configured for standby replacement, and the equipment cost is high.
Meanwhile, desorption and other treatment are needed after the adsorbent is saturated under the static condition, and if the adsorbent is used for continuous production, a plurality of columns need to be configured for standby replacement;
sometimes, in order to shorten the adsorption time, the height of the adsorption medium layer is increased, but the resistance drop is increased, and the energy consumption is increased.
The product treated by the prior art has more loss of effective components.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a method and a device for liquid-solid system dynamic adsorption, which aim to realize the following purposes:
(1) after the treatment, the obtained product has stable quality;
(2) the invention can fully utilize the adsorbent and is suitable for continuous production;
(3) the method and the device have low equipment cost and low energy consumption;
(4) the utilization rate of the adsorbent is high;
(5) the product treated by the method has low impurity content and low loss of effective components;
in order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for dynamic adsorption of liquid-solid systems, which is characterized in that: comprises preparing suspension containing adsorbent, feeding, and dynamically adsorbing solid phase in the column.
The following is a further improvement of the above technical solution:
the adsorption scheme of the invention relates to the following process flows:
liquid used by matching the adsorbent and the adsorbent enters a batching tank after being metered, the adsorbent-containing suspension is obtained by stirring and mixing uniformly, the adsorbent-containing suspension is fed from the lower end of the solid-phase dynamic adsorption tower A, and the feed inlet is positioned at the lower end of the last disc. The feed liquid to be treated enters from the bottom of the solid phase dynamic adsorption tower A. Discharging from the top of the tower, entering a filter E, and filtering to obtain the used adsorbent and a product solution.
The adsorbent-containing suspension is prepared by mixing an adsorbent and a liquid used by matching the adsorbent according to a mass ratio of 1:2-10 to obtain the adsorbent-containing suspension, wherein the adsorbent is used as a dispersion medium and is mixed in the liquid to keep the adsorbent in a flowing state all the time.
The adsorbent is activated carbon or adsorption resin; the liquid used by matching the adsorbent is water or feed liquid to be treated, and the adsorbent is required to be ensured not to be dissolved in the liquid.
The active carbon is one of 20-40 mesh shell active carbon, powdered shell active carbon and 50-80 mesh coconut shell active carbon; the adsorption resin is one of D315 type adsorption resin, DA201 type adsorption resin and 213 type adsorption resin; the feed liquid to be treated is one of methionine mother liquid, threonine mother liquid, sucrose solution, dye wastewater and methanol-containing wastewater.
Meanwhile, in order to ensure that the adsorbent is uniformly mixed with the feed liquid after entering the solid phase dynamic adsorption tower, the adsorbent does not sink to block a feed inlet, and the density of the adsorbent is required to be less than that of the liquid matched with the adsorbent; the mass ratio of the adsorbent to the liquid used in combination with the adsorbent is less than or equal to 50%.
The mass ratio of the adsorbent to the feed liquid to be treated is 1: 1000-10000, and the tower internal flow velocity of the feed liquid to be treated and the suspension containing the adsorbent is 0.1-2 cm/s. Continuously feeding the suspension containing the adsorbent from a feed inlet at the lower end of the solid-phase dynamic adsorption tower, and continuously feeding the feed liquid to be treated from the bottom of the solid-phase dynamic adsorption tower; the feed liquid to be treated and the suspension containing the adsorbent enter the solid phase dynamic adsorption tower in a parallel flow state.
The solid phase in the tower is dynamically adsorbed and stirred, the linear velocity of a stirring blade is between 1m/s and 6m/s, the solid phase and the stirring blade are fully contacted through an inner disc of the tower, and the retention time of the mixed materials is 0.2 to 1 hour. The discharged material at the top of the tower enters a filter, the used adsorbent is obtained at the front section of the filter, and the product solution is obtained at the rear section of the filter; the obtained adsorbent can be incinerated or can be put into a dosing tank for continuous recycling after treatment.
A liquid-solid system dynamic adsorption device comprises a solid phase dynamic adsorption tower; in order to realize the solid phase dynamic adsorption, the adsorbent is fully contacted with the solution to be treated, and the solid phase dynamic adsorption tower is specially designed; the stirring blade and the disks are arranged in the solid phase dynamic adsorption tower, the diameter of each disk is equal to the inner diameter of the solid phase dynamic adsorption tower, the stirring blade is arranged in the middle of each adjacent disk, the diameter of each stirring blade is 0.4-0.6 times of the inner diameter of the solid phase dynamic adsorption tower, each stirring blade is a straight blade and has no inclination angle, abrasion to the adsorbent 1 in the stirring process is avoided, and meanwhile, the influence on the flow field of an upper area is avoided. The ratio of the distance between adjacent disks to the inner diameter of the column is 0.3-2: 1.
The disc is perforated, the diameter of the perforated hole is at least 10 times of that of 1 particle of the adsorbent, the perforated area of the disc is divided into an inner disc layer and an outer disc layer, the rotating shaft is used as the circle center, 1/2 of the radius of the disc is used as a dividing point, the circular area close to the circle center is the inner disc layer, and the rest of the circular area is the outer disc layer.
The hole opening rates of the inner layer and the outer layer of the disc are different; if the aperture ratio of the inner layer of the disc is 1% -10%, the aperture ratio of the outer layer of the disc is 10% -20%;
the aperture ratio of the same layer of the two adjacent disks is different, and if the aperture ratio of the inner layer of the upper disk is 1% -10%, the aperture ratio of the inner layer of the lower disk is 10% -20%. The design mode can enable the flow route of the mixed solution in the tower to be wavy, avoids the mixed solution from directly rising along the tower, enables the solution adsorbent to be fully mixed, and avoids dead zones. The specific number of layers of the disc is determined by the properties of the feed liquid to be treated.
Two specific aperturing schemes are as follows:
the opening rate of the inner layer of the disc is 1-10%, the opening rate of the outer layer of the disc is 10-20%, and the opening rate of the inner layer of the disc of the odd layer is always smaller than that of the outer layer; even-numbered layers of the disc, the opening ratio of the inner layer of the disc: 10% -20%, disc outer layer aperture ratio: 1% -10%, the aperture ratio of the inner layer of the disk of the even number layer is always larger than that of the outer layer;
or,
the opening rate of the inner layer of the disc is 10-20%, and the opening rate of the outer layer of the disc is as follows: 1% -10%, and the aperture ratio of the inner layer of the disc of the odd layer is always larger than that of the outer layer. (ii) a Even-numbered layers of the disc, the opening ratio of the inner layer of the disc: 1% -10%, disc outer layer aperture ratio: 10% -20%, and the aperture ratio of the inner layer of the disk of the even layer is always smaller than that of the outer layer.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention adopts dynamic adsorption, so that the adsorbent is fully contacted with the solution, the phenomenon of saturation of an adsorption layer along with adsorption does not exist, and the stable product quality can be ensured;
the method is used for continuous decolorization of a solution, the decolorization rate of the product is detected every 10-90 minutes, the decolorization rate is detected for 1000 times, and the deviation range of percentage points is only +/-0.007 to +/-0.01;
the method is used for continuous methanol removal treatment of methanol-containing wastewater, the methanol content is detected every 60 minutes, the methanol removal rate is detected for 40 times, and the deviation range of percentage points is +/-0.04.
2) The invention keeps the flowing state of the adsorbent all the time, does not need to be stopped and replaced, and is suitable for continuous production.
3) The invention adopts dynamic adsorption, and only under the stirring condition, the materials are uniformly mixed with the adsorbent, so that the product with the same quality can be continuously obtained under the same treatment capacity without extra power consumption, and the energy consumption is saved by 30%. In the prior art, in order to improve the adsorption time, a method of increasing the height of a bed layer is adopted, but the resistance drop is increased, and the power consumption is increased.
4) The dynamic adsorption device of the invention has the advantages that the utilization rate of the adsorbent is 100 percent by uniformly mixing the adsorbent and the materials. In the prior art, in the static adsorption process with large treatment capacity, when a solution flows, the upper surface of the solution is cambered and protrudes outwards due to the resistance of the tube wall, adsorbents on two sides are not well utilized, and the utilization rate of the static adsorption adsorbent is only about 80%.
5) The product after continuous treatment of the invention has low impurity residue and low loss of effective components, and the impurity residue and the loss rate of the effective components in the product solution of each batch are kept stable and have small fluctuation,
the method is used for continuous decolorization of a solution, the impurity residue and amino acid loss rate of a product are detected every 10-90 minutes for 1000 times, the range of the impurity residue rate is 1.25-1.91%, and the deviation range of percentage points is only +/-0.04-0.06; the loss rate of the effective components is 0.07-2.38% after 1000 times of detection, and the deviation range of percentage points is only +/-0.02 to +/-0.22.
The method is used for treating dye wastewater, the COD removal rate of the product is detected every 70 minutes, the COD removal rate is 5-5.4% after 1000 times of detection, and the deviation range of percentage points is only +/-0.06.
Description of the drawings:
FIG. 1: the invention adopts a flow chart of a solid-phase dynamic adsorption tower to carry out dynamic adsorption of a liquid-solid system;
FIG. 2 is a drawing: a schematic view of a overlook structure of a disc in the solid-phase dynamic adsorption tower (the opening ratio of an outer layer is greater than that of an inner layer);
FIG. 3: a schematic view of a overlook structure of a disc in the solid-phase dynamic adsorption tower (the opening ratio of an outer layer is smaller than that of an inner layer);
in the figure:
a-a solid phase dynamic adsorption tower; b, a rotating shaft; c, stirring blades; d, a disc;
e, a filter; f, a batching tank; h, inner layer of disc; i, an outer layer of the disc;
1-an adsorbent; 2-liquid used by matching with the adsorbent; 3-adsorbent-containing suspension; 4-feed liquid to be treated; 5, discharging at the top of the tower; 6-adsorbent after use; 7-product solution.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1A method of dynamic adsorption of liquid and solid substances
The method comprises the following steps:
(1) preparation of adsorbent-containing suspension
Adding a liquid 2 used by matching the adsorbent 1 and the adsorbent into a batching tank F according to the proportion of 1:2 (by mass), and uniformly stirring and mixing to obtain a suspension 3 containing the adsorbent;
the adsorbent 1 is 20-40 meshes of shell activated carbon;
the liquid 2 used with the adsorbent is water.
(2) Feeding of the feedstock
The method comprises the following steps of continuously feeding adsorbent-containing suspension 3 from a feed inlet at the lower end of a solid-phase dynamic adsorption tower A, continuously feeding to-be-treated feed liquid 4 from the bottom of the solid-phase dynamic adsorption tower A, wherein the mass ratio of the adsorbent 1 to the to-be-treated feed liquid 4 is 1:1000, and the in-tower flow rates of the to-be-treated feed liquid 4 and the adsorbent-containing suspension 3 are both 0.1 cm/s.
The feed liquid 4 to be treated is methionine mother liquor;
and detecting the absorbance before the treatment of the feed liquid to be treated.
(3) Dynamic adsorption of solid phase in tower
The linear velocity of a stirring blade C of the solid phase dynamic adsorption tower A is 1m/s, the retention time of the mixed materials is 0.5h, the discharged materials 5 at the top of the tower enter a filter E, the used adsorbent 6 and a product solution 7 are obtained by filtration, and the used adsorbent 6 is sent to post-treatment; the product solution 7 is detected for absorbance, impurity residue and effective component loss rate every 10 minutes.
Example 2 dynamic adsorption method for liquid-solid systems
The method comprises the following steps:
(1) preparation of adsorbent-containing suspension
The adsorbent 1 and the liquid 2 matched with the adsorbent are put into a batching tank F according to the proportion of 3:10 (by mass), and are stirred and mixed evenly to obtain suspension 3 containing the adsorbent,
the adsorbent 1 is powdered fruit shell activated carbon;
the liquid 2 used in cooperation with the adsorbent is threonine mother liquor.
(2) Feeding of the feedstock
Continuously feeding adsorbent-containing suspension 3 from a feed inlet at the lower end of the solid-phase dynamic adsorption tower A, and continuously feeding to-be-treated feed liquid 4 from the bottom of the solid-phase dynamic adsorption tower A; the mass ratio of the adsorbent 1 to the material liquid 4 to be treated is 1:3000, and the tower internal flow rates of the material liquid 4 to be treated and the suspension 3 containing the adsorbent are both 0.8 cm/s.
The feed liquid 4 to be treated is threonine mother liquid;
and detecting the absorbance before the treatment of the feed liquid to be treated.
(3) Dynamic adsorption of solid phase in tower
The linear velocity of a stirring blade C of the solid phase dynamic adsorption tower A is 3m/s, the retention time of the mixed materials is 0.3h, the discharged materials 5 at the top of the tower enter a filter E, and the used adsorbent 6 and the product solution 7 are obtained by filtering; the used adsorbent 6 is sent to post-treatment; the product solution 7 is detected for absorbance, impurity residue and effective component loss rate every 30 minutes.
Example 3 dynamic adsorption method for liquid-solid systems
The method comprises the following steps:
(1) preparation of adsorbent-containing suspension
The adsorbent 1 and the liquid 2 matched with the adsorbent are fed into a batching tank F according to the proportion (by mass) of 1:5, and are stirred and mixed uniformly to obtain a suspension 3 containing the adsorbent;
the adsorbent 1 is D315 type adsorbent resin;
the liquid 2 used with the adsorbent is water.
(2) Feeding of the feedstock
Continuously feeding adsorbent-containing suspension 3 from a feed inlet at the lower end of the solid-phase dynamic adsorption tower A, and continuously feeding to-be-treated feed liquid 4 from the bottom of the solid-phase dynamic adsorption tower A; the mass ratio of the adsorbent 1 to the material liquid 4 to be treated is 1:5000, and the tower internal flow rates of the material liquid 4 to be treated and the suspension 3 containing the adsorbent are both 1.2 cm/s.
The feed liquid 4 to be treated is a sucrose solution;
and detecting the absorbance before the treatment of the feed liquid to be treated.
(3) Dynamic adsorption of solid phase in tower
The linear velocity of a stirring blade C of the solid phase dynamic adsorption tower A is 4m/s, the retention time of the mixed materials is 0.2h, the discharged materials 5 at the top of the tower enter a filter E, and the used adsorbent 6 and the product solution 7 are obtained by filtering; the used adsorbent 6 is sent to post-treatment; the product solution 7 is detected for absorbance, impurity residue and effective component loss rate every 50 minutes.
Example 4A method of dynamic adsorption of liquid and solid substances
The method comprises the following steps:
(1) preparation of adsorbent-containing suspension
The adsorbent 1 and the liquid 2 used together by the adsorbent enter a batching tank F according to the proportion of 1:10 (by mass), and the suspension 3 containing the adsorbent is obtained by uniformly stirring and mixing.
The adsorbent 1 is DA201 type adsorbent resin;
the liquid 2 used with the adsorbent is water.
(2) Feeding of the feedstock
The suspension 3 containing the adsorbent is continuously fed from a feed inlet at the lower end of the solid phase dynamic adsorption tower A, the feed liquid 4 to be treated continuously enters from the bottom of the solid phase dynamic adsorption tower A, the mass ratio of the adsorbent 1 to the feed liquid 4 to be treated is 1:8000, and the flow rate in the tower of the feed liquid 4 to be treated and the suspension 3 containing the adsorbent is 1.5 cm/s.
The feed liquid 4 to be treated is dye wastewater;
and detecting the absorbance before the treatment of the feed liquid to be treated.
(3) Dynamic adsorption of solid phase in tower
The linear velocity of a stirring blade C of the solid phase dynamic adsorption tower A is 4m/s, the retention time of the mixed materials is 0.8h, the discharged materials 5 at the top of the tower enter a filter E, and the used adsorbent 6 and the product solution 7 are obtained by filtering; the used adsorbent 6 is sent to post-treatment; the absorbance and the COD removal rate of the product solution 7 were measured every 70 minutes.
Example 5A method of dynamic adsorption of liquid and solid substances
The method comprises the following steps:
(1) preparation of adsorbent-containing suspension
The adsorbent 1 and the liquid 2 used by matching the adsorbent are put into a batching tank F according to the proportion of 1:5 (by mass), and are stirred and mixed evenly to obtain suspension 3 containing the adsorbent,
the adsorbent 1 is 213 type adsorbent resin;
the liquid 2 used with the adsorbent is methionine mother liquor.
(2) Feeding of the feedstock
The method comprises the following steps of continuously feeding adsorbent-containing turbid liquid 3 from a feed inlet at the lower end of a solid-phase dynamic adsorption tower A, continuously feeding to-be-treated feed liquid 4 from the bottom of the solid-phase dynamic adsorption tower A, wherein the mass ratio of an adsorbent 1 to the to-be-treated feed liquid 4 is 1:10000, and the tower internal flow rates of the to-be-treated feed liquid 4 and the adsorbent-containing turbid liquid 3 are both 2 cm/s.
The feed liquid 4 to be treated is methionine mother liquor;
and detecting the absorbance before the treatment of the feed liquid to be treated.
(3) Dynamic adsorption of solid phase in tower
The linear velocity of a stirring blade C of the solid phase dynamic adsorption tower A is 5m/s, the retention time of the mixed materials is 1h, the discharged materials 5 at the tower top enter a filter E, and the used adsorbent 6 and the product solution 7 are obtained by filtering; the used adsorbent 6 is sent to post-treatment; the product solution 7 is detected for absorbance, impurity residue and effective component loss rate every 90 minutes.
The main detection index of the treatment effect is the decoloration rate of the feed liquid. The decolorization ratio is detected by a spectrophotometer. The calculation formula is as follows:
decolorization rate = (absorbance of material liquid to be treated-absorbance of product solution)/absorbance of material liquid to be treated x 100%.
The results are shown in Table 1 below.
TABLE 1 adsorption Effect of the adsorption method described in examples 1 to 5 of the present invention
Deviation: the deviation percentage range of each test result from the second test to the first test result is used as the standard to indicate the stability of the test result
The invention also detects the impurity residue and the loss rate of effective components in the process of adsorbing the feed liquid to be treated in the embodiments 1 to 5, and the results are shown in the following table 2:
TABLE 2 influence of the adsorption method according to the invention described in examples 1 to 5 on the impurity residue and the loss rate of the active principle
Deviation: the deviation range of the percentage point of each test result from the first test result is indicated by taking the first test result as a standard, and the stability of the test result is indicated by the deviation range of the percentage point of each test result from the second test.
Example 6A method of dynamic adsorption of liquid and solid substances
The method comprises the following steps:
(1) preparation of adsorbent-containing suspension
The adsorbent 1 and the liquid 2 matched with the adsorbent are fed into a batching tank F according to the proportion (by mass) of 1:5, and are stirred and mixed uniformly to obtain a suspension 3 containing the adsorbent;
the adsorbent 1 is 50-80 meshes of coconut shell activated carbon;
the liquid 2 used in cooperation with the adsorbent is water;
(2) feeding of the feedstock
Continuously feeding adsorbent-containing suspension 3 from a feed inlet at the lower end of the solid-phase dynamic adsorption tower A, and continuously feeding to-be-treated feed liquid 4 from the bottom of the solid-phase dynamic adsorption tower A; the mass ratio of the adsorbent 1 to the material liquid 4 to be treated is 1:6000, and the tower internal flow velocity of the material liquid 4 to be treated and the suspension liquid 3 containing the adsorbent is 1 cm/s.
The feed liquid 4 to be treated is methanol-containing wastewater;
and detecting the content of the methanol before the treatment of the feed liquid to be treated.
(3) Dynamic adsorption of solid phase in tower
The linear velocity of a stirring blade C of the solid phase dynamic adsorption tower A is 3m/s, the retention time of the mixed materials is 0.6h, the discharged materials 5 at the top of the tower enter a filter E, and the used adsorbent 6 and the product solution 7 are obtained by filtering; the used adsorbent 6 is sent to post-treatment; product solution 7 was tested every 60 minutes. The detection index is the removal rate of methanol, and the detection results are shown in the following table 3:
TABLE 3 adsorption Effect of the adsorption method according to the invention as described in example 6
Deviation: the deviation range of the percentage point of each test result from the first test result is indicated by taking the first test result as a standard, and the stability of the test result is indicated by the deviation range of the percentage point of each test result from the second test.
EXAMPLE 7 device for dynamic adsorption of liquid and solid substances
Set up stirring leaf C and disc D in the solid phase dynamic adsorption tower A, disc D diameter equals solid phase dynamic adsorption tower A internal diameter, sets up stirring leaf C in the middle of adjacent disc D, and stirring leaf C's diameter is 0.4~0.6 times of solid phase dynamic adsorption tower A internal diameter, and stirring leaf C is straight leaf, does not have the inclination, avoids producing wearing and tearing to adsorbent 1 at the stirring in-process. The ratio of the distance between adjacent disks D to the inner diameter of the tower is 0.3-2: 1.
The disk D is perforated, the diameter of the perforated hole is at least 10 times that of the 1 particle of the adsorbent, the perforated area of the disk D is divided into a disk inner layer H and a disk outer layer I, the rotating shaft B is used as the circle center, the 1/2 position of the radius of the disk D is a dividing point, the circular area close to the circle center is the disk inner layer H, and the rest is the disk outer layer I.
The inner and outer layers of the same disk D have different opening rates. The opening rate of the inner layer H of the disc of 1 layer, 3 layers, 5 layers, … … layers and 2n +1 layers (n is an integer more than or equal to 1) is more than or equal to 1 percent and less than or equal to 10 percent, and the opening rate of the outer layer of the disc is as follows: the opening rate of the outer layer of the disc is more than or equal to 10 percent and less than or equal to 20 percent. The aperture ratio of the inner layer is always smaller than that of the outer layer.
The opening ratio of the inner layer H of the disc of 2 layers, 4 layers, 6 layers, … … and 2n layers calculated from the tower top is as follows: the opening rate of the inner layer of the disc is more than or equal to 10% and less than or equal to 20%, and the opening rate of the outer layer of the disc is as follows: the opening rate of the outer layer of the disc is more than or equal to 1 percent and less than or equal to 10 percent. The aperture ratio of the inner layer is always larger than that of the outer layer.
EXAMPLE 8 apparatus for dynamic adsorption of liquid-solid System
Set up stirring leaf C and disc D in the solid phase dynamic adsorption tower A, disc D diameter equals solid phase dynamic adsorption tower A internal diameter, sets up stirring leaf C in the middle of adjacent disc D, and stirring leaf C's diameter is 0.4~0.6 times of solid phase dynamic adsorption tower A internal diameter, and stirring leaf C is straight leaf, does not have the inclination, avoids producing wearing and tearing to adsorbent 1 at the stirring in-process. The ratio of the distance between adjacent disks D to the inner diameter of the tower is 0.3-2: 1. The disk D is provided with holes, the diameter of each hole is at least ten times that of the adsorbent 1 particles, the hole area of the disk D is divided into a disk inner layer H and a disk outer layer I, the rotating shaft B is used as the circle center, one half of the radius of the disk D is used as a dividing point, the circular area close to the circle center is used as the disk inner layer H, and the rest is used as the disk outer layer I.
The inner and outer layers of the same disk D have different opening rates. The porosity of the inner layer H of the disc is more than or equal to 10% and less than or equal to 20%, and the porosity of the outer layer I of the disc is calculated from the tower top, wherein the porosity of the inner layer H of the disc is more than or equal to 10% and less than or equal to 20%, and the porosity of the outer layer I of the disc is calculated from the tower top: the opening rate of the outer layer of the disc is more than or equal to 1 percent and less than or equal to 10 percent. The aperture ratio of the inner layer is always larger than that of the outer layer.
The opening ratio of the inner layer H of the disc of 2 layers, 4 layers, 6 layers, … … and 2n layers calculated from the tower top is as follows: the aperture ratio of the inner layer of the disc is more than or equal to 1% and less than or equal to 10%, the aperture ratio of the outer layer I of the disc is as follows: the opening rate of the outer layer of the disc is more than or equal to 10 percent and less than or equal to 20 percent. The aperture ratio of the inner layer is always smaller than that of the outer layer.
The adsorbent 1 can be directly discarded after being filtered out, and can also be recycled after being treated.
The solid phase dynamic adsorption tower A is at normal pressure, the whole tower is filled with feed liquid, and the discharge mode at the upper end is overflow.
All percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for dynamic adsorption of liquid-solid systems, which is characterized in that: comprises preparing suspension containing adsorbent, feeding, and dynamically adsorbing solid phase in the column;
stirring blades and a disc are arranged in the tower; the opening rate of the inner layer of the disc is 1-10%, the opening rate of the outer layer of the disc is 10-20%, and the opening rate of the inner layer of the disc is always smaller than that of the outer layer of the disc of the odd layer;
even-numbered layers of the disc, the opening ratio of the inner layer of the disc: 10% -20%, disc outer layer aperture ratio: 1% -10%, the aperture ratio of the inner layer of the even-numbered disc is always larger than that of the outer layer;
or,
the opening rate of the inner layer of the disc is 10-20%, and the opening rate of the outer layer of the disc is as follows: 1% -10%, the aperture ratio of the inner layer of the disc of the odd layer is always larger than that of the outer layer; even-numbered layers of the disc, the opening ratio of the inner layer of the disc: 1% -10%, disc outer layer aperture ratio: 10% -20%, and the aperture ratio of the inner layer of the disk of the even layer is always smaller than that of the outer layer.
2. The method according to claim 1, wherein: the adsorbent-containing suspension is prepared by mixing the adsorbent and liquid used by matching the adsorbent according to the mass ratio of 1:2-10 to obtain the adsorbent-containing suspension.
3. The method according to claim 2, wherein: the adsorbent is activated carbon or adsorption resin; the liquid used by matching the adsorbent is water or feed liquid to be treated.
4. The method according to claim 3, wherein: the activated carbon is one of powdered fruit shell activated carbon and coconut shell activated carbon of 50-80 meshes; the adsorption resin is one of D315 type adsorption resin, DA201 type adsorption resin and 213 type adsorption resin; the feed liquid to be treated is one of methionine mother liquid, threonine mother liquid, sucrose solution, dye wastewater and methanol-containing wastewater.
5. The method according to claim 3, wherein: the density of the adsorbent is less than that of the liquid matched with the adsorbent; the mass ratio of the adsorbent to the liquid used in combination with the adsorbent is less than or equal to 50%.
6. The method according to claim 2, wherein: the mass ratio of the adsorbent to the feed liquid to be treated is 1: 1000-10000, and the tower internal flow velocity of the feed liquid to be treated and the suspension containing the adsorbent is 0.1-2 cm/s.
7. The method according to claim 1, wherein: the solid phase dynamic adsorption in the tower is carried out, the linear velocity of a stirring blade of the solid phase dynamic adsorption tower is 1m/s-6m/s, and the retention time of the mixed material is 0.2-1 h.
8. The method according to claim 1, wherein: the diameter of each disc is equal to the inner diameter of the solid-phase dynamic adsorption tower, the stirring blades are arranged in the middle of the adjacent discs and are straight blades, the diameter of each stirring blade is 0.4-0.6 times of the inner diameter of the solid-phase dynamic adsorption tower, and the ratio of the distance between the adjacent discs to the inner diameter of the tower is 0.3-2: 1.
9. The method according to claim 8, wherein: the disc is perforated, the diameter of the perforated hole is at least 10 times of that of the adsorbent particles, the perforated area of the disc is divided into a disc inner layer and a disc outer layer, the rotating shaft is used as the circle center, 1/2 of the radius of the disc is used as a dividing point, the circular area close to the circle center is used as the disc inner layer, and the rest of the circular area is used as the disc outer layer.
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| 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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| 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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Application publication date: 20161221 Assignee: Ningbo Zhenhai Refining and Chemical Xinhecheng Biotechnology Co.,Ltd. Assignor: SHANDONG XINHECHENG AMINO ACID Co.,Ltd. Contract record no.: X2024980000380 Denomination of invention: A method and device for dynamic adsorption of liquid-solid systems Granted publication date: 20180427 License type: Common License Record date: 20240115 |