CN108404879A - A kind of preparation method of high-performance Dye Adsorption material - Google Patents
A kind of preparation method of high-performance Dye Adsorption material Download PDFInfo
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The present invention provides a kind of preparation methods of high-performance Dye Adsorption material, include the following steps:(1)Straw powder, beech wood powder and benzyl carbinol solution are mixed and extracted, extract is discarded;(2)Ethanol water is added, glacial acetic acid is used in combination to adjust pH, stirring;(3)Heating, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirring;(4)Deionized water is added after cleaning and is configured to aqueous suspension, is placed in high-speed grinder and grinds;(5)It is transferred to homogeneous in high pressure homogenizer and obtains finely dispersed suspension;(6)Graphene oxide, giantreed activated carbon/carboxy methyl konjaku gel micro-ball and humic acid, high speed dispersion is added;(7)It is transferred in Ultrasonic cell smash and is ultrasonically treated;(8)It pours and casts from culture dish, be freeze-dried to obtain the final product.Material prepared by this method has superelevation porosity, very good to the adsorption effect of dyestuff.
Description
Technical field
The present invention relates to a kind of preparation methods of high-performance Dye Adsorption material.
Background technology
Aeroge makes it in the U.S. as a kind of special low density porous material, excellent specific surface area and porosity
《Science》On magazine, it is cited as one of ten big hot topic science and technology of 21 century, being paid close attention to by various countries researcher.In aeroge
The decentralized medium in portion is mostly air, and porosity is up to 80%-99.8%, and bore hole size is generally 1-100nm, while also possessing pole
Big specific surface area, can reach 400-1000m2/g.Since material itself is mostly gas, density can be down to 3-600kg/m3。
Aeroge has the advantages such as high-specific surface area, high porosity and low-density, absorption, catalysis, heat-insulated etc. all
There is larger application prospect.And different raw materials and method is selected to become the weight of research to improve the aeroge of strong adsorption
Point.
Invention content
Technical problems to be solved:The object of the present invention is to provide a kind of preparation method of high-performance Dye Adsorption material,
Prepared material has superelevation porosity, very good to the adsorption effect of dyestuff.
Technical solution:A kind of preparation method of high-performance Dye Adsorption material, ingredient by weight, including following step
Suddenly:
(1)10-20 parts of straw powders, 10-20 parts of beech wood powders and 200 parts of benzene-ethanol solution are mixed, 5- is extracted at 90 DEG C
6h discards extract, wherein the volume ratio of benzene and ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 4-5, stir 5-6h;
(3)It is heated to 80-90 DEG C, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 10-20min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 20-30min obtains finely dispersed suspension;
(6)2-3 parts of graphene oxides of addition, 0.2-0.5 parts of giantreed activated carbon/carboxy methyl konjaku gel micro-balls and 0.2-0.4 parts
Humic acid, the high speed dispersion 10min at 14000-15000rpm;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 750-800W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 8-10h at < -55 DEG C of temperature to obtain the final product.
It is further preferred that the preparation method of the giantreed activated carbon/carboxy methyl konjaku gel micro-ball is:
The first step:5 parts of konjac glucomannans, 2 parts of monoxones and 40 part of 70% ethanol water are mixed, are warming up to after stirring 4 h
60 DEG C, 4 parts NaOH and 30 part 70 % ethanol waters are added, react 3 h;
Second step:Mixture is washed repeatedly to neutrality with 85% ethanol water, and being put into baking oven at 50 DEG C dry 12 h must change
Konjac glucomannan after property;
Third walks:2 parts of giantreed activated carbons and 96 parts of deionized waters are mixed, at the uniform velocity stirring makes powder be uniformly dispersed, and adds 2 parts
Modified konjac glucomannan stirs 1-2h, ultrasonic deaeration 3-5min;
4th step:Mixed liquor is added drop-wise to the AlCl of 3wt% with syringe pump3In solution, bead is collected after being crosslinked 24-26 h, is taken out
Bead is rinsed in filter repeatedly;
5th step:It is put into baking oven at 50 DEG C dry 10-12 h to obtain the final product.
It is further preferred that the grain size of the giantreed activated carbon/carboxy methyl konjaku gel micro-ball is 20-40 μm.
It is further preferred that the preparation method of the giantreed activated carbon is:
The first step:It is dried after giantreed is cleaned, is crushed to 40 mesh, be put into air dry oven in 105 DEG C of dry 5-8h;
Second step:10 parts of giantreed powder, 25 parts of pyrophosphoric acids and 30 parts of deionized waters are mixed, stirs evenly, impregnates 4- at room temperature
5h;
Third walks:Filtering, is transferred in Muffle furnace, the carbonization-activation 1h at 350-600 DEG C;
4th step:It is cooled to room temperature, is washed with distilled water to neutrality, be put into baking oven the drying at 100 DEG C, be ground to grain size <
20 μm to obtain the final product.
Advantageous effect:
1. surface of graphene oxide contains a large amount of hydroxyl, contain a large amount of carboxyl on nano-cellulose and humic acid, so three
Person easily forms hydrogen bond by functional group, and then is adhered to each other to each other, and very strong interaction force is presented.
2. gel micro-ball is uniformly distributed in aeroge, very strong suction-operated is played for dyestuff.
3. high-performance Dye Adsorption material of the present invention has superelevation porosity, 99.7% or more, have for methylene blue
There are very high adsorbance, adsorbance to reach as high as 279.9g/g, it is very good to the adsorption effect of dyestuff.
Specific implementation mode
Embodiment 1
A kind of preparation method of high-performance Dye Adsorption material, ingredient by weight, include the following steps:
(1)10 parts of straw powders, 10 parts of beech wood powders and 200 parts of benzene-ethanol solution are mixed, 5h is extracted at 90 DEG C, discards
Extract, wherein the volume ratio of benzene and ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 4, stir 5h;
(3)80 DEG C are heated to, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 10min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 20min obtains finely dispersed suspension;
(6)2 parts of graphene oxides, 0.2 part of giantreed activated carbon/carboxy methyl konjaku gel micro-ball and 0.2 part of humic acid is added,
High speed dispersion 10min under 14000rpm;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 750W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 8h at -57 DEG C of temperature to obtain the final product.
Embodiment 2
A kind of preparation method of high-performance Dye Adsorption material, ingredient by weight, include the following steps:
(1)15 parts of straw powders, 15 parts of beech wood powders and 200 parts of benzene-ethanol solution are mixed, 5.5h is extracted at 90 DEG C, abandons
Remove extract, wherein the volume ratio of benzene and ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 4.5, stir 5.5h;
(3)85 DEG C are heated to, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 15min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 25min obtains finely dispersed suspension;
(6)22 parts of graphene oxides, 0.3 part of giantreed activated carbon/carboxy methyl konjaku gel micro-ball and 0.3 part of humic acid is added,
High speed dispersion 10min under 14500rpm;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 770W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 9h at -58 DEG C of temperature to obtain the final product.
Embodiment 3
A kind of preparation method of high-performance Dye Adsorption material, ingredient by weight, include the following steps:
(1)15 parts of straw powders, 15 parts of beech wood powders and 200 parts of benzene-ethanol solution are mixed, 5.5h is extracted at 90 DEG C, abandons
Remove extract, wherein the volume ratio of benzene and ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 4.5, stir 5.5h;
(3)85 DEG C are heated to, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 15min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 25min obtains finely dispersed suspension;
(6)2.5 parts of graphene oxides, 0.4 part of giantreed activated carbon/carboxy methyl konjaku gel micro-ball and 0.3 part of humic acid is added,
High speed dispersion 10min under 14500rpm;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 780W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 9h at -59 DEG C of temperature to obtain the final product.
Embodiment 4
A kind of preparation method of high-performance Dye Adsorption material, ingredient by weight, include the following steps:
(1)20 parts of straw powders, 20 parts of beech wood powders and 200 parts of benzene-ethanol solution are mixed, 6h is extracted at 90 DEG C, discards
Extract, wherein the volume ratio of benzene and ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 5, stir 6h;
(3)90 DEG C are heated to, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 20min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 30min obtains finely dispersed suspension;
(6)3 parts of graphene oxides, 0.5 part of giantreed activated carbon/carboxy methyl konjaku gel micro-ball and 0.4 part of humic acid is added,
High speed dispersion 10min under 15000rpm;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 800W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 10h at -60 DEG C of temperature to obtain the final product.
Comparative example 1
The present embodiment is with embodiment 1 the difference is that not containing giantreed activated carbon/carboxy methyl konjaku gel micro-ball, specially:
A kind of preparation method of high-performance Dye Adsorption material, ingredient by weight, include the following steps:
(1)10 parts of straw powders, 10 parts of beech wood powders and 200 parts of benzene-ethanol solution are mixed, 5h is extracted at 90 DEG C, discards
Extract, wherein the volume ratio of benzene and ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 4, stir 5h;
(3)80 DEG C are heated to, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 10min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 20min obtains finely dispersed suspension;
(6)2 parts of graphene oxides and 0.2 part of humic acid, the high speed dispersion 10min at 14000rpm is added;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 750W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 8h at -57 DEG C of temperature to obtain the final product.
Comparative example 2
The present embodiment is with embodiment 1 the difference is that not containing humic acid, specially:
A kind of preparation method of high-performance Dye Adsorption material, ingredient by weight, include the following steps:
(1)10 parts of straw powders, 10 parts of beech wood powders and 200 parts of benzene-ethanol solution are mixed, 5h is extracted at 90 DEG C, discards
Extract, wherein the volume ratio of benzene and ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 4, stir 5h;
(3)80 DEG C are heated to, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 10min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 20min obtains finely dispersed suspension;
(6)2 parts of graphene oxides and 0.2 part of giantreed activated carbon/carboxy methyl konjaku gel micro-ball is added, the high speed at 14000rpm
Disperse 10min;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 750W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 8h at -57 DEG C of temperature to obtain the final product.
Comparative example 3
The present embodiment is with embodiment 1 the difference is that replacing beech wood powder with straw powder, specially:
A kind of preparation method of high-performance Dye Adsorption material, ingredient by weight, include the following steps:
(1)20 parts of straw powders and 200 parts of benzene-ethanol solution are mixed, 5h is extracted at 90 DEG C, discards extract, wherein benzene and
The volume ratio of ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 4, stir 5h;
(3)80 DEG C are heated to, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 10min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 20min obtains finely dispersed suspension;
(6)2 parts of graphene oxides, 0.2 part of giantreed activated carbon/carboxy methyl konjaku gel micro-ball and 0.2 part of humic acid is added,
High speed dispersion 10min under 14000rpm;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 750W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 8h at -57 DEG C of temperature to obtain the final product.
Comparative example 4
The present embodiment is with embodiment 1 the difference is that replacing straw powder with beech wood powder, specially:
A kind of preparation method of high-performance Dye Adsorption material, ingredient by weight, include the following steps:
(1)20 parts of beech wood powders and 200 parts of benzene-ethanol solution are mixed, 5h is extracted at 90 DEG C, discards extract, wherein
The volume ratio of benzene and ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 4, stir 5h;
(3)80 DEG C are heated to, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 10min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 20min obtains finely dispersed suspension;
(6)2 parts of graphene oxides, 0.2 part of giantreed activated carbon/carboxy methyl konjaku gel micro-ball and 0.2 part of humic acid is added,
High speed dispersion 10min under 14000rpm;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 750W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 8h at -57 DEG C of temperature to obtain the final product.
The partial properties index of 1 high-performance Dye Adsorption material of table
Name of product | Porosity(%) | Methylene blue adsorption number amount(g/g) |
Embodiment 1 | 99.73 | 278.9 |
Embodiment 2 | 99.76 | 279.4 |
Embodiment 3 | 99.82 | 279.9 |
Embodiment 4 | 99.79 | 279.7 |
Comparative example 1 | 99.75 | 263.4 |
Comparative example 2 | 99.73 | 271.9 |
Comparative example 3 | 99.67 | 259.8 |
Comparative example 4 | 99.69 | 259.2 |
The partial properties index of high-performance Dye Adsorption material prepared by the method for the present invention is seen the above table, it may be seen that it has
There is superelevation porosity, 99.7% or more, there is very high adsorbance, adsorbance to reach as high as 279.9g/g methylene blue,
It is very good to the adsorption effect of dyestuff.
Claims (4)
1. a kind of preparation method of high-performance Dye Adsorption material, it is characterised in that:Ingredient by weight, including following step
Suddenly:
(1)10-20 parts of straw powders, 10-20 parts of beech wood powders and 200 parts of benzene-ethanol solution are mixed, 5- is extracted at 90 DEG C
6h discards extract, wherein the volume ratio of benzene and ethyl alcohol is 2:1;
(2)200 parts of ethanol waters are added, glacial acetic acid is used in combination to adjust pH to 4-5, stir 5-6h;
(3)It is heated to 80-90 DEG C, it is 10.5 that NaOH solution, which is added dropwise, and maintains reaction system pH, stirs 2h;
(4)Deionized water is added after being cleaned with deionized water and is configured to the aqueous suspension that mass concentration is 0.3%, is placed in high speed and grinds
In grinding machine, abrasive disk space is -5, and rotating speed is to grind 10-20min under 1500r/min;
(5)It being transferred in high pressure homogenizer, the pressure of level-one homogenizing valve is 700bar, and the pressure of double-stage homogenization valve is 100bar,
Homogenizing time is that 20-30min obtains finely dispersed suspension;
(6)2-3 parts of graphene oxides of addition, 0.2-0.5 parts of giantreed activated carbon/carboxy methyl konjaku gel micro-balls and 0.2-0.4 parts
Humic acid, the high speed dispersion 10min at 14000-15000rpm;
(7)It is transferred in Ultrasonic cell smash, 10min is ultrasonically treated under 750-800W power;
(8)It pours and casts from culture dish, be placed in freeze drier, dry 8-10h at < -55 DEG C of temperature to obtain the final product.
2. a kind of preparation method of high-performance Dye Adsorption material according to claim 1, it is characterised in that:The reed
The preparation method of bamboo absorbent charcoal/carboxy methyl konjaku gel micro-ball is:
The first step:5 parts of konjac glucomannans, 2 parts of monoxones and 40 part of 70% ethanol water are mixed, are warming up to after stirring 4 h
60 DEG C, 4 parts NaOH and 30 part 70 % ethanol waters are added, react 3 h;
Second step:Mixture is washed repeatedly to neutrality with 85% ethanol water, and being put into baking oven at 50 DEG C dry 12 h must change
Konjac glucomannan after property;
Third walks:2 parts of giantreed activated carbons and 96 parts of deionized waters are mixed, at the uniform velocity stirring makes powder be uniformly dispersed, and adds 2 parts
Modified konjac glucomannan stirs 1-2h, ultrasonic deaeration 3-5min;
4th step:Mixed liquor is added drop-wise to the AlCl of 3wt% with syringe pump3In solution, bead is collected after being crosslinked 24-26 h, filter,
Bead is rinsed repeatedly;
5th step:It is put into baking oven at 50 DEG C dry 10-12 h to obtain the final product.
3. a kind of preparation method of high-performance Dye Adsorption material according to claim 1, it is characterised in that:The reed
The grain size of bamboo absorbent charcoal/carboxy methyl konjaku gel micro-ball is 20-40 μm.
4. a kind of preparation method of high-performance Dye Adsorption material according to claim 2, it is characterised in that:The reed
The preparation method of bamboo absorbent charcoal is:
The first step:It is dried after giantreed is cleaned, is crushed to 40 mesh, be put into air dry oven in 105 DEG C of dry 5-8h;
Second step:10 parts of giantreed powder, 25 parts of pyrophosphoric acids and 30 parts of deionized waters are mixed, stirs evenly, impregnates 4- at room temperature
5h;
Third walks:Filtering, is transferred in Muffle furnace, the carbonization-activation 1h at 350-600 DEG C;
4th step:It is cooled to room temperature, is washed with distilled water to neutrality, be put into baking oven the drying at 100 DEG C, be ground to grain size <
20 μm to obtain the final product.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110237826A (en) * | 2019-06-21 | 2019-09-17 | 郑州大学 | A kind of inorganic porous material and its preparation and application for removing removing heavy metals |
CN113447646A (en) * | 2021-06-22 | 2021-09-28 | 浙江理工大学 | By using C-SiO2Method for accelerating ELISA detection process by using adsorbing material |
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