CN108816206A - A kind of preparation method of efficient absorption oil absorption material - Google Patents
A kind of preparation method of efficient absorption oil absorption material Download PDFInfo
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- CN108816206A CN108816206A CN201810849459.7A CN201810849459A CN108816206A CN 108816206 A CN108816206 A CN 108816206A CN 201810849459 A CN201810849459 A CN 201810849459A CN 108816206 A CN108816206 A CN 108816206A
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- 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
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Abstract
The present invention relates to a kind of preparation methods of efficient absorption oil absorption material, belong to environment-friendly materials technical field.The present invention carries out gel using oil spilling of the fuel thickener made of soyabean protein powder to absorption, then floats on the water surface.There was only carbon carbon saturation segment and phenyl ring side group in the segment of polystyrene, nonpolarity or low pole is presented, there is good hydrophobic-lipophilic.Electrostatic spinning fiber has lesser fibre diameter, lesser fiber membrane aperture, higher porosity and coarse micro-nano multilevel structure, and because of the introducing of multilevel structure, the specific surface area and pore volume for increasing substantially fiber enhance oil product in the wettability of fiber surface, the small-bore of fiber can also enhance capillary pressure, improve to the adsorptivity of oil product and huge specific surface area also increases oil absorption;The solidifying oil of oil suction is high-efficient, and oil suction coagulates oil mass greatly and not will cause secondary pollution, can be widely applied to the preparation field that light wood material is coagulated in marine oil spill oil suction.
Description
Technical field
The present invention relates to a kind of preparation methods of efficient absorption oil absorption material, belong to environment-friendly materials technical field.
Background technique
With the rapid development of science and technology, the discharge of a large amount of industrial wastewaters and oil carrier, oil tank leakage accident cause water
Body pollution, oil pollutant are to cause one of major pollutants of water pollution, constitute serious prestige to ecological environment
The side of body.Oil pollutant in common absorption method processing water body.Oil absorption material is as a kind of functionality for waste oil recycling, processing
Material is widely used in millwork leakage of oil, oil, food waste oil and sea and land crude oil leakage in plant chimney stalk
Processing.Common are type oil absorption material and inorganic type oil absorption material exist more adsorption efficiency is low, easily cause secondary pollution, at
The defects of this is high.How effectively to administer the petroleum and products thereof spilt into ocean or other water bodys is many countries and mechanism
Research emphasis, by prolonged effort, existing main oil spilling control measures include:Physical method(The oil fence, asphalt felt,
Oil skimmer etc.), chemical method(Detergent, fuel thickener etc.)And biological method(Dispensing bites oily microorganism or nutritive salt etc. and promotes petroleum
Decomposition), the often combined use of a variety of governing measures in an oil spill accident.Although having developed a variety of oil spilling improvement sides
Method, but there are still some at high cost, low efficiencys, oil spilling processing be not thorough the problems such as still allow of no optimist.Therefore, how to make
It is one of hot and difficult issue of current research that standby efficient out, cheap oil spilling, which administers material, with huge social benefit and
Economic benefit.Wherein, fuel thickener can float on the water surface and beat convenient for machinery by oil spilling rapid condensation at solid or semisolid bulk
Fishing, it has many advantages, such as effectively to inhibit, and the diffusion of oil, toxicity is low, condensation of oil is convenient for recycling;Oil absorbent can effectively adsorb oil spilling,
And oil cut rate can be effectively kept, convenient for salvaging, recycling.
Small molecule fuel thickener is a hot spot of current research, mainly utilizes the self assembly performance of small molecule, small molecule
Between can be self-assembly of in one-dimensional direction fibre by non-covalent interactions such as hydrogen bond, Van der Waals force, electrostatic attractions
Shape, band-like, tubulose or helical form nanostructure are tieed up, then intertwine with each other into three-dimensional network structure, utilizes surface on this basis
Oil spilling equal solvent molecule is retained or be fixed in network by tension, capillary force etc. forms gel.Physical gel is typically belonged to,
Different with chemical gel, physical gel can be realized the reversible phase transition of sol-gel under certain outside stimulus, such as hot
Time of small molecule fuel thickener and solidifying oil may be implemented using the phase transition of this sol-gel for processing, concussion, mechanical shearing etc.
It receives and recycles.And the small molecule structure unit in small molecule fuel thickener be mainly some abundances, have unique stereochemical structure and
The natural products molecule of more decorating sites, such as:Amino acid, carbohydrate, cholesterol, organic salt etc., this not only simplifies synthesis step,
Many advantages, such as more imparting gel rubber system environmental protection, economy, biocompatibility has huge researching value and application potential.
But the method that fuel thickener reported in the literature can effectively coagulate oil now usually mixes fuel thickener with oil product, using adding
Cosolvent is added in promotion gelling in heat of solution-room temperature cooling means in the mixture of fuel thickener and oil product, this is for reality
Border is using there are certain difficulties.A kind of important material is exactly using natural material as base in the developing direction of oil absorbent
Plinth, by simply handling the oil absorbent product of preparation environment-friendly type, in numerous processing methods, high temperature pyrolysis carbonization is a kind of ratio
More effective, simple method.Although oil absorbent can effectively adsorb oil spilling, factice cannot be coagulated.
In short, preparing Biocomposite material using waste spinning fiber, dirt of the traditional treatment method to environment not only can solve
Dye problem, and solve the problems, such as shortage of resources and waste to a certain extent, accomplish real environmentally friendly low-carbon, to have
Certain economic benefit and social benefit.Therefore, how to prepare efficient, cheap oil spilling and administer the heat that material is current research
One of point and difficult point, with huge Social benefit and economic benefit.
Summary of the invention
The technical problems to be solved by the invention:It is deposited for common are type oil absorption material and inorganic type oil absorption material more
Adsorption efficiency it is low, easily cause the problem of secondary pollution, propose a kind of preparation method of efficient absorption oil absorption material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1)Soyabean protein powder, deionized water, sodium chloroacetate and sodium hydroxide is taken to be uniformly mixing to obtain mixed liquor A;
(2)Mixed liquor A is heated to 40 DEG C of reaction 2h, 70 DEG C of reaction 2h is then heated to and obtains mixed liquid B, then by mixed liquid B
It is cooled to 0 DEG C and obtains mixed liquor C;
(3)It takes mixed liquor C, acetone and tetradecylic acid acyl chlorides is added, 4mol/L sodium hydroxide solution is added dropwise and adjusts pH9 ~ 10, reaction 3 ~
4h obtains reaction solution;
(4)It extracts reaction solution, aluminium chloride is added, addition ferric chloride solution adjusts pH to 6 ~ 8 after precipitating, and centrifugation washing obtains after dry
To fuel thickener;
(5)Polystyrene, tetrahydrofuran and nano SiO 2 particle are stirred evenly, electrostatic spinning apparatus is put into and is spun
Silk, obtains electrostatic spinning fiber, obtains fibrous material for 24 hours in 80 DEG C of dryings;
(6)Fibrous material and maleic anhydride inoculated polypropylene are taken, silane coupling agent, twin-screw extrusion master batch is added;
(7)Starch and deionized water are mixed, adhesive is obtained;
(8)Master batch and ammonium hydrogen carbonate are taken, adhesive is added, foaming 30min obtains foamed material under the conditions of 100 DEG C of sealing, will send out
Foam material crushed after being dried obtains granular foamed material;
(9)Fuel thickener and granular foamed material are taken, is put into acetone and stirs, 30 ~ 40 DEG C, after 2 ~ 3h is warming up to, filters out drying, obtain
To efficient absorption oil absorption material.
Step(1)The soyabean protein powder, deionized water, sodium chloroacetate and sodium hydroxide mass ratio be 4:15:5:2.
Step(3)The mass ratio of the solution C, acetone and tetradecylic acid acyl chlorides is 40:15:3.
Step(4)The mass ratio of the reaction solution and aluminium chloride is 20:1.
Step(5)The mass ratio of the polystyrene tetrahydrofuran and nano SiO 2 particle is 3:6:1.
Step(6)The fibrous material, maleic anhydride inoculated polypropylene, silane coupling agent mass ratio are 500:500:1.
Step(6)The silane coupling agent is vinyltriethoxysilane, vinyltrimethoxysilane, vinyl three
One of (beta-methoxy ethyoxyl) silane.
Step(7)The starch and the mass ratio of deionized water are 2:3.
Step(8)The master batch, ammonium hydrogen carbonate and adhesive quality ratio are 5:6:10.
Step(9)The mass ratio of the fuel thickener, granular foamed material and acetone is 1:4:6.
The present invention is compared with other methods, and advantageous effects are:
(1)Soybean protein itself contains part ester, these ester groups be it is oil-soluble, referred to as lipophilic group, their presence makes carboxylic
Methyl soybean protein has part lipophilic, so that grease system be made to be capable of forming WO emulsion;In soybean protein
It is added to ferric ion, so fuel thickener has more hydroxyls, is capable of forming more Hydrogenbonds, thus make to be formed
The structure of oleogel is more stable;And the water solubility of salt that ferric ion and carboxymethyl are formed is small, so product is in water
It is not easy to be dispersed by water, oleogel water imbibition is small, the water surface can be floated on, so solidifying oil better performances;
(2)There was only carbon carbon saturation segment and phenyl ring side group in the segment of polystyrene, nonpolarity or low pole is presented, has good
Hydrophobic-lipophilic, therefore, manufactured electrostatic spinning fiber have good hydrophobic-lipophilic;Simultaneously electrostatic spinning fiber have compared with
Small fibre diameter, lesser fiber membrane aperture, higher porosity and coarse micro-nano multilevel structure, and because it is multistage
The introducing of structure, the specific surface area and pore volume for increasing substantially fiber enhance oil product in the wettability of fiber surface, fiber
Small-bore can also enhance capillary pressure, improve to the adsorptivity of oil product and huge specific surface area also increase oil suction
Amount;
(3)The present invention improves the adsorptivity to oil spilling using electrostatic spinning fiber, then carries out foaming processing to electrostatic spinning fiber, so that
The density of entire material reduces, and after foaming is handled, the hole of entire material is more, can adsorb more oil spillings;
It recycles fuel thickener made of soyabean protein powder to carry out gel to the oil spilling of absorption, then floats on the water surface, facilitate recycling and again
It utilizes;The solidifying oil of oil suction is high-efficient, and oil suction coagulates oil mass greatly and not will cause secondary pollution, can be widely applied to marine oil spill oil suction
The preparation field of solidifying light wood material.
Specific embodiment
40 ~ 50g soyabean protein powder, 150 ~ 200g deionized water, 50 ~ 75g sodium chloroacetate and 20 ~ 25g sodium hydroxide is taken to stir
It mixes and uniformly obtains mixed liquor A, solution A is heated to 40 DEG C of reaction 2h, then be warming up to 70 DEG C of reaction 2h and obtain solution B;It will mixing
Liquid B is cooled to 0 DEG C and obtains mixed liquor C, takes 200 ~ 250g mixed liquor C, and 75 ~ 100g acetone and 25 ~ 30g tetradecylic acid acyl chlorides is added,
4mol/L sodium hydroxide is added dropwise and adjusts pH to 9 ~ 10,3 ~ 4h of reaction obtains reaction solution;250 ~ 300g reaction solution is taken, 12 ~ 15g is added
Ferric chloride solution is added after precipitating and adjusts pH to 6 ~ 8 for aluminium chloride, and centrifugation washing obtains fuel thickener after dry;90 ~ 100g is poly-
Styrene, 180 ~ 200g tetrahydrofuran and 30 ~ 40g nano SiO 2 particle stir evenly, and are put into electrostatic spinning apparatus progress
Spinning obtains electrostatic spinning fiber, obtains fibrous material for 24 hours in 80 DEG C of dryings;Take 200 ~ 250g fibrous material and 200 ~ 250g horse
The silane coupling agent of 0.5 ~ 1g, twin-screw extrusion master batch is added in maleic anhydride grafted polypropylene;By 200g starch and 300g deionization
Water mixing, obtains adhesive;200 ~ 220g master batch and 240 ~ 280g ammonium hydrogen carbonate are taken, 400 ~ 440g adhesive, sealing 100 is added
The 30min that foams under the conditions of DEG C obtains foamed material;By foamed material crushed after being dried, granular foamed material is obtained;Take 50 ~ 60g
Fuel thickener and the granular foamed material of 200 ~ 250g, are put into 300g acetone and stir, be warming up to 30 ~ 40 DEG C, after 2 ~ 3h, filter out dry
It is dry, efficient absorption oil absorption material is obtained after crushing.
Example 1
40g soyabean protein powder, 150g deionized water, 50g sodium chloroacetate and 20g sodium hydroxide is taken to be uniformly mixing to obtain mixed liquor A,
Mixed liquor A is heated to 40 DEG C of reaction 2h, then is warming up to 70 DEG C of reaction 2h and obtains mixed liquid B;Mixed liquid B is cooled to 0 DEG C to obtain
To mixed liquor C, take 200g mixed liquor C, 75g acetone and 25g tetradecylic acid acyl chlorides be added, be added dropwise 4mol/L sodium hydroxide adjust pH to
9, reaction 3h obtains reaction solution;250g reaction solution is taken, 12g aluminium chloride is added, ferric chloride solution is added after precipitating and adjusts pH to 6,
Centrifugation washing, obtains fuel thickener after dry;90g polystyrene, 180g tetrahydrofuran and 30g nano SiO 2 particle are stirred
Uniformly, it is put into electrostatic spinning apparatus and carries out spinning, obtain electrostatic spinning fiber, obtain fibrous material for 24 hours in 80 DEG C of dryings;Take 200g
The silane coupling agent of 0.5g, twin-screw extrusion master batch is added in fibrous material and 200g maleic anhydride inoculated polypropylene;200g is formed sediment
Powder and the mixing of 300g deionized water, obtain adhesive;200g master batch and 240g ammonium hydrogen carbonate are taken, 400g adhesive, sealing is added
The 30min that foams under the conditions of 100 DEG C obtains foamed material;By foamed material crushed after being dried, granular foamed material is obtained;Take 50g
Fuel thickener and the granular foamed material of 200g, are put into 300g acetone and stir, be warming up to 30 DEG C, after 2h, filter out and obtain after dry, pulverize
To efficient absorption oil absorption material.
Example 2
45g soyabean protein powder, 175g deionized water, 62g sodium chloroacetate and 23g sodium hydroxide is taken to be uniformly mixing to obtain mixed liquor A,
Mixed liquor A is heated to 40 DEG C of reaction 2h, then is warming up to 70 DEG C of reaction 2h and obtains mixed liquid B;Mixed liquid B is cooled to 0 DEG C to obtain
To mixed liquor C, take 225g mixed liquor C, 87g acetone and 27g tetradecylic acid acyl chlorides be added, be added dropwise 4mol/L sodium hydroxide adjust pH to
9.5, reaction 3.5h obtains reaction solution;275g reaction solution is taken, 13g aluminium chloride is added, ferric chloride solution is added after precipitating and adjusts pH
To 7, centrifugation washing obtains fuel thickener after dry;By 95g polystyrene, 190g tetrahydrofuran and 35g nano SiO 2 particle
It stirs evenly, is put into electrostatic spinning apparatus and carries out spinning, obtain electrostatic spinning fiber, obtain fibrous material for 24 hours in 80 DEG C of dryings;It takes
The silane coupling agent of 0.75g, twin-screw extrusion master batch is added in 225g fibrous material and 225g maleic anhydride inoculated polypropylene;It will
200g starch and the mixing of 300g deionized water, obtain adhesive;210g master batch and 260g ammonium hydrogen carbonate are taken, 420g gluing is added
Agent, foaming 30min obtains foamed material under the conditions of 100 DEG C of sealing;By foamed material crushed after being dried, granular foaming material is obtained
Material;55g fuel thickener and the granular foamed material of 225g are taken, is put into 300g acetone and stirs, is warming up to 35 DEG C, after 2.5h, is filtered out dry
It is dry, efficient absorption oil absorption material is obtained after crushing.
Example 3
50g soyabean protein powder, 200g deionized water, 75g sodium chloroacetate and 25g sodium hydroxide is taken to be uniformly mixing to obtain mixed liquor A,
Mixed liquor A is heated to 40 DEG C of reaction 2h, then is warming up to 70 DEG C of reaction 2h and obtains mixed liquid B;Mixed liquid B is cooled to 0 DEG C to obtain
To mixed liquor C, 250g mixed liquor C is taken, 100g acetone and 30g tetradecylic acid acyl chlorides is added, 4mol/L sodium hydroxide is added dropwise and adjusts pH
To 10,3 ~ 4h of reaction obtains reaction solution;300g reaction solution is taken, 15g aluminium chloride is added, ferric chloride solution is added after precipitating and adjusts pH
To 8, centrifugation washing obtains fuel thickener after dry;By 100g polystyrene, 200g tetrahydrofuran and 40g silica nanometer
Grain stirs evenly, and is put into electrostatic spinning apparatus and carries out spinning, obtains electrostatic spinning fiber, obtains fibrous material for 24 hours in 80 DEG C of dryings;
250g fibrous material and 250g maleic anhydride inoculated polypropylene are taken, the silane coupling agent of 1g, twin-screw extrusion master batch is added;It will
200g starch and the mixing of 300g deionized water, obtain adhesive;220g master batch and 280g ammonium hydrogen carbonate are taken, 440g gluing is added
Agent, foaming 30min obtains foamed material under the conditions of 100 DEG C of sealing;By foamed material crushed after being dried, granular foaming material is obtained
Material;60g fuel thickener and the granular foamed material of 250g are taken, is put into 300g acetone and stirs, 40 DEG C, after 3h is warming up to, filters out drying,
Efficient absorption oil absorption material is obtained after crushing.
The oil absorption material that efficient absorption oil absorption material prepared by the present invention and Shanghai company produce is detected, specifically
Testing result such as following table table 1:
Detection method:
(1)Oil absorbency test
500mL beaker equipped with the oil product after 200mL weathering is placed on after preheating 20min in 20 DEG C of water bath with thermostatic control, then will inhaled
Light wood material is put on homemade wire netting, then slowly immerses wire netting in oil product to be measured, weighing(It deducts on silk screen and silk screen
Adhere to the quality of oil product), the adsorbance of oil absorption material is calculated, with oil suction multiplying power(g/g)It indicates.
(2)Oil keeping test:
Claim oil absorption material W1 to be put in oil product, after it adsorbs 15min, be moved on stainless (steel) wire, stand 5min, weighs, note
Material weighing is taken out, is denoted as respectively after 5min, 10min, 20min, 40min, 60min, 90min and 120min are drained for W
W3。
1 efficient absorption oil absorption material performance characterization of table
It follows that efficient absorption oil absorption material prepared by the present invention, oil suction multiplying power is high, protects oil cut rate height, not will cause secondary dirt
Dye has high market value and application value.
Claims (10)
1. a kind of preparation method of efficient absorption oil absorption material, which is characterized in that specific production step is:
(1)Soyabean protein powder, deionized water, sodium chloroacetate and sodium hydroxide is taken to be uniformly mixing to obtain mixed liquor A;
(2)Mixed liquor A is heated to 40 DEG C of reaction 2h, 70 DEG C of reaction 2h is then heated to and obtains mixed liquid B, then by mixed liquid B
It is cooled to 0 DEG C and obtains mixed liquor C;
(3)Mixed liquor C is taken, acetone and tetradecylic acid acyl chlorides is added, 4mol/L sodium hydroxide solution is added dropwise and adjusts pH to 9 ~ 10, reaction
3 ~ 4h obtains reaction solution;
(4)It extracts reaction solution, aluminium chloride is added, addition ferric chloride solution adjusts pH to 6 ~ 8 after precipitating, and centrifugation washing obtains after dry
To fuel thickener;
(5)Polystyrene, tetrahydrofuran and nano SiO 2 particle are stirred evenly, electrostatic spinning apparatus is put into and is spun
Silk, obtains electrostatic spinning fiber, obtains fibrous material for 24 hours in 80 DEG C of dryings;
(6)Fibrous material and maleic anhydride inoculated polypropylene are taken, silane coupling agent, twin-screw extrusion master batch is added;
(7)Starch and deionized water are mixed, adhesive is obtained;
(8)Master batch and ammonium hydrogen carbonate are taken, adhesive is added, foaming 30min obtains foamed material under the conditions of 100 DEG C of sealing, will send out
Foam material crushed after being dried obtains granular foamed material;
(9)Fuel thickener and granular foamed material are taken, is put into acetone and stirs, 30 ~ 40 DEG C, after 2 ~ 3h is warming up to, filters out drying, obtain
To efficient absorption oil absorption material.
2. a kind of preparation method of efficient absorption oil absorption material as described in claim 1, which is characterized in that step(1)It is described
Soyabean protein powder, deionized water, sodium chloroacetate and sodium hydroxide mass ratio be 4:15:5:2.
3. a kind of preparation method of efficient absorption oil absorption material as described in claim 1, which is characterized in that step(3)It is described
The mass ratio of solution C, acetone and tetradecylic acid acyl chlorides is 40:15:3.
4. a kind of preparation method of efficient absorption oil absorption material as described in claim 1, which is characterized in that step(4)It is described
The mass ratio of reaction solution and aluminium chloride is 20:1.
5. a kind of preparation method of efficient absorption oil absorption material as described in claim 1, which is characterized in that step(5)It is described
The mass ratio of polystyrene tetrahydrofuran and nano SiO 2 particle is 3:6:1.
6. a kind of preparation method of efficient absorption oil absorption material as described in claim 1, which is characterized in that step(6)It is described
Fibrous material, maleic anhydride inoculated polypropylene, silane coupling agent mass ratio are 500:500:1.
7. a kind of preparation method of efficient absorption oil absorption material as described in claim 1, which is characterized in that step(6)It is described
Silane coupling agent is vinyltriethoxysilane, vinyltrimethoxysilane, vinyl three (beta-methoxy ethyoxyl) silane
One of.
8. a kind of preparation method of efficient absorption oil absorption material as described in claim 1, which is characterized in that step(7)It is described
Starch and the mass ratio of deionized water are 2:3.
9. a kind of preparation method of efficient absorption oil absorption material as described in claim 1, which is characterized in that step(8)It is described
Master batch, ammonium hydrogen carbonate and adhesive quality ratio are 5:6:10.
10. a kind of preparation method of efficient absorption oil absorption material as described in claim 1, which is characterized in that step(9)It is described
The mass ratio of fuel thickener, granular foamed material and acetone is 1:4:6.
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Cited By (3)
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CN110482637A (en) * | 2019-07-03 | 2019-11-22 | 同济大学 | A kind of Processes and apparatus for clearing up oil pollution of waters |
CN116212825A (en) * | 2023-03-10 | 2023-06-06 | 山东交通学院 | Modified waste coffee grounds biochar adsorption material and preparation method thereof |
CN116212825B (en) * | 2023-03-10 | 2024-05-14 | 山东交通学院 | Modified waste coffee grounds biochar adsorption material and preparation method thereof |
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CN104017234A (en) * | 2014-05-27 | 2014-09-03 | 哈尔滨工业大学 | Preparation method of polyurethane sponge and dicarbamic alkyl ester oil gelling agent composite oil spillage treatment material |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110482637A (en) * | 2019-07-03 | 2019-11-22 | 同济大学 | A kind of Processes and apparatus for clearing up oil pollution of waters |
CN110482637B (en) * | 2019-07-03 | 2021-03-26 | 同济大学 | Process and equipment for cleaning oil stain in water area |
CN116212825A (en) * | 2023-03-10 | 2023-06-06 | 山东交通学院 | Modified waste coffee grounds biochar adsorption material and preparation method thereof |
CN116212825B (en) * | 2023-03-10 | 2024-05-14 | 山东交通学院 | Modified waste coffee grounds biochar adsorption material and preparation method thereof |
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Application publication date: 20181116 |