CN114950334A - LaCl applied to adsorption of As 3 Functionalized expanded graphite and preparation method thereof - Google Patents
LaCl applied to adsorption of As 3 Functionalized expanded graphite and preparation method thereof Download PDFInfo
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- CN114950334A CN114950334A CN202210659527.XA CN202210659527A CN114950334A CN 114950334 A CN114950334 A CN 114950334A CN 202210659527 A CN202210659527 A CN 202210659527A CN 114950334 A CN114950334 A CN 114950334A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0207—Compounds of Sc, Y or Lanthanides
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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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- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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- C02F2101/103—Arsenic compounds
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Abstract
The invention discloses a LaCl for adsorbing As 3 Functionalized expanded graphite, the use of said LaCl for adsorbing As 3 The raw materials used in the preparation process of the functionalized expanded graphite are as follows: 1g expandable graphite, 1000ml polyvinyl alcohol (PVA) solution of 10mg/ml, 1.23g LaCl 3 5ml of 25 percent ammonia water and a plurality of portions of ultrapure water, including the preparation of ball-milling expanded graphite and LaCl 3 The preparation of the modified ball-milling expandable graphite, the equilibrium adsorption isothermal experiment, the adsorption kinetics experiment and the analysis of the experimental result are carried out in five processes, the ball-milling expandable graphite is ground into sheets, the vermicular characteristic is avoided, the ball-milling expandable graphite floats on the water surface, and the expandable graphite with the sheet structure adsorbs LaCl 3 Then, the obtained LaCl was prepared 3 The modified ball-milling expanded graphite has stronger affinity with As in wastewater, and the characteristics of pore structure, developed micropores and large specific surface area of the expandable graphite increase adsorption sites and strengthen LaCl 3 And the modified ball-milling expanded graphite removes As in water.
Description
Technical Field
The invention relates to the technical field of As adsorption, in particular to LaCl applied to adsorbing As 3 Functionalized expanded graphite and a preparation method thereof.
Background
Arsenic (As) is a highly toxic protoplasm poison, which has been identified As the first carcinogen by the international cancer research organization, and is listed As one of the priority pollutants in water by the World Health Organization (WHO). Therefore, there is increasing concern about the removal of As from water. At present, methods for removing As in water mainly comprise methods such As adsorption, coagulating sedimentation/microfiltration, ion exchange, membrane technology and the like, wherein the adsorption method is widely concerned because of the advantages of simple equipment, reliable operation, stable arsenic removal performance, high treatment efficiency, small adsorption interference, reusable adsorbent, little secondary pollution to the environment and the like.
Lanthanum is an abundant rare earth element, and has the advantages of high adsorption capacity, high adsorption speed, good selectivity and reproducibility when used as an adsorbent. Has strong binding capacity to phosphate. As is in the same main group As phosphorus and has a similar structure. Therefore, many researches take lanthanum As a potential material for adsorbing As, an adsorbent taking the lanthanum material As a raw material is widely applied to purifying polluted water bodies, but the wide application of lanthanum is limited by high price and scarcity of resources, while iron salt resources are rich and cheap, and the adsorbent is mainly used As a chemical As removal material in the past, but the adsorption capacity of As is not high enough, and the research is only limited to the research on graphene loaded iron-based materials at present. Expanded Graphite (EG) is a novel functional carbon material, which is a loose and porous vermicular substance obtained by intercalation, washing, drying and high-temperature expansion of natural graphite flakes. Has unique pore structure, developed micropores, large specific surface area, easy regeneration, and the like, and has the characteristics of softness, compression resilience, adsorbability, ecological environment harmony, biocompatibility, radiation resistance and the like which are not possessed by natural graphite. The vermicular nature of expanded graphite makes it prone to floating on the water surface, which limits the affinity for As in wastewater, reduces adsorption sites, and reduces its removal of As from the water.
Disclosure of Invention
The invention mainly aims to provide LaCl applied to adsorbing As 3 The functionalized expanded graphite and the preparation method thereof can effectively solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the technical scheme that:
LaCl applied to adsorption of As 3 Functionalized expanded graphite, the use of said LaCl for adsorbing As 3 The raw materials used in the preparation process of the functionalized expanded graphite are as follows: 1g expandable graphite, 1000ml polyvinyl alcohol (PVA) solution of 10mg/ml, 1.23g LaCl 3 5ml of 25% ammonia water, and several portions of ultrapure water.
LaCl applied to adsorption of As 3 Preparation method of functionalized expanded graphite, and LaCl for adsorbing As 3 The preparation method of the functionalized expanded graphite comprises the following specific steps:
the method comprises the following steps: preparing ball-milling expanded graphite, namely weighing 1g of expandable graphite, and carrying out microwave high-fire treatment for 5s to ensure that the expandable graphite is heated and expanded to form vermicular expanded graphite;
step two: ball milling the mixture by a ball mill, grinding the mixture into flaky substances, adding the flaky substances into 1000ml of 10mg/ml polyvinyl alcohol (PVA) solution, and carrying out ice-water bath ultrasound;
step three: performing first centrifugation to obtain supernatant, performing second centrifugation to obtain precipitate, and re-dispersing the precipitate into 200ml ultrapure water;
step four: LaCl 3 Preparation of modified ball-milled expandable graphite, weighing 1.23g of LaCl 3 Dissolving in 500ml of ultrapure water, and dissolving by magnetic stirring;
step five: 5ml of 25% ammonia water was added to adjust the pH to 11, and the mixture was stirred while heating;
step six: adding 100ml of the treated expanded graphite suspension, and continuously heating and stirring;
step seven: after cooling to room temperature, the solution was washed with ultrapure water 3 times and redispersed with ultrapure water to 200ml to give LaCl 3 Functionalized expanded graphite.
As a further scheme of the invention, the first step to the third step are the preparation process of the ball-milling expanded graphite, and the fourth step to the seventh step are LaCl 3 The preparation process of modified ball-milling expandable graphite.
As a further scheme of the invention, the ball milling time of the ball mill in the second step is 3 hours, and the ice-water bath ultrasound time is 6 hours.
As a further scheme of the invention, the rotating speed and time of the first centrifugal treatment in the third step are 3000rmp for 20min, and the rotating speed and time of the second centrifugal treatment are 10000rmp for 20 min.
As a further scheme of the invention, the heating temperature in the fifth step is 45 ℃, and the heating time is 30 min.
As a further scheme of the invention, the temperature end point of the continuous temperature rise in the sixth step is 90 ℃, and the heating time is 2 hours.
Compared with the prior art, the invention has the following beneficial effects:
the ball-milling expandable graphite is ground into sheets, so that the vermicular characteristic of the ball-milling expandable graphite is avoided, the ball-milling expandable graphite floats on the water surface, and the expandable graphite with the sheet structure adsorbs LaCl 3 Then, the obtained LaCl was prepared 3 The modified ball-milling expanded graphite has stronger affinity with As in wastewater, and the characteristics of pore structure, developed micropores and large specific surface area of the expandable graphite increase adsorption sites and strengthen LaCl 3 And the modified ball-milling expanded graphite removes As in water.
Drawings
FIG. 1 shows a LaCl solution for adsorbing As in accordance with the present invention 3 A preparation method of the functionalized expanded graphite and a flow chart of the characterization of the functionalized expanded graphite;
FIG. 2 is a graph of the effect of different As concentrations on As adsorption by a material according to the present invention;
FIG. 3 is a graph showing the change of the adsorption amount with time at different As concentrations according to the present invention;
FIG. 4 is a graph showing the removal rate of La-EG versus As at various As concentrations according to the present invention.
Detailed Description
In order to make the technical means, creation characteristics, achievement purposes and effects of the invention easy to understand, the LaCl is combined below 3 The invention is further illustrated by the specific characterization of the embodiment of the functionalized expanded graphite.
As shown in fig. 1, a LaCl for adsorbing As 3 Functionalized expanded graphite, the use of said LaCl for adsorbing As 3 The raw materials used in the preparation process of the functionalized expanded graphite are as follows: 1g expandable graphite, 1000ml polyvinyl alcohol (PVA) solution of 10mg/ml, 1.23g LaCl 3 5ml of 25% ammonia water, and several portions of ultrapure water.
LaCl applied to adsorption of As 3 Preparation method of functionalized expanded graphite, and LaCl for adsorbing As 3 The preparation method of the functionalized expanded graphite comprises the following specific steps:
the method comprises the following steps: preparing ball-milling expanded graphite, namely weighing 1g of expandable graphite, and carrying out microwave high-fire treatment for 5s to ensure that the expandable graphite is heated and expanded to form vermicular expanded graphite;
step two: ball milling the mixture by a ball mill, grinding the mixture into flaky substances, adding the flaky substances into 1000ml of 10mg/ml polyvinyl alcohol (PVA) solution, and carrying out ice-water bath ultrasound;
step three: performing first centrifugation, collecting supernatant, performing second centrifugation, collecting precipitate, and dispersing the precipitate into 200ml ultrapure water;
step four: LaCl 3 Preparation of modified ball-milled expandable graphite, weighing 1.23g of LaCl 3 Dissolving in 500ml of ultrapure water, and dissolving by magnetic stirring;
step five: 5ml of 25% ammonia water was added to adjust the pH to 11, and the mixture was stirred while heating;
step six: adding 100ml of the treated expanded graphite suspension, and continuously heating and stirring;
step seven: cooling to room temperature, washing with ultrapure water for 3 times, and re-dispersing with ultrapure water to 200ml to obtain LaCl 3 The expanded graphite is functionalized.
As a further embodiment of the present invention, the first step to the third step are ball-milling expansionThe preparation process of the graphite comprises the fourth step, the seventh step and the sixth step of LaCl 3 The preparation process of modified ball-milling expandable graphite.
As a further scheme of the invention, the ball milling time of the ball mill in the second step is 3 hours, and the ice-water bath ultrasound time is 6 hours.
As a further scheme of the invention, the rotating speed and time of the first centrifugal treatment in the third step are 3000rmp for 20min, and the rotating speed and time of the second centrifugal treatment are 10000rmp for 20 min.
As a further scheme of the invention, the heating temperature in the fifth step is 45 ℃, and the heating time is 30 min.
As a further scheme of the invention, the temperature end point of the continuous temperature rise in the sixth step is 90 ℃, and the heating time is 2h
Example 1
Equilibrium adsorption isothermal experiment
Selecting an As (III) solution with initial concentration of 0.1, 0.2, 0.5, 1.0, 2.0, 5.0, 10.0 and 20.0ppm, adding 2ml of LaCl which is uniformly mixed 3 The modified ball-milling expanded graphite material is added into 38ml of the solution, and is vibrated and adsorbed for 1h under the condition of 298K, and the concentration of As (III) in the adsorbed solution is measured.
Example 2
Adsorption kinetics experiment
Selecting an As (III) solution with the initial concentration of 0.1, 0.2, 0.5, 1.0, 2.0, 5.0, 10.0 and 20.0ppm, adding 2ml of adsorbing material, oscillating and adsorbing under the condition of 298K, and measuring the As (III) concentration in the adsorbed solution after 1, 2, 5, 10, 15, 20, 30, 45 and 60 min.
Analysis of the results of the experiment
As shown in FIG. 2, As the As concentration increases, LaCl 3 The adsorption amount of the modified ball-milling expanded graphite (La-EG) to As is gradually increased. When the As concentration is less than 5mg/L, the adsorption rate of the material to As is high. When the As concentration is 20mg/L, the adsorption quantity of the La-EG reaches 98.24 mg/g.
As shown in fig. 3, a: low concentration of As; b: high As concentration, the adsorption process of As is very rapid within 0-5min, and then the adsorption equilibrium is reached at 30 min.
As shown in FIG. 4, the La-EG material has different removal rates for As with different concentrations, wherein 1-8 correspond to concentrations of 0.1-20 mg/L, respectively, and when the initial concentration is 0.1mg/L, the removal rate reaches 84.27%, and the removal rate gradually decreases with the increase of the As concentration. The removal rate of As with concentration of less than 1.0mg/L is more than 70%, and the removal rate of As with concentration of 2.0-5.0mg/L is still more than 55%.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. LaCl applied to adsorption of As 3 The functionalized expanded graphite is characterized in that: the LaCl applied to adsorb As 3 The raw materials used in the preparation process of the functionalized expanded graphite are as follows: 1g expandable graphite, 1000ml polyvinyl alcohol (PVA) solution of 10mg/ml, 1.23g LaCl 3 5ml of 25% ammonia water, and several portions of ultrapure water.
2. LaCl applied to adsorption of As 3 The preparation method of the functionalized expanded graphite is characterized by comprising the following steps: the LaCl applied to adsorb As 3 The preparation method of the functionalized expanded graphite comprises the following specific steps:
the method comprises the following steps: preparing ball-milling expanded graphite, namely weighing 1g of expandable graphite, and carrying out microwave high-fire treatment for 5s to ensure that the expandable graphite is heated and expanded to form vermicular expanded graphite;
step two: ball milling the mixture by a ball mill, grinding the mixture into flaky substances, adding the flaky substances into 1000ml of 10mg/ml polyvinyl alcohol (PVA) solution, and carrying out ice-water bath ultrasound;
step three: performing first centrifugation to obtain supernatant, performing second centrifugation to obtain precipitate, and re-dispersing the precipitate into 200ml ultrapure water;
step four: LaCl 3 Preparation of modified ball-milled expandable graphite, weighing 1.23g of LaCl 3 Dissolving in 500ml of ultrapure water, and dissolving by magnetic stirring;
step five: 5ml of 25% ammonia water was added to adjust the pH to 11, and the mixture was stirred while heating;
step six: adding 100ml of the treated expanded graphite suspension, and continuously heating and stirring;
step seven: after cooling to room temperature, the solution was washed with ultrapure water 3 times and redispersed with ultrapure water to 200ml to give LaCl 3 Functionalized expanded graphite.
3. LaCl for adsorbing As according to claim 2 3 The preparation method of the functionalized expanded graphite is characterized by comprising the following steps: the first step to the third step are the preparation process of the ball-milling expanded graphite, and the fourth step to the seventh step are LaCl 3 The preparation process of modified ball-milling expandable graphite.
4. LaCl for adsorbing As according to claim 2 3 The preparation method of the functionalized expanded graphite is characterized by comprising the following steps: and in the second step, the ball milling time of the ball mill is 3 hours, and the ice-water bath ultrasound time is 6 hours.
5. LaCl for adsorbing As according to claim 2 3 The preparation method of the functionalized expanded graphite is characterized by comprising the following steps: and in the third step, the rotating speed and time of the first centrifugal treatment are 3000rmp and 20min, and the rotating speed and time of the second centrifugal treatment are 10000rmp and 20 min.
6. LaCl for adsorbing As according to claim 2 3 The preparation method of the functionalized expanded graphite is characterized by comprising the following steps: and the heating temperature in the fifth step is 45 ℃, and the heating time is 30 min.
7. According to the claims2 said LaCl for adsorbing As 3 The preparation method of the functionalized expanded graphite is characterized by comprising the following steps: and in the sixth step, the temperature end point of the continuous temperature rise is 90 ℃, and the heating time is 2 h.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104525111A (en) * | 2014-12-26 | 2015-04-22 | 上海大学 | Preparation method of lanthanum oxide modified expanded graphite adsorptive phosphorus removal agent |
| CN104722271A (en) * | 2015-03-31 | 2015-06-24 | 上海大学 | Preparation method of phosphorous removal adsorbent of expanded graphite loading lanthanum hydroxide |
| CN105771894A (en) * | 2016-04-15 | 2016-07-20 | 上海大学 | Phosphorus removal adsorbing agent for expanded graphite loaded composite metal and preparation method thereof |
| CN105854806A (en) * | 2016-06-03 | 2016-08-17 | 上海大学 | Lanthanum-iron-compound-metal-oxide-loading expanded-graphite phosphate removing agent and preparing method thereof |
| CN108190876A (en) * | 2018-02-26 | 2018-06-22 | 北京环境特性研究所 | A kind of graphene composite absorber and preparation method thereof |
| CN109529775A (en) * | 2019-01-18 | 2019-03-29 | 闽南师范大学 | A kind of synthetic method and absorption property of graphene oxide-lanthanum hydroxide composite material |
| CN111569819A (en) * | 2020-04-23 | 2020-08-25 | 武汉理工大学 | Hollow magnetic iron/lanthanum nano-microsphere and preparation method and application thereof |
-
2022
- 2022-06-13 CN CN202210659527.XA patent/CN114950334A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525111A (en) * | 2014-12-26 | 2015-04-22 | 上海大学 | Preparation method of lanthanum oxide modified expanded graphite adsorptive phosphorus removal agent |
| CN104722271A (en) * | 2015-03-31 | 2015-06-24 | 上海大学 | Preparation method of phosphorous removal adsorbent of expanded graphite loading lanthanum hydroxide |
| CN105771894A (en) * | 2016-04-15 | 2016-07-20 | 上海大学 | Phosphorus removal adsorbing agent for expanded graphite loaded composite metal and preparation method thereof |
| CN105854806A (en) * | 2016-06-03 | 2016-08-17 | 上海大学 | Lanthanum-iron-compound-metal-oxide-loading expanded-graphite phosphate removing agent and preparing method thereof |
| CN108190876A (en) * | 2018-02-26 | 2018-06-22 | 北京环境特性研究所 | A kind of graphene composite absorber and preparation method thereof |
| CN109529775A (en) * | 2019-01-18 | 2019-03-29 | 闽南师范大学 | A kind of synthetic method and absorption property of graphene oxide-lanthanum hydroxide composite material |
| CN111569819A (en) * | 2020-04-23 | 2020-08-25 | 武汉理工大学 | Hollow magnetic iron/lanthanum nano-microsphere and preparation method and application thereof |
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