CN112295540A - Preparation method of carbon quantum dot modified activated carbon heavy metal adsorption material - Google Patents

Preparation method of carbon quantum dot modified activated carbon heavy metal adsorption material Download PDF

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Publication number
CN112295540A
CN112295540A CN202011020095.5A CN202011020095A CN112295540A CN 112295540 A CN112295540 A CN 112295540A CN 202011020095 A CN202011020095 A CN 202011020095A CN 112295540 A CN112295540 A CN 112295540A
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quantum dot
activated carbon
carbon
solution
carbon quantum
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CN202011020095.5A
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张太亮
郑存川
袁磊
李朝晖
张旭
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Chengdu Zhicheng Zhongwu Oil And Gas Technology Service Co ltd
Southwest Petroleum University
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Chengdu Zhicheng Zhongwu Oil And Gas Technology Service Co ltd
Southwest Petroleum University
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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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a carbon quantum dot modified activated carbon heavy metal adsorption material, which comprises the following steps: step one, pretreating activated carbon; step two, placing the activated carbon pretreated in the step one in a carbon quantum dot aqueous solution, performing ultrasonic dispersion at normal temperature, and finally standing for precipitation; and step three, drying the activated carbon subjected to standing precipitation in the step two to finally obtain the carbon quantum dot modified activated carbon adsorption material. The selective adsorption performance of the new material prepared by the invention on heavy metal ions is improved; and the adsorbing material has stable performance and high biocompatibility, and the application range of the adsorbent is enlarged.

Description

Preparation method of carbon quantum dot modified activated carbon heavy metal adsorption material
Technical Field
The invention relates to a preparation method of a carbon quantum dot modified activated carbon heavy metal adsorption material.
Background
At present, the treatment method for heavy metal polluted wastewater mainly comprises the following steps: chemical deposition, electrochemical, membrane filtration and adsorption, all of which have their advantages and disadvantages and bring about environmental pollution. The adsorption method has the characteristics of simple operation, no secondary pollution and high adsorption efficiency in the heavy metal waste treatment technology, but also has the defects of high cost and short service life. The active carbon is used as an adsorbent, and the effect on selective adsorption is poor when the active carbon is used singly, so that the active carbon and other materials are required to be compounded to form a new material for improving the performance.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of a carbon quantum dot modified activated carbon heavy metal adsorption material.
The technical scheme provided by the invention for solving the technical problems is as follows: a carbon quantum dot modified activated carbon heavy metal adsorption material comprises the following steps:
step one, pretreating activated carbon;
step two, placing the activated carbon pretreated in the step one in a carbon quantum dot aqueous solution, performing ultrasonic dispersion at normal temperature, and finally standing for precipitation;
and step three, drying the activated carbon subjected to standing precipitation in the step two to finally obtain the carbon quantum dot modified activated carbon adsorption material.
The further technical scheme is that the pretreatment process in the step one is as follows: the block active carbon is treated by crushing, grinding and sieving, then is placed in pure water for soaking, and the sediment on the lower layer is dried; placing the dried active carbon in HNO3Soaking in the solution, washing the soaked activated carbon, and drying to obtain the pretreated activated carbon.
The further technical proposal is that the HNO3The concentration of the solution was 10%, which was in HNO3The soaking time in the solution is 24 hours, and the drying temperature is 105 ℃.
The further technical scheme is that the sieving in the first step is a 60-mesh sieve.
The further technical scheme is that the carbon quantum dot aqueous solution in the second step is prepared by the following steps: mixing citric acid and ethylenediamine, dissolving in water, ultrasonically mixing uniformly, placing the uniformly mixed solution in a reaction kettle for heat preservation, dialyzing the heat-preserved solution to obtain a carbon quantum dot solution, and finally mixing the carbon quantum dot solution with pure water to obtain a carbon quantum dot solution water solution.
The further technical scheme is that the mixing ratio of the citric acid to the ethylenediamine is 1: 1.
the further technical scheme is that the ultrasonic treatment time is 30 minutes, the heat preservation temperature is 200 ℃, the heat preservation time is 5 hours, and the dialysis time is 24 hours.
Compared with the prior art, the method has the following advantages: the selective adsorption performance of the new material prepared by the invention on heavy metal ions is improved; and the adsorbing material has stable performance and high biocompatibility, and the application range of the adsorbent is enlarged.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
1) Preparing a carbon quantum dot solution: mixing citric acid and ethylenediamine according to the proportion of 1: 1, dissolving the mixture in 30mL of pure water, carrying out ultrasonic treatment for 30min, uniformly mixing, placing the uniformly mixed solution in a reaction kettle at 200 ℃, preserving the heat for 5h, then placing the heat-preserved solution in a dialysis bag, and dialyzing for 24h to obtain a carbon quantum dot solution;
2) active carbon pretreatment: crushing the blocky activated carbon, grinding the blocky activated carbon to pass through a 60-mesh screen, soaking the blocky activated carbon in pure water, taking the lower-layer precipitate, and drying the lower-layer precipitate in an oven; 10g of dried activated carbon is added into 100mL of 10% HNO3Soaking in the solution for 24h, washing with pure water, and oven drying at 105 deg.C to obtain pretreated active carbon；
3) Carbon quantum dot modified activated carbon: adding a carbon quantum dot solution with the concentration of 10% into 100mL of pure water, then placing 5g of the pretreated activated carbon into 100mL of mixed solution, ultrasonically dispersing for 2h at normal temperature, finally standing for precipitation for 4h, washing with pure water and drying to obtain the carbon quantum dot modified activated carbon adsorbing material of the example 1.
Wherein the carbon quantum dot concentration is expressed as volume fraction (%) of the carbon quantum dot solution.
Example 2
1) Preparing a carbon quantum dot solution: mixing citric acid and ethylenediamine according to the proportion of 1: 1, dissolving the mixture in 30mL of pure water, carrying out ultrasonic treatment for 30min, uniformly mixing, placing the uniformly mixed solution in a 200 ℃ reaction kettle for heat preservation for 5h, then placing the heat preserved solution in a dialysis bag, and dialyzing for 24h to obtain a carbon quantum dot solution;
2) active carbon pretreatment: crushing the blocky activated carbon, grinding the blocky activated carbon to pass through a 60-mesh screen, soaking the blocky activated carbon in pure water, taking the lower-layer precipitate, and drying the lower-layer precipitate in an oven; 10g of dried activated carbon is added into 100mL of 10% HNO3Soaking the solution for 24 hours, washing the solution by pure water, and then drying the solution in an oven at 105 ℃ to obtain the pretreated activated carbon.
3) Carbon quantum dot modified activated carbon: adding a carbon quantum dot solution with the concentration of 50% into 100mL of pure water, then placing 5g of the pretreated activated carbon into 100mL of the carbon quantum dot aqueous solution, ultrasonically dispersing for 2h at normal temperature, finally standing for precipitation for 4h, washing with pure water, and drying to obtain the carbon quantum dot modified activated carbon adsorbing material of the embodiment 2.
Example 3
1) Preparing a carbon quantum dot solution: mixing citric acid and ethylenediamine according to the proportion of 1: 1, dissolving the mixture in 30mL of pure water, carrying out ultrasonic treatment for 30min, uniformly mixing, placing the uniformly mixed solution in a high-temperature reaction kettle, keeping different temperatures, keeping the temperature for 5h, then placing the reacted solution in a dialysis bag, and dialyzing for 24h to obtain a carbon quantum solution.
2) Active carbon pretreatment: pulverizing the block active carbon, grinding to 60 mesh, soaking in pure water, collecting the lower layer precipitate, and oven dryingDrying in the middle; 10g of dried activated carbon is added into 100mL of 10% HNO3Soaking the solution for 24 hours, washing the solution by pure water, and then drying the solution in a drying oven at 105 ℃ to obtain pretreated activated carbon;
3) carbon quantum dot modified activated carbon: adding a carbon quantum dot solution with the concentration of 100% into 100mL of pure water, then placing 5g of the pretreated activated carbon into 100mL of the carbon quantum dot aqueous solution, ultrasonically dispersing for 2h at normal temperature, finally standing for precipitation for 4h, washing with pure water, and drying to obtain the carbon quantum dot modified activated carbon adsorbing material of the embodiment 3.
The carbon quantum dot-modified activated carbon adsorbent prepared in examples 1 to 3 was subjected to adsorption experiments, and the adsorption efficiency of the adsorbent was measured at intervals of time, and the effects of different adsorption times (0, 0.5, 1, 2, 4, 6, 12, and 24 hours), adsorption temperatures (25 ℃, 45 ℃, 65 ℃), and amounts (0, 1g/L, and 2g/L) on the removal efficiency of heavy metals were examined, and the results are as follows.
The results show that the carbon quantum dot modified activated carbon adsorbing material prepared in example 1 has the addition amount of 2g/L, the adsorption time of 12h, the adsorption temperature of 65 ℃ and Cr content3+The adsorption rate of (C) can reach 92.25%.
The results show that the carbon quantum dot modified activated carbon adsorbing material prepared in example 2 has the addition amount of 2g/L, the adsorption time of 12h, the adsorption temperature of 65 ℃ and Cr content3+The adsorption rate of the adsorbent reaches 83.66 percent at most.
The results show that the carbon quantum dot modified activated carbon adsorbing material prepared in example 3 has the addition amount of 2g/L, the adsorption time of 12h, the adsorption temperature of 65 ℃ and Cr content3+The adsorption rate of the catalyst can reach 74.56 percent at most.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited to the above embodiments, and those skilled in the art can make various changes and modifications without departing from the scope of the present invention.

Claims (7)

1. A preparation method of a carbon quantum dot modified activated carbon heavy metal adsorption material is characterized by comprising the following steps:
step one, pretreating activated carbon;
step two, placing the activated carbon pretreated in the step one in a carbon quantum dot aqueous solution, performing ultrasonic dispersion at normal temperature, and finally standing for precipitation;
and step three, drying the activated carbon subjected to standing precipitation in the step two to finally obtain the carbon quantum dot modified activated carbon adsorption material.
2. The preparation method of the carbon quantum dot modified activated carbon heavy metal adsorption material according to claim 1, wherein the pretreatment process in the first step is as follows: the block active carbon is treated by crushing, grinding and sieving, then is placed in pure water for soaking, and the sediment on the lower layer is dried; placing the dried active carbon in HNO3Soaking in the solution, washing the soaked activated carbon, and drying to obtain the pretreated activated carbon.
3. The preparation method of the carbon quantum dot modified activated carbon heavy metal adsorption material according to claim 2, characterized in that the HNO3The concentration of the solution was 10%, which was in HNO3The soaking time in the solution is 24 hours, and the drying temperature is 105 ℃.
4. The method for preparing the carbon quantum dot modified activated carbon heavy metal adsorption material according to claim 2, wherein the sieving in the first step is a 60-mesh sieve.
5. The preparation method of the carbon quantum dot modified activated carbon heavy metal adsorption material according to claim 1, wherein the carbon quantum dot aqueous solution in the second step is prepared by the following steps: mixing citric acid and ethylenediamine, dissolving in water, ultrasonically mixing uniformly, placing the uniformly mixed solution in a reaction kettle for heat preservation, dialyzing the heat-preserved solution to obtain a carbon quantum dot solution, and finally mixing the carbon quantum dot solution with pure water to obtain a carbon quantum dot solution water solution.
6. The carbon quantum dot modified activated carbon heavy metal adsorption material as claimed in claim 5, wherein the mixing ratio of citric acid and ethylenediamine is 1: 1.
7. the carbon quantum dot modified activated carbon heavy metal adsorption material as claimed in claim 5, wherein the ultrasonic time is 30 minutes, the heat preservation temperature is 200 ℃, the heat preservation time is 5 hours, and the dialysis time is 24 hours.
CN202011020095.5A 2020-09-25 2020-09-25 Preparation method of carbon quantum dot modified activated carbon heavy metal adsorption material Pending CN112295540A (en)

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CN113042004A (en) * 2021-04-13 2021-06-29 昆明理工大学 Preparation method and application of modified carbon-based material
CN113398888A (en) * 2021-07-13 2021-09-17 江苏建霖环保科技有限公司 Composite water purifying agent and preparation method thereof
CN113753878A (en) * 2021-09-30 2021-12-07 大连理工大学 Gravity field assisted method for regulating defect density of carbon material based on carbon quantum dots
CN115475604A (en) * 2022-09-16 2022-12-16 北京林业大学 Manufacturing method of composite multifunctional adsorbent based on cork activated carbon and amino carbon quantum dots
CN116037064A (en) * 2023-02-10 2023-05-02 北方民族大学 Nitrogen-doped carbon microsphere material, preparation method and application thereof
CN116199224A (en) * 2023-05-06 2023-06-02 成都达奇科技股份有限公司 Preparation method of coal-based granular activated carbon, product and dye wastewater decoloring method

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CN113042004A (en) * 2021-04-13 2021-06-29 昆明理工大学 Preparation method and application of modified carbon-based material
CN113042004B (en) * 2021-04-13 2022-08-05 昆明理工大学 Preparation method and application of modified carbon-based material
CN113398888A (en) * 2021-07-13 2021-09-17 江苏建霖环保科技有限公司 Composite water purifying agent and preparation method thereof
CN113753878A (en) * 2021-09-30 2021-12-07 大连理工大学 Gravity field assisted method for regulating defect density of carbon material based on carbon quantum dots
CN113753878B (en) * 2021-09-30 2023-08-15 大连理工大学 Gravity field assisted method for regulating and controlling defect density of carbon material based on carbon quantum dots
CN115475604A (en) * 2022-09-16 2022-12-16 北京林业大学 Manufacturing method of composite multifunctional adsorbent based on cork activated carbon and amino carbon quantum dots
CN115475604B (en) * 2022-09-16 2024-02-20 北京林业大学 Manufacturing method of composite multifunctional adsorbent based on cork activated carbon and amino carbon quantum dots
CN116037064A (en) * 2023-02-10 2023-05-02 北方民族大学 Nitrogen-doped carbon microsphere material, preparation method and application thereof
CN116199224A (en) * 2023-05-06 2023-06-02 成都达奇科技股份有限公司 Preparation method of coal-based granular activated carbon, product and dye wastewater decoloring method

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