CN113856653A - Preparation method of porous organic heavy metal adsorbent - Google Patents
Preparation method of porous organic heavy metal adsorbent Download PDFInfo
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- CN113856653A CN113856653A CN202111314882.5A CN202111314882A CN113856653A CN 113856653 A CN113856653 A CN 113856653A CN 202111314882 A CN202111314882 A CN 202111314882A CN 113856653 A CN113856653 A CN 113856653A
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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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- 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)
Abstract
The invention relates to the technical field of synthesis of novel high polymer materials, in particular to a preparation method of a porous organic heavy metal adsorbent, which comprises the following steps: dissolving a certain amount of trithiocyanuric acid in 100mL of aqueous solution, and slowly adding 30mL of sodium hydroxide aqueous solution while stirring; stirring the prepared solution at room temperature and filtering; mixing the prepared filtrate with 16mL aqueous solution of trisodium trithiocyanate, stirring in ice-water bath, and adding iodine-potassium iodide solution; repeatedly washing and filtering the stirred sample by using deionized water, adding a certain amount of hydrochloric acid solution and stirring; and (3) carrying out suction filtration on the stirred product, washing the product with deionized water, and then carrying out vacuum drying to obtain a light yellow solid. The porous organic heavy metal adsorbent prepared by the invention has larger specific surface area and pore volume and excellent heavy metal adsorption performance; the specificity and high-capacity adsorption of other heavy metal ions are realized; and the preparation method is simple, environment-friendly, free of secondary pollution and the like.
Description
Technical Field
The invention relates to the technical field of synthesis of novel high polymer materials, in particular to a preparation method of a porous organic heavy metal adsorbent.
Background
In recent years, the pollution of heavy metals to water is becoming serious and one of the pollution problems which are the most harmful to water resources. Heavy metals mainly come from the discharge of industrial sewage such as mining, electroplating, metal smelting and the like, the application of pesticides and fertilizers and the like, and enter a water body in various ways, and in addition, the heavy metals have high toxicity, biological accumulation and nondegradable property, so that the life safety of human beings is seriously threatened if the heavy metal pollution cannot be effectively treated.
Various water treatment techniques and processes have been developed, such as chemical precipitation, ion exchange, electrochemical methods, membrane separation, and adsorption. Among them, the adsorption method has attracted much attention, and is considered to be one of the most economical and effective methods for removing heavy metal ions in wastewater, particularly for treating large-volume low-concentration heavy metal wastewater, due to its advantages of large adsorption capacity, wide source of adsorption materials, high adsorption efficiency, high speed, simple operation, high adsorption selectivity, etc. However, the cost, the adsorption efficiency and the recycling performance of the adsorbent can affect the practical application of the adsorbent, especially the treatment of low-concentration and large-volume heavy metal wastewater. Therefore, research and development of an environment-friendly adsorption material which is efficient, easy to prepare, easy to separate, free of secondary pollution and capable of being recycled is still a key direction of domestic and foreign research. In view of this, we propose a method for preparing a porous organic heavy metal adsorbent.
Disclosure of Invention
The invention aims to provide a preparation method of a porous organic heavy metal adsorbent, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a porous organic heavy metal adsorbent comprises the following steps:
step 1: dissolving a certain amount of trithiocyanuric acid in 100mL of aqueous solution, and slowly adding 30mL of sodium hydroxide aqueous solution while stirring;
step 2: stirring the solution prepared in the step 1 at room temperature and then filtering;
and step 3: mixing the filtrate prepared in the step 2 with 16mL of aqueous solution of trisodium trithiocyanate, stirring in an ice-water bath, and adding an iodine-potassium iodide solution;
and 4, step 4: repeatedly washing and filtering the stirred sample by using deionized water, adding a certain amount of hydrochloric acid solution and stirring;
and 5: and (4) carrying out suction filtration on the product obtained by stirring in the step (4), washing the product with deionized water, and then carrying out vacuum drying to obtain a light yellow solid.
Preferably, in the step 1, the adding amount of trithiocyanuric acid is 0.03 mol; the concentration of the sodium hydroxide solution is 1 mol.L-1。
Preferably, in step 3, the mass fraction of the aqueous solution of trisodium trithiocyanate is 15%, and the iodine-potassium iodide solution is a saturated solution.
Preferably, in step 4, the concentration of the hydrochloric acid solution is 0.1-0.5 mol.L-1。
Preferably, in step 5, the vacuum drying temperature is 40-80 ℃.
Compared with the prior art, the invention has the beneficial effects that: according to the preparation method of the porous organic heavy metal adsorbent, the prepared environment-friendly heavy metal adsorbent has large specific surface area and pore volume and excellent heavy metal adsorption performance; introducing high-content active functional group sulfydryl to realize the specificity and high-capacity adsorption of other heavy metal ions; the method has the advantages of simple preparation method, environmental friendliness, no secondary pollution and the like, and has great application potential in the heavy metal water treatment industry.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a porous organic heavy metal adsorbent comprises the steps of adding 0.03mol of trithiocyanuric acid into 100mL of deionized water, slowly adding 30mL of sodium hydroxide aqueous solution under stirring, stirring for two hours at room temperature, and filtering to obtain filtrate, namely the trithiocyanuric acid monosodium salt aqueous solution.
16mL of an aqueous solution of trisodium trithiocyanate (w.t.15%) was mixed with the filtrate obtained above, stirred in a bath of water, 30mL of a saturated iodine-potassium iodide solution was slowly added when the temperature was below 0 ℃, stirred at 0 ℃ for two hours, slowly warmed to room temperature, and stirred overnight. Suction filtration, washing with deionized water for multiple times, adding 0.1M hydrogen chloride solution, and stirring for 3 h. And then carrying out suction filtration, washing with deionized water, and then carrying out vacuum drying at 60 ℃ to obtain a light yellow solid product.
Example 2
Adding 0.03mol of trithiocyanuric acid into 100mL of deionized water, slowly adding 30mL of sodium hydroxide aqueous solution while stirring, stirring for two hours at room temperature, and filtering to obtain filtrate, namely the trithiocyanuric acid monosodium salt aqueous solution.
16mL of an aqueous solution of trisodium trithiocyanate (w.t.15%) was mixed with the filtrate obtained above, stirred in a bath of water, 30mL of a saturated iodine-potassium iodide solution was slowly added when the temperature was below 0 ℃, stirred at 0 ℃ for two hours, slowly warmed to room temperature, and stirred overnight. And (4) carrying out suction filtration, washing with deionized water for multiple times, adding a 0.3M hydrogen chloride solution, and stirring for 3 hours. And then carrying out suction filtration, washing with deionized water, and then carrying out vacuum drying at 40 ℃ to obtain a light yellow solid product.
Example 3
Adding 0.03mol of trithiocyanuric acid into 100mL of deionized water, slowly adding 30mL of sodium hydroxide aqueous solution while stirring, stirring for two hours at room temperature, and filtering to obtain filtrate, namely the trithiocyanuric acid monosodium salt aqueous solution.
16mL of an aqueous solution of trisodium trithiocyanate (w.t.15%) was mixed with the filtrate obtained above, stirred in a bath of water, 30mL of a saturated iodine-potassium iodide solution was slowly added when the temperature was below 0 ℃, stirred at 0 ℃ for two hours, slowly warmed to room temperature, and stirred overnight. Suction filtration, washing with deionized water for multiple times, adding 0.1M hydrogen chloride solution, and stirring for 3 h. And then carrying out suction filtration, washing with deionized water, and then carrying out vacuum drying at 80 ℃ to obtain a light yellow solid product.
Through the content, the porous organic heavy metal adsorbent prepared by the method has larger specific surface area and pore volume and excellent heavy metal adsorption performance; introducing high-content active functional group sulfydryl to realize the specificity and high-capacity adsorption of other heavy metal ions; the method has the advantages of simple preparation method, environmental friendliness, no secondary pollution and the like, and has great application potential in the heavy metal water treatment industry.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. The preparation method of the porous organic heavy metal adsorbent is characterized by comprising the following steps:
step 1: dissolving a certain amount of trithiocyanuric acid in 100mL of aqueous solution, and slowly adding 30mL of sodium hydroxide aqueous solution while stirring;
step 2: stirring the solution prepared in the step 1 at room temperature and then filtering;
and step 3: mixing the filtrate prepared in the step 2 with 16mL of aqueous solution of trisodium trithiocyanate, stirring in an ice-water bath, and adding an iodine-potassium iodide solution;
and 4, step 4: repeatedly washing and filtering the stirred sample by using deionized water, adding a certain amount of hydrochloric acid solution and stirring;
and 5: and (4) carrying out suction filtration on the product obtained by stirring in the step (4), washing the product with deionized water, and then carrying out vacuum drying to obtain a light yellow solid.
2. The method for preparing the porous organic heavy metal adsorbent according to claim 1, wherein: in the step 1, the adding amount of trithiocyanuric acid is 0.03 mol; the concentration of the sodium hydroxide solution is 1 mol.L-1。
3. The method for preparing the porous organic heavy metal adsorbent according to claim 1, wherein: in the step 3, the mass fraction of the aqueous solution of the trisodium trithiocyanate is 15%, and the iodine-potassium iodide solution is a saturated solution.
4. The method for preparing the porous organic heavy metal adsorbent according to claim 1, wherein: in step 4, the concentration of the hydrochloric acid solution is 0.1-0.5 mol.L-1。
5. The method for preparing the porous organic heavy metal adsorbent according to claim 1, wherein: in step 5, the vacuum drying temperature is 40-80 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111314882.5A CN113856653A (en) | 2021-11-08 | 2021-11-08 | Preparation method of porous organic heavy metal adsorbent |
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| CN202111314882.5A CN113856653A (en) | 2021-11-08 | 2021-11-08 | Preparation method of porous organic heavy metal adsorbent |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016187796A1 (en) * | 2015-05-21 | 2016-12-01 | 江南大学 | Preparation method and use of heavy metal ion adsorbent |
| CN109894100A (en) * | 2019-04-15 | 2019-06-18 | 滨州学院 | A kind of preparation and application of graphene oxide/iron oxide/poly- trithiocyanuric acid trisodium salt porous adsorbing material |
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2021
- 2021-11-08 CN CN202111314882.5A patent/CN113856653A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016187796A1 (en) * | 2015-05-21 | 2016-12-01 | 江南大学 | Preparation method and use of heavy metal ion adsorbent |
| CN109894100A (en) * | 2019-04-15 | 2019-06-18 | 滨州学院 | A kind of preparation and application of graphene oxide/iron oxide/poly- trithiocyanuric acid trisodium salt porous adsorbing material |
Non-Patent Citations (1)
| Title |
|---|
| XIAOPAN LI ET AL.: "Design and synthesis of an efficient nanoporous adsorbent for Hg2+ and Pb2+ ions in water" * |
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Application publication date: 20211231 |