CN113491997B - Lead ion sieve Na-TiAlSi-O, preparation method and application thereof - Google Patents
Lead ion sieve Na-TiAlSi-O, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a lead ion sieve Na-TiAl Si-O, a preparation method and application thereof; the preparation method comprises the following preparation steps: adding metatitanic acid powder, sodium silicate powder, aluminum oxide powder and sodium hydroxide powder into deionized water, mixing and stirring, and then sequentially precipitating, filtering, cleaning and drying to obtain a lead ion sieve precursor Pre-Na/TiAl Si/O; will contain Sr 2+ Carrying out hydrothermal reaction on the ionic salt solution and a lead ion sieve precursor Pre-Na/TiA l Si/O, and after the hydrothermal reaction, sequentially cooling, precipitating, filtering, cleaning and drying to obtain a lead ion sieve intermediate Sr/TiAl Si/O; soaking the intermediate Sr/TiAl Si/O of the lead ion sieve in NaC l solution, stirring, and sequentially precipitating, filtering, cleaning and drying to obtain Na/TiA l Si/O of the lead ion sieve; the obtained lead ion sieve Na/TiAl Si/O is to Pb 2+ Has very high selectivity and large adsorption capacity.
Description
Technical Field
The invention relates to the technical field of nanofiltration membranes, in particular to a lead ion sieve Na-TiAlSi-O, a preparation method and application thereof.
Background
Lead ion (Pb) 2+ ) Is a heavy metal ion, can be enriched and absorbed by passive plants in corresponding environments, and can cause harm to human health when being directly drunk or being contacted with a water body containing lead ions. Lead poisoning can cause irreversible damage to the liver, kidneys, reproductive system, and brain.
For the high-concentration lead ion wastewater, an alkali precipitation method and a cathode electrodeposition method can be adopted to remove the high-concentration lead ion wastewater; for water bodies containing low-concentration lead ions, an adsorption method or an ion exchange method is generally adopted to remove the lead ions, the adsorption method has the advantages of high efficiency, simplicity, convenience, good selectivity and the like, and currently, common adsorbents comprise resin, diatomite, chitosan, bentonite, activated carbon and the like. The adsorption materials for adsorbing low-concentration lead ions in water in the market, such as cation exchange resin, zeolite and other products, have low lead ion selectivity, small adsorption quantity and low adsorption rate, and cannot meet the treatment requirement of the water containing low-concentration lead ions.
Therefore, aiming at the problems, the invention urgently needs to provide a lead ion sieve Na-TiAlSi-O, a preparation method and application thereof.
Disclosure of Invention
The invention aims to provide a lead ion sieve Na-TiAlSi-O, a preparation method and application thereof, and solves the technical problems that the adsorption materials for adsorbing low-concentration lead ions in a water body on the market, such as cation exchange resin, zeolite and other products, have low selectivity, small adsorption quantity and small adsorption rate on the lead ions and cannot meet the treatment requirement of the water body containing the low-concentration lead ions in the prior art through the design of the preparation method of the lead ion sieve Na-TiAlSi-O.
The invention provides a preparation method of a lead ion sieve Na-TiAlSi-O, which is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
adding metatitanic acid powder, sodium silicate powder, aluminum oxide powder and sodium hydroxide powder into deionized water, mixing and stirring, and sequentially precipitating, filtering, cleaning and drying to obtain a lead ion sieve precursor Pre-Na/TiAlSi/O;
will contain Sr 2+ Carrying out hydrothermal reaction on the ionic salt solution and a lead ion sieve precursor Pre-Na/TiAlSi/O, and after the hydrothermal reaction, sequentially cooling, precipitating, filtering, cleaning and drying to obtain a lead ion sieve intermediate Sr/TiAlSi/O;
and soaking the intermediate Sr/TiAlSi/O of the lead ion sieve in a NaCl solution, stirring, and sequentially precipitating, filtering, cleaning and drying to obtain the Na/TiAlSi/O of the lead ion sieve.
Preferably, containing Sr 2+ The ionic salt solution is strontium chloride or strontium nitrate.
Preferably, in the preparation of the lead ion sieve precursor Pre-Na/TiAlSi/O, the amount of metatitanic acid powder is 0.1-1mol, the amount of sodium silicate powder is 1-2mol, the amount of alumina powder is 0.5-1mol, the amount of sodium hydroxide powder is 4-6mol, and the amount of deionized water is 1L;
200mL of SrCl with the concentration of 0.5-3mol/L is added in the process of preparing a lead ion sieve intermediate Sr/TiAlSi/O 2 Adding 100g of lead ion sieve precursor Pre-Na/TiAlSi/O into a hydrothermal reaction kettle for hydrothermal reaction;
in the process of preparing the lead ion sieve Na/TiAlSi/O, 50g of lead ion sieve intermediate Sr/TiAlSi/O is soaked in 500mL of NaCl solution with the concentration of 1-3 mol/L.
Preferably, after the metatitanic acid powder, the sodium silicate powder, the alumina powder and the sodium hydroxide powder are added into deionized water, mixing and stirring are carried out for 2-8h; filtering the precipitate, cleaning the precipitate, and drying the precipitate at 80-88 ℃ to obtain a lead ion sieve precursor Pre-Na/TiAlSi/O;
in the hydrothermal reaction process, the hydrothermal temperature is 120-180 ℃, the hydrothermal reaction time is 10-24h, the mixture is cooled to room temperature, precipitate is filtered, and deionized water is used for cleaning the precipitate and drying the precipitate to obtain a lead ion sieve intermediate Sr/TiAlSi/O;
and (3) soaking the intermediate Sr/TiAlSi/O of the lead ion sieve in a NaCl solution, stirring for 2-10h, precipitating and filtering, washing the precipitate with deionized water, and drying to obtain the Na/TiAlSi/O of the lead ion sieve.
Preferably, when washing the precipitate, the precipitate needs to be washed until the pH is neutral, and then dried.
Preferably, sr is added 2+ And carrying out hydrothermal reaction on the ionic salt solution and a lead ion sieve precursor Pre-Na/TiAlSi/O at the temperature of 150-170 ℃.
Preferably, sr is added 2+ The ionic salt solution and the lead ion sieve precursor Pre-Na/TiAlSi/O are subjected to hydrothermal reactionThe time is 12-20h.
Preferably, in the process of preparing the lead ion sieve precursor Pre-Na/TiAlSi/O, the lead ion sieve intermediate Sr/TiAlSi/O and the lead ion sieve Na/TiAlSi/O, the drying temperature of the precipitate obtained after precipitation and cleaning is 85 ℃.
The invention also provides a lead ion sieve Na-TiAlSi-O obtained by the preparation method of the lead ion sieve Na-TiAlSi-O.
The invention also provides an application of the lead ion sieve Na-TiAlSi-O in the treatment of lead-containing wastewater.
Compared with the prior art, the preparation method of the lead ion sieve Na-TiAlSi-O provided by the invention has the following steps:
1. the invention provides a preparation method of lead ion sieve Na-TiAlSi-O, and provides a method for utilizing Sr 2+ Performing ion imprinting of Pb 2+ Has an ionic radius of 0.119nm, sr 2+ Has an ionic radius of 0.118nm and Pb 2+ And Sr 2+ Has a very close ionic radius and the same charge number, thereby utilizing Sr 2+ Lead ion sieve Na/TiAlSi/O-B pair Pb obtained after ion imprinting 2+ Has very high selectivity and large adsorption capacity.
2. The preparation method of the lead ion sieve Na-TiAlSi-O provided by the invention is simple, and the obtained lead ion sieve Na/TiAlSi/O-B is used for Pb 2+ Has very high selectivity and large adsorption capacity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic diagram of a process of synthesizing raw materials of the lead ion sieve Na-TiAlSi-O;
FIG. 2 is a scanning electron microscope image of the lead ion sieve Na-TiAlSi-O according to the first embodiment;
FIG. 3 shows the results of treating the actual wastewater containing lead ions with the lead ion sieve Na-TiAlSi-O according to the first embodiment;
FIG. 4 is a scanning electron microscope image of the lead ion sieve Na-TiAlSi-O according to the second embodiment;
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a preparation method of a lead ion sieve Na-TiAlSi-O, which is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
s1) adding metatitanic acid powder, sodium silicate powder, aluminum oxide powder and sodium hydroxide powder into deionized water, mixing and stirring, and then sequentially precipitating, filtering, cleaning and drying to obtain a lead ion sieve precursor Pre-Na/TiAlSi/O;
s2) adding Sr 2+ Carrying out hydrothermal reaction on the ionic salt solution and a lead ion sieve precursor Pre-Na/TiAlSi/O, and after the hydrothermal reaction, sequentially cooling, precipitating, filtering, cleaning and drying to obtain a lead ion sieve intermediate Sr/TiAlSi/O;
and S3) soaking the lead ion sieve intermediate Sr/TiAlSi/O in a NaCl solution, stirring, and sequentially precipitating, filtering, cleaning and drying to obtain the lead ion sieve Na/TiAlSi/O.
Specifically, containing Sr 2+ The ionic salt solution is strontium chloride or strontium nitrate.
Specifically, in the preparation of a lead ion sieve precursor Pre-Na/TiAlSi/O, the amount of metatitanic acid powder is 0.1-1mol, the amount of sodium silicate powder is 1-2mol, the amount of alumina powder is 0.5-1mol, the amount of sodium hydroxide powder is 4-6mol, and deionized water is 1L;
200mL of the Sr/TiAlSi/O solution with the concentration of 0.5-3mol is used for determining the concentration of the Sr/TiAlSi/O solution in the process of preparing the lead ion sieve intermediateSrCl of L 2 Adding 100g of lead ion sieve precursor Pre-Na/TiAlSi/O into a hydrothermal reaction kettle for hydrothermal reaction;
in the process of preparing the lead ion sieve Na/TiAlSi/O, 50g of lead ion sieve intermediate Sr/TiAlSi/O is soaked in 500mL of NaCl solution with the concentration of 1-3 mol/L.
Specifically, metatitanic acid powder, sodium silicate powder, aluminum oxide powder and sodium hydroxide powder are added into deionized water and then mixed and stirred for 2-8h; filtering the precipitate, cleaning the precipitate, and drying the precipitate at 80-88 ℃ to obtain a lead ion sieve precursor Pre-Na/TiAlSi/O;
in the hydrothermal reaction process, the hydrothermal temperature is 120-180 ℃, the hydrothermal reaction time is 10-24h, the mixture is cooled to room temperature, precipitate is filtered, and deionized water is used for cleaning the precipitate and drying the precipitate to obtain a lead ion sieve intermediate Sr/TiAlSi/O;
and (3) soaking the intermediate Sr/TiAlSi/O of the lead ion sieve in a NaCl solution, stirring for 2-10h, precipitating and filtering, washing the precipitate with deionized water, and drying to obtain the Na/TiAlSi/O of the lead ion sieve.
Specifically, when washing the precipitate, the precipitate needs to be washed until the pH is neutral, and then dried.
Specifically, sr is added 2+ And carrying out hydrothermal reaction on the ionic salt solution and a lead ion sieve precursor Pre-Na/TiAlSi/O at the temperature of 150-170 ℃.
Specifically, sr is added 2+ And carrying out hydrothermal reaction on the ionic salt solution and a lead ion sieve precursor Pre-Na/TiAlSi/O for 12-20h.
Specifically, in the process of preparing a lead ion sieve precursor Pre-Na/TiAlSi/O, a lead ion sieve intermediate Sr/TiAlSi/O and a lead ion sieve Na/TiAlSi/O, the drying temperature of precipitates obtained after precipitation and cleaning is 85 ℃.
The invention also provides the lead ion sieve Na-TiAlSi-O obtained based on the preparation method of the lead ion sieve Na-TiAlSi-O.
The invention also provides an application of the lead ion sieve Na-TiAlSi-O in the treatment of lead-containing wastewater.
As shown in figure 1, the synthesis principle of the lead ion sieve Na-TiAlSi-O is as follows:
the preparation of the lead ion sieve Na-TiAlSi-O is divided into four stages:
1. the framework preforming stage is to construct a compound framework containing four elements of titanium, aluminum, silicon and oxygen, wherein the compound framework shows electronegativity, sodium ions are adsorbed on framework sites with electronegativity, and the framework has no determined tunnel size and no sites capable of selectively adsorbing lead ions. However, the framework pre-forming stage is to provide a framework containing titanium, aluminum, silicon and oxygen in the ion imprinting stage, and the disordered framework can surround Sr in the hydrothermal reaction process 2+ The ions undergo skeletal recombination.
2. In the stage of skeleton recombination and ion imprinting, a lead ion sieve precursor Pre-Na/TiAlSi/O and higher-concentration SrCl are mixed 2 The solution is mixed in a hydrothermal reaction kettle, hydrothermal reaction is carried out in the adding process, the hydrothermal reaction can lead disordered frameworks to be recombined, the frameworks still have electronegativity in the process of framework recombination, so that the negatively charged frameworks are recombined around positively charged cations, and almost high-concentration Sr is arranged around the frameworks 2+ Ions, the framework thus obtained for Sr 2+ The ions have size imprinting effect, and the obtained lead ion sieve intermediate Sr/TiAlSi/O.
3. In the ion exchange stage, the lead ion sieve intermediate Sr/TiAlSi/O is soaked in a high-concentration NaCl solution, and Na is utilized + Concentration advantage of (1), imprinting Sr in the skeleton 2+ And performing ion exchange to obtain the real lead ion sieve Na/TiAlSi/O.
4. Treatment of Pb-containing materials 2+ In the waste liquid stage, adding Na/TiAlSi/O of a lead ion sieve into the liquid containing Pb 2+ In the waste liquid, due to Pb 2+ Has an ionic radius of 0.119,Sr 2+ Has an ionic radius of 0.118nm, and thus Pb 2+ And Sr 2+ Have similar ion radius and charge number.
5. The regeneration and recycling stage of the lead ion sieve for treating Pb-containing materials 2+ Lead ion sieve Na/TiAlS in waste liquidi/O selective adsorption of Pb 2+ Then changing the lead ion sieve into Pb/TiAlSi/O, when the lead ion sieve Na/TiAlSi/O is completely changed into Pb/TiAlSi/O, considering that the lead ion sieve is saturated, therefore, regeneration is needed, soaking the lead ion sieve Pb/TiAlSi/O with saturated adsorption in NaCl solution with higher concentration, and utilizing Na + The lead ion sieve Na/TiAlSi/O is changed into the lead ion sieve Pb/TiAlSi/O again, and the regeneration and the recycling of the lead ion sieve are realized.
Example one
Framework preforming stage: adding 0.5mol of metatitanic acid powder, 1.5mol of silicic acid powder, 0.5mol of alumina powder and 5mol of sodium hydroxide powder into 1L of deionized water, stirring for 4 hours, filtering the precipitate, cleaning the precipitate with deionized water until the pH value is neutral, and drying the precipitate at 85 ℃ to obtain a lead ion sieve precursor Pre-Na/TiAlSi/O;
framework recombination and ion imprinting stages: 200mL of SrCl with the concentration of 3mol/L is added into a hydrothermal reaction kettle 2 Adding 100g of lead ion sieve precursor Pre-Na/TiAlSi/O into the solution, carrying out hydrothermal reaction for 24h at 150 ℃, cooling to room temperature, filtering the precipitate, washing with deionized water, and drying the precipitate to obtain a lead ion sieve intermediate Sr/TiAlSi/O;
ion exchange stage: 50g of lead ion sieve intermediate Sr/TiAlSi/O is soaked in 500mL of NaCl solution with the concentration of 2mol/L for 2-10h under mechanical stirring, and high-concentration Na in the solution is utilized + Sr in lead ion sieve intermediate Sr/TiAlSi/O 2+ And (3) filtering the precipitate, washing with deionized water, and drying to obtain the lead ion sieve Na/TiAlSi/O (sample 1).
The obtained sample 1 is shown in fig. 2, wherein a diagram b in fig. 2 is an enlarged view of a diagram a. As can be seen from fig. 2, the synthesized sample 1 has a microstructure of a long bar shape and a size of micrometer scale.
The prepared sample 1 was subjected to adsorption of lead ions with commercially available zeolite (purchased from shengsuchen technologies ltd, beijing) and cationic resin (purchased from shoudang senna chemical ltd), and the selectivity and adsorption capacity of the sample 1 were analyzed.
In particular toGround, configuration contains K + 、Na + 、Mg 2+ 、Ca 2+ And Pb 2+ Five kinds of cation mixed liquor, K in the mixed liquor + 、Na + 、Mg 2 + 、Ca 2+ And Pb 2+ The concentrations were all 100mg/L. 3 mixed solutions of 1L are measured, 0.1g of sample 1, 0.1g of zeolite and 0.1g of cation exchange resin are respectively added into the corresponding 1L of mixed solutions, the mixed solutions are adsorbed for 2 hours under stirring, the lead ion selectivity and the lead ion adsorption capacity of the mixed ion solution of the three adsorbing materials are examined, and the test results are shown in tables 1 and 2.
Tables 1 and 2 show that sample 1 is more selective for lead ions and has a greater capacity for adsorbing lead ions than zeolite and cation exchange resin.
And (3) actual water body testing:
mixing 85g of sample 1 and 15g of polyacrylonitrile, adding 200gN, N-Dimethylacetamide (DMAC) liquid, stirring for 5 hours, loading the feed liquid into an injector, spraying the feed liquid into deionized water, and performing phase conversion molding to obtain molded lead ion sieve particles.
The formed lead ion sieve particles are filled in an adsorption column, under the condition that the hydraulic retention time is 0.5h, the treatment of wastewater containing actual lead ions (the water source is the wastewater containing lead in the production of one domestic lead storage battery factory) is carried out, and raw water and produced water are taken for lead ion analysis, so that the results shown in the following table 3 and figure 3 are obtained.
As can be seen from FIG. 3 and Table 3, the concentration of lead ions in the lead ion-containing wastewater is actually 62.3mg/L, and after the wastewater passes through the lead ion sieve adsorption column, before the lead ion sieve is saturated by adsorption, the lead ion concentration of the produced water is very low, the lead ion concentration of the produced water is 0.01-0.02mg/L, the removal rate is 99.9%, and the quality of the produced water is very stable and hardly fluctuates. Therefore, the standard-reaching produced water which hardly contains lead ions can be obtained by using the lead ion sieve to treat the actual lead ion-containing wastewater, and the sample 1 can be used for treating the actual lead ion-containing wastewater and has a good application prospect.
Example two
Framework preforming stage: adding 1mol of metatitanic acid powder, 1mol of sodium silicate powder, 1mol of alumina powder and 6mol of sodium hydroxide powder into 1L of deionized water, stirring for 8 hours, filtering the precipitate, cleaning the precipitate with deionized water until the pH value is neutral, and drying at 85 ℃ to obtain a lead ion sieve precursor Pre-Na/TiAlSi/O;
in the stage of skeleton recombination and ion imprinting, 200mL of total NO (2 mol/LSr) solution is added into a hydrothermal reaction kettle 3 ) 2 Adding 100g of lead ion sieve precursor Pre-Na/TiAlSi/O into the solution, carrying out hydrothermal reaction for 10h at 180 ℃, cooling to room temperature, filtering the precipitate, cleaning with deionized water, and drying the precipitate to obtain a lead ion sieve intermediate Sr/TiAlSi/O;
ion exchange stage: 50g of lead ion sieve intermediate Sr/TiAlSi/O is soaked in 500mL of NaCl solution with the concentration of 1mol/L for 2 hours under mechanical stirring, and high-concentration Na in the solution is utilized + Sr in lead ion sieve intermediate Sr/TiAlSi/O 2+ And (3) filtering the precipitate, washing with deionized water, and drying to obtain the lead ion sieve Na/TiAlSi/O (sample 2).
The obtained sample 2 is shown in fig. 4, wherein the d diagram in fig. 4 is an enlarged view of the c diagram.
TABLE 1 lead ion Selectivity of three adsorption materials for Mixed ion solutions
TABLE 2 adsorption capacity of the three adsorption materials for lead ions
| Material | Commercially available zeolites | Commercial cation exchange resin | Sample No. 1 |
| Pb 2+ Adsorption capacity | 53mg/g | 76mg/g | 505mg/g |
TABLE 3 results of sample 1 on treating the actual lead ion-containing wastewater
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. A preparation method of a lead ion sieve Na-TiAlSi-O is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
adding metatitanic acid powder, sodium silicate powder, aluminum oxide powder and sodium hydroxide powder into deionized water, mixing and stirring, and then sequentially precipitating, filtering, cleaning and drying to obtain a lead ion sieve precursor Pre-Na/TiAlSi/O;
will contain Sr 2+ Carrying out hydrothermal reaction on the ionic salt solution and a lead ion sieve precursor Pre-Na/TiAlSi/O, and after the hydrothermal reaction, sequentially cooling, precipitating, filtering, cleaning and drying to obtain a lead ion sieve intermediate Sr/TiAlSi/O;
soaking the intermediate Sr/TiAlSi/O of the lead ion sieve in a NaCl solution, stirring, and sequentially precipitating, filtering, cleaning and drying to obtain the Na-TiAlSi-O of the lead ion sieve;
in the preparation of a lead ion sieve precursor Pre-Na/TiAlSi/O, the amount of metatitanic acid powder is 0.1-1mol, the amount of sodium silicate powder is 1-2mol, the amount of alumina powder is 0.5-1mol, the amount of sodium hydroxide powder is 4-6mol, and the amount of deionized water is 1L;
200mL of SrCl with the concentration of 0.5-3mol/L is added in the process of preparing a lead ion sieve intermediate Sr/TiAlSi/O 2 Adding 100g of lead ion sieve precursor Pre-Na/TiAlSi/O into a hydrothermal reaction kettle for hydrothermal reaction;
in the process of preparing the lead ion sieve Na-TiAlSi-O, 50g of lead ion sieve intermediate Sr/TiAlSi/O is soaked in 500mL of NaCl solution with the concentration of 1-3 mol/L;
adding metatitanic acid powder, sodium silicate powder, aluminum oxide powder and sodium hydroxide powder into deionized water, mixing and stirring for 2-8h, precipitating, filtering, cleaning precipitates, and drying the precipitates at 80-88 ℃ to obtain a lead ion sieve precursor Pre-Na/TiAlSi/O;
in the hydrothermal reaction process, the hydrothermal temperature is 120-180 ℃, the hydrothermal reaction time is 10-24h, the mixture is cooled to room temperature, precipitate is filtered, and deionized water is used for cleaning the precipitate and drying the precipitate to obtain a lead ion sieve intermediate Sr/TiAlSi/O;
and (3) soaking the intermediate Sr/TiAlSi/O of the lead ion sieve in a NaCl solution, stirring for 2-10h, precipitating and filtering, washing the precipitate with deionized water, and drying to obtain the Na-TiAlSi-O of the lead ion sieve.
2. The method for preparing the lead ion sieve Na-TiAlSi-O according to claim 1, which is characterized in that: when the precipitate is cleaned, the precipitate is required to be cleaned until the pH value is neutral, and then drying treatment is carried out.
3. The method for preparing the lead ion sieve Na-TiAlSi-O according to claim 1, which is characterized in that: will contain Sr 2+ And carrying out hydrothermal reaction on the ionic salt solution and a lead ion sieve precursor Pre-Na/TiAlSi/O at the temperature of 150-170 ℃.
4. The method for preparing the lead ion sieve Na-TiAlSi-O according to claim 1, which is characterized in that: will contain Sr 2+ And carrying out hydrothermal reaction on the ionic salt solution and a lead ion sieve precursor Pre-Na/TiAlSi/O for 12-20h.
5. The method for preparing the lead ion sieve Na-TiAlSi-O according to claim 1, which is characterized in that: in the process of preparing a lead ion sieve precursor Pre-Na/TiAlSi/O, a lead ion sieve intermediate Sr/TiAlSi/O and a lead ion sieve Na-TiAlSi-O, the drying temperature of precipitates obtained after precipitation and cleaning is 85 ℃.
6. A lead ion sieve Na-TiAlSi-O obtained based on the method for preparing the lead ion sieve Na-TiAlSi-O according to any one of claims 1 to 5.
7. The application of the lead ion sieve Na-TiAlSi-O in the treatment of lead-containing wastewater based on the lead ion sieve Na-TiAlSi-O in claim 6.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064226A (en) * | 1992-04-10 | 1992-09-09 | 天津大学 | Deleading ion sieve |
| CA2332706A1 (en) * | 2000-02-10 | 2001-08-10 | The Boc Group, Inc. | Method of manufacture of multicationic molecular sieves |
| CN103599757A (en) * | 2013-10-28 | 2014-02-26 | 江苏大学 | Preparation method of magnetic temperature-sensitive surface strontium ion blotting adsorbent |
| CN104525094A (en) * | 2015-01-09 | 2015-04-22 | 重庆工商大学 | Preparation method of manganese oxide ion sieve adsorbent and precursor thereof |
| CN105498676A (en) * | 2015-11-30 | 2016-04-20 | 中国科学院合肥物质科学研究院 | Sulfur-bearing hydroxyapatite lead ion adsorbent as well as synthetic method and application thereof |
| CN110844918A (en) * | 2019-11-12 | 2020-02-28 | 中国科学院福建物质结构研究所 | Y molecular sieve for synthesizing dimethyl carbonate by carbonylation of methyl nitrite and preparation method thereof |
| CN111204812A (en) * | 2020-01-09 | 2020-05-29 | 南京工业大学 | Preparation method of metal cation-doped modified lithium ion sieve |
| CN111450805A (en) * | 2020-04-09 | 2020-07-28 | 福州大学 | Chitosan-based lead ion imprinted adsorbent and preparation method thereof |
| CN113000013A (en) * | 2021-03-01 | 2021-06-22 | 厦门大学 | Method for treating radioactive strontium by using sodium manganese silicate adsorbent |
-
2021
- 2021-06-30 CN CN202110738810.7A patent/CN113491997B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064226A (en) * | 1992-04-10 | 1992-09-09 | 天津大学 | Deleading ion sieve |
| CA2332706A1 (en) * | 2000-02-10 | 2001-08-10 | The Boc Group, Inc. | Method of manufacture of multicationic molecular sieves |
| CN103599757A (en) * | 2013-10-28 | 2014-02-26 | 江苏大学 | Preparation method of magnetic temperature-sensitive surface strontium ion blotting adsorbent |
| CN104525094A (en) * | 2015-01-09 | 2015-04-22 | 重庆工商大学 | Preparation method of manganese oxide ion sieve adsorbent and precursor thereof |
| CN105498676A (en) * | 2015-11-30 | 2016-04-20 | 中国科学院合肥物质科学研究院 | Sulfur-bearing hydroxyapatite lead ion adsorbent as well as synthetic method and application thereof |
| CN110844918A (en) * | 2019-11-12 | 2020-02-28 | 中国科学院福建物质结构研究所 | Y molecular sieve for synthesizing dimethyl carbonate by carbonylation of methyl nitrite and preparation method thereof |
| CN111204812A (en) * | 2020-01-09 | 2020-05-29 | 南京工业大学 | Preparation method of metal cation-doped modified lithium ion sieve |
| CN111450805A (en) * | 2020-04-09 | 2020-07-28 | 福州大学 | Chitosan-based lead ion imprinted adsorbent and preparation method thereof |
| CN113000013A (en) * | 2021-03-01 | 2021-06-22 | 厦门大学 | Method for treating radioactive strontium by using sodium manganese silicate adsorbent |
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