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Preparation method of novel mesoporous material for absorbing heavy metal ions in wastewater

A technology of heavy metal ions and mesoporous materials, applied in the fields of adsorption water/sewage treatment, non-metallic elements, chemical instruments and methods, etc., can solve the problems of different grafting amount, limitation, collapse of pore structure, etc.

Inactive Publication Date: 2013-02-06
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the grafting amount of different silane coupling agents is also different, which limits the subsequent grafting reaction.
The functionalized mesoporous silica obtained by the co-condensation method, although the rare earth metal compound is evenly distributed, the content cannot exceed 25%
If too much silane coupling agent is added to the precursor gel, it will affect the polycondensation process and cause the collapse of the pore structure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for synthesizing an ultra-stable and ordered mesoporous silicon rare earth molecular sieve, adding a rare earth salt solution while adding a silicon source, the process steps are as follows:

[0027] ●Synthesis of mesoporous molecular sieve precursor: at room temperature, the template agent polyethylene oxide-polypropylene oxide-polyethylene oxide P123 (PEO-PPO-PEO, Ma=5800) triembedded The block copolymer was added into the deionized water, stirred thoroughly, and after it was completely dissolved, the temperature was kept at room temperature.

[0028] ●Add silicon source tetraethyl orthosilicate, neodymium nitrate, sodium hydroxide and deionized water to the solution to adjust the pH value of the reaction system to 11.2, and the molar ratio of each reactant is: TPA + / Nd 2 o 3 / SiO 2 / Na 2 O / H 2 O=1:0.055~0.275:2.58:0.057~2.64:316.5.

[0029] Among them, TPA + It is a template agent, stirred and crystallized in an alkaline environment, the crystallizat...

Embodiment 2

[0033] An ordered double mesoporous silica rare earth material, using ethyl orthosilicate and polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer (F127) and cetyltrimethylammonium bromide ( The self-assembly of CTAB) is obtained by rapid decompression suction filtration and roasting to remove the organic template. The material has large mesopores with a pore size of 38±2nm? A double mesoporous silicon oxide rare earth material arranged in an orderly direction; the material is obtained by the following steps:

[0034] Dissolve 2mL of polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer (F127) and 6mL of cetyltrimethylammonium bromide (CTAB) in deionized water, stir well until it is completely dissolved, Constant temperature at room temperature for 2h. And adjust the pH>10 of the reaction system.

[0035] ●Add 1.8mL tetraethyl orthosilicate dropwise under stirring, the reaction mixture reacts at room temperature under magnetic stirring for 2 hour...

Embodiment 3

[0039] ● Dissolve a certain amount of template agent cetyltrimethylammonium bromide (CTAB) in a certain amount of deionized water at room temperature, stir well until it is completely dissolved, and keep the temperature at 25°C for 1 hour. Then, continue to stir, add a certain amount of ethylenediamine at one time to adjust the pH value of the reaction system, and control the amount of ethylenediamine added so that the pH value of the system is about 11.5.

[0040] ●Then, add a certain amount of tetraethyl orthosilicate (TEOS) and Nd(NO 3 ) 3 . At this time n(TEOS):n(Nd(NO 3 ) 3 ):n(CTAB):n(H 2 NCH 2 CH 2 NH 2 ):n(H 2 O)=1:0.05:0.31:22:1200. In an alkaline environment, stir, crystallize, react at 100 ° C for 7 h to stop the reaction, age, and synthesize the precursor of the mesoporous molecular sieve; the obtained product is subjected to vacuum filtration,

[0041] ●Finally, wash it with deionized water until neutral, dry the solid at 110°C for 10h, and then roast th...

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PUM

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Abstract

The invention relates to a preparation method of a novel mesoporous material for absorbing heavy metal ions in wastewater. The preparation method comprises the following steps of: 1, preparing a template; 2, hydrolyzing silicon source and rare-earth salt solution so as to form sol-gel, and crystallizing; and 3, removing a template agent, so as to obtain a sample. According to the preparation method, the synthetic method, which is low in cost, low in toxicity, simple, convenient and fast, is adopted, and the template agent is recovered, so that the cost is reduced, the performance of the mesoporous material is optimized; a mesoporous molecular sieve is simple in synthetic route, low in cost, and high in adsorptive property respect to the special ions in the solutions. After the mesoporous material is applied to a heavy metal ion absorption experiment, the ion concentrations of Pb2+, Zn2+, Cu2+ and Pb2+ in the solution after treatment are lower than the national drinking water standard. The mesoporous material is high in absorbing efficiency for Ag+.

Description

technical field [0001] The invention relates to a preparation method of a multifunctional mesoporous adsorption material for absorbing heavy metal ions in waste water. Background technique [0002] Research in recent years has found that due to the regular structure of the mesoporous molecular sieve with a single skeleton, the lack of protonic acid and Lewis acid centers, and low reactivity, it cannot perform well as an adsorbent. Modification by doping atoms or organic molecules The functionalization of mesoporous molecular sieves by means of immobilization and immobilization of active components can change its adsorption performance. The introduction of heteroatoms is to embed metal heteroatoms into the bone molecular sieve framework during the preparation process, thereby changing the stability and hydrophobic properties of mesoporous molecular sieves; organic functional group modification means modifying the surface of mesoporous molecular sieves by copolymerization or g...

Claims

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Application Information

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IPC IPC(8): B01J20/10B01J20/30C02F1/28C02F1/62
Inventor 杨鸿鹰段宝民张玉荣
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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