CN-121974366-A - Amino-functionalized mesoporous silicon-based molecular sieve adsorption material, and preparation method and application thereof

CN121974366ACN 121974366 ACN121974366 ACN 121974366ACN-121974366-A

Abstract

The invention discloses an amino-functionalized mesoporous silicon-based molecular sieve adsorption material, a preparation method and application thereof, the amino functionalized mesoporous silica-based molecular sieve adsorption material is prepared by taking copper tailings as raw materials through pretreatment, main reaction and post-treatment steps. The mesoporous molecular sieve material is suitable for heavy metal pollutant treatment and functional building material development. The method has the advantages of simple preparation, low cost, excellent adsorption performance, effective removal of lead and cadmium ions in water, and environment-friendly and pollution-free prepared building materials.

Inventors

FU YANXIONG
LI YUEXIAN
CHEN DONG
YANG WANXIN
Yu Muyan
LI AN
ZHU HONGXU
Yu Xiaolv
LIU WEIWEI
XU ANBING
CHEN HUAJUN
LUO JING
XIONG GUOHUAN
Huang Shuaiwu

Assignees

易门铜业有限公司

Dates

Publication Date: 20260505
Application Date: 20251229

Claims (10)

1. The amino-functionalized mesoporous silica-based molecular sieve adsorption material is characterized in that the amino-functionalized mesoporous silica-based molecular sieve adsorption material is prepared by taking copper tailings as raw materials through pretreatment, main reaction and post-treatment.
2. A method for preparing the amino-functionalized mesoporous silica-based molecular sieve adsorption material according to claim 1, which comprises pretreatment, main reaction and post-treatment, and specifically comprises the following steps: A. The pretreatment, namely crushing, grinding, sieving, calcining at high temperature and acid leaching the raw copper tailings to obtain solid residues, and performing alkali dissolution activation on the solid residues to obtain a silicon-aluminum source precursor solution a; B. The main reaction: 1) Uniformly stirring and mixing a silicon-aluminum source precursor solution a and a 3-aminopropyl triethoxysilane solution to obtain uniform sol b; 2) Carrying out hydrothermal crystallization reaction on the uniform sol b, discarding supernatant after the reaction is finished, and collecting off-white precipitate to obtain a material c; C. Post-treatment: 1) Subjecting the material c to alternate centrifugal washing by using absolute ethyl alcohol and deionized water until a washing solution is neutral to obtain a solid product d; 2) And drying the solid product d to obtain the target amino-functionalized mesoporous silica-based molecular sieve adsorption material.
3. The method according to claim 2, wherein the crushing, grinding and sieving in the step a is to crush and grind copper tailings through a 400-mesh sieve.
4. The method according to claim 2, wherein the high-temperature calcination in the step a is performed by placing the ground copper tailing powder in a corundum crucible, and calcining in a static air atmosphere in a transfer muffle furnace.
5. The method according to claim 4, wherein the calcination is performed at a temperature rising rate of 4 to 6 ℃ per minute to 750 to 850 ℃ for 2 to 4 hours.
6. The preparation method according to claim 2, wherein the acid leaching treatment in the step A is to mix the calcined powder with hydrochloric acid solution and then stir the mixture for 2 to 4 hours under the condition of constant temperature water bath at 70 to 80 ℃.
7. The preparation method according to claim 2, wherein the alkali dissolution activation in the step a is to add sodium hydroxide solution into the solid residue, and stir and react for 2-4 hours at 70-80 ℃.
8. The preparation method according to claim 2, wherein the hydrothermal crystallization reaction in the step B2) is to perform static crystallization for 20-28 h in a blast drying oven at 120-140 ℃ after sealing and adjusting the pH value of the uniform sol B system to 1.5-2.5.
9. The method according to claim 2, wherein the drying in step C2) is re-drying in a vacuum oven at a temperature of 50 to 70 ℃ for 10 to 14 hours.
10. The use of an amino-functionalized mesoporous silica-based molecular sieve adsorbent material according to claim 1, wherein the amino-functionalized mesoporous silica-based molecular sieve adsorbent material is used in the preparation of an amino-functionalized mesoporous silica-based molecular sieve or a functionalized additive.

Description

Amino-functionalized mesoporous silicon-based molecular sieve adsorption material, and preparation method and application thereof Technical Field The invention belongs to the field of waste recycling, and particularly relates to an amino-functionalized mesoporous silicon-based molecular sieve adsorption material, and a preparation method and application thereof. Background Along with the continuous acceleration of the industrialization process, copper is taken as an important industrial resource, and a large amount of copper tailings are generated in the mining and dressing processes of the copper. The large-scale stockpiling of the tailings not only occupies land, but also brings more serious problems that heavy metals (such As Cu, as and Pb) and residual flotation agents contained in the copper tailings are easy to migrate along with percolate to cause persistent pollution to surrounding soil and water, and the tailings are frequent in breaking risk of the tailings reservoir dam body and easy to cause property loss and casualties in safety, and high treatment cost is generated in the aspect of society and economy due to unreasonable disposal of the tailings, and meanwhile, the migration and transformation of the heavy metals directly endangers public health. The current mainstream disposal mode (such as landfill or low added value building material utilization) is difficult to fundamentally break the dual pressure of resources and environment, so that development of high-value utilization technology is needed to realize the green transformation goal of treating waste with waste. The mesoporous silicon-based molecular sieve has important application value in the fields of catalysis, adsorption and the like because of high specific surface area, adjustable aperture and ordered pore canal structure. Traditional synthesis mainly relies on commercial silicon sources (such as ethyl orthosilicate) and surfactant templates, and mesoporous structures are formed by assembling in alkaline or acidic media by a sol-gel method. Patent CN1915815 discloses a method for modifying MCM-41 molecular sieve. The method firstly needs to completely synthesize the MCM-41 molecular sieve carrier, and then covers a layer of silicon atoms on the inner wall of the pore canal of the carrier for modification through secondary processing (such as silanization treatment). The process has obvious disadvantages of high cost of raw materials such as used silicon source, complex step-by-step modification process and obvious energy consumption and time cost. Resulting in poor overall economy and difficulty in adapting to cost-sensitive large-scale industrial production and applications. Patent CN1597516 discloses a preparation method of microporous-mesoporous composite molecular sieve, the preparation method needs to undergo two static crystallization processes (total duration can be up to 194 hours) for several days, in addition, the method needs to construct mesopores by dissolving crystal edge silicon aluminum, uncontrollability of solubility of the mesoporous composite molecular sieve leads to irregular distribution of mesopore size of final product, and possibly insufficient order and uniformity, thereby affecting shape selectivity of the final product in advanced catalytic reaction. Therefore, it is necessary to develop a product and a method that solve the above technical problems. Disclosure of Invention The invention provides an amino-functionalized mesoporous silicon-based molecular sieve adsorption material, and a preparation method and an application of the amino-functionalized mesoporous silicon-based molecular sieve adsorption material. The first object of the invention is realized in such a way that the amino-functionalized mesoporous silica-based molecular sieve adsorption material is prepared by taking copper tailings as raw materials through pretreatment, main reaction and post-treatment. The second object of the present invention is achieved by comprising pretreatment, main reaction and post-treatment, specifically comprising: A. The pretreatment, namely crushing, grinding, sieving, calcining at high temperature and acid leaching the raw copper tailings to obtain solid residues, and performing alkali dissolution activation on the solid residues to obtain a silicon-aluminum source precursor solution a; B. The main reaction: 1) Uniformly stirring and mixing a silicon-aluminum source precursor solution a and a 3-aminopropyl triethoxysilane solution to obtain uniform sol b; 2) Carrying out hydrothermal crystallization reaction on the uniform sol b, discarding supernatant after the reaction is finished, and collecting off-white precipitate to obtain a material c; C. Post-treatment: 1) Subjecting the material c to alternate centrifugal washing by using absolute ethyl alcohol and deionized water until a washing solution is neutral to obtain a solid product d; 2) And drying the solid product d to obtain the target amino-functionali